CN103646777A - Method for preparing crystal boundary nano-composite intensified neodymium iron boron magnet - Google Patents
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Abstract
The invention discloses a method for preparing a crystal boundary nano-composite intensified neodymium iron boron magnet, and relates to the technology of preparing permanent magnet materials. The method comprises the steps that firstly, principal phase alloy is manufactured into an ingot casting or rapid hardening ribbon through a casting method or a rapid hardening melt-spinning method, and the crystal boundary phase alloy is manufactured into a rapid quenching belt through a rapid quenching method; secondly, the principal phase alloy and the crystal boundary phase alloy are respectively manufactured into powder; thirdly, the graphene nanosheet powder and the crystal boundary phase alloy powder are mixed, then ball-milling is carried out, and the graphene nanosheet powder is evenly scattered into the crystal boundary phase alloy powder; fourthly, the crystal boundary phase alloy powder intensified through the graphene nanosheet powder is evenly mixed with the principal phase alloy powder to be directionally pressed in a magnetic field into a green body; fifthly, the spark plasma sintering and tempering are carried out on the green body, and then the high-tenacity crystal boundary nano-composite intensified neodymium iron boron magnet is manufactured. The tenacity of the crystal boundary phase is improved through the crystal boundary nanometer composite intensifying, and on the premise of guaranteeing the magnetic performance of the magnet, the tenacity of the magnet is improved. The method is simple in technology, easy to operate and suitable for being produced in batches on a large scale.
Description
Technical field
The present invention relates to permanent magnetic material preparing technical field, refer in particular to the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary.
Background technology
Sintered NdFeB magnet, as third generation rare earth permanent-magnetic material, has the incomparable excellent magnetic property of other permanent magnetic materials and high cost performance.Therefore,, since self-discovery, it has obtained research and swift and violent development widely, in high-tech sectors such as computer, communication electronics, automobile, aviations, is used widely.Along with improving constantly of magnetic property, its range of application is also in continuous expansion, and this also makes the shortcoming of its poor mechanical property highlight gradually, becomes and limits its further subject matter of application.Therefore, the mechanical property of raising Sintered NdFeB magnet becomes the important foundation that expands its range of application.
Sintered NdFeB magnet is a kind of fragile material, and its tension, bending strength and fracture toughness are lower, and this causes its obdurability poor.Obdurability official post Sintered NdFeB magnet easily ftractures, falls the problems such as limit, arrisdefect in preparation and fabrication process, affects it and prepares rate of finished products and machining accuracy.In addition, obdurability is poor has also limited its application in the higher occasion of mechanical property requirements, as fields such as Aero-Space, high-speed electric expreess locomotives.Sintered NdFeB magnet obdurability poor with its principal phase Nd
2fe
14the crystal structure of B is closely-related.Principal phase is tetragonal structure, and slip system number is fewer, makes its plastic deformation more difficult.In addition, the magnetocrystalline anisotropy of Sintered NdFeB magnet is also the major reason that causes its poor mechanical property, and this originates from the large internal stress that anisotropy causes.Research shows, the fracture mode of Sintered NdFeB magnet is mainly along brilliant brittle fracture, and this is to be caused by weak Grain-Boundary Phase.Therefore, Grain-Boundary Phase reduction is also the poor major reason of its obdurability.In recent years, people have also done certain research to the mechanical property of Sintered NdFeB magnet.The method adopting is at present mainly microalloying method.It is not only relevant with interpolation element to the improvement of magnet obdurability that element adds the microalloying causing, and be subject to the impact of magnet composition.Sometimes intensity and toughness can improve simultaneously, but sometimes present this those long trend that disappear.In addition, alloying also can cause the decline of magnet magnetic property sometimes.Therefore, do not find so far the method for suitable effective raising Sintered NdFeB magnet obdurability.
To, guaranteeing, under the prerequisite of Sintered NdFeB magnet magnetic property, to improve its obdurability, will start with from the strengthening of crystal boundary, because this can effectively suppress or be avoided along the generation of brilliant fracture.The crystal boundary modified raising that has been widely used in magnet magnetic property and decay resistance, wherein the crystal boundary of nano metal, Nano compound add can with Grain-Boundary Phase generation chemical reaction, reach the object of modification Grain-Boundary Phase, thereby the magnetic property and the decay resistance that improve magnet, the Patents of application is and the immediate patent application of the present invention.But, compare with the present invention, there is following fundamental difference.First, crystal boundary is introduced material difference.The present invention introduces the graphene nanometer sheet of mechanical property excellence first in the Grain-Boundary Phase of Sintered NdFeB magnet, forms the crystal boundary composite construction that nanometer strengthens; Secondly, mechanism is different.What the present invention emphasized is intercrystalline strengthening, is different from crystal boundary modified in existing patent.In crystal boundary modified, the nano metal of introducing and Nano compound all with Grain-Boundary Phase generation alloying reaction, thereby improve the physico-chemical property of Grain-Boundary Phase, improve magnet magnetic property and decay resistance; And intercrystalline strengthening is to introduce the hardening constituent not reacting with it in Grain-Boundary Phase, thereby play the effect that strengthens Grain-Boundary Phase mechanical property; Finally, method is had any different.In order to make graphene nanometer sheet hardening constituent more be uniformly distributed in Grain-Boundary Phase, the present invention has introduced a kind of new-type technology-resonance sound hybrid technology that mixes, low frequency, high sound intensity wave energy can produce uniform shearing field in whole container, the rapid fluidisation of material is mixed, compare that traditional planetary stirring, vane type are stirred and ultrasonic mixing etc., can reach better Blending Efficiency of Blending.
The nano combined intensifying method of pairing Jin Jing circle that the present invention proposes is that two alloyages and nano combined reinforcement technique are organically combined to a kind of novel intercrystalline strengthening method forming, and has effectively overcome existing methodical deficiency.The present invention be take pairing gold process as basis, by resonance sound hybrid technology and ball-milling technology, in crystal-boundary phase alloy magnetic, introduce equally distributed graphene nanometer sheet, form crystal boundary nanometer and strengthen composite construction, to improve the obdurability of Grain-Boundary Phase, improve the mechanical property of Sintered NdFeB magnet.In addition, the intercrystalline strengthening of introducing mutually can not affect Hard Magnetic principal phase composition and magnetic property, and the crystal-boundary phase alloy powder of nano combined strengthening still can effectively promote liquid-phase sintering, and crystal boundary liquid phase is uniformly distributed, and guarantees the high magnetic property of magnet.
Summary of the invention
The object of the invention is for overcoming now methodical deficiency, the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary is provided, it adopts the nano combined intensifying method of pairing Jin Jing circle that graphene nanometer sheet powder is evenly distributed in Grain-Boundary Phase, form crystal boundary nanometer and strengthen composite construction, improve the obdurability of magnet Grain-Boundary Phase, suppress, along the generation of brilliant fracture, to improve the obdurability of magnet.In addition, the crystal-boundary phase alloy powder of nano combined strengthening still can promote liquid-phase sintering, and crystal boundary liquid phase is uniformly distributed, and guarantees the high magnetic property of magnet.
The technical scheme that the present invention addresses the above problem is: adopt the nano combined intensifying method of pairing Jin Jing circle to prepare Sintered NdFeB magnet, graphene nanometer sheet powder is evenly distributed in Grain-Boundary Phase, the mechanical property of strengthening Grain-Boundary Phase, guarantee that crystal boundary liquid phase is uniformly distributed and effective densification of magnet simultaneously, guarantee the high magnetic property of magnet.Its concrete steps are:
1) main-phase alloy adopts casting method or rapid hardening to get rid of band method and makes ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts quick-quenching method to make rapid tempering belt;
2) by main-phase alloy and crystal-boundary phase alloy respectively by Mechanical Crushing or hydrogen explosion is broken carries out coarse crushing, coarse crushing is carried out fine grinding by ball milling or airflow milling, and making average particulate diameter is the main-phase alloy powder of 2-6 μ m and the crystal-boundary phase alloy powder of 1-5 μ m;
3) after graphene nanometer sheet powder is mixed with crystal-boundary phase alloy powder resonance sound, add dispersant to carry out vacuum or protective atmosphere ball milling, graphene nanometer sheet powder is dispersed in crystal-boundary phase alloy powder, obtains the crystal-boundary phase alloy powder that graphene nano strengthens;
4) by step 3) after the crystal-boundary phase alloy powder that strengthens of the graphene nano that obtains evenly mixes with main-phase alloy powder, in the magnetic field of 1.2-2.0T, be orientated die mould and make green compact;
5) green compact are carried out to discharge plasma sintering, and through 900-1000 ℃ of one-level tempering 1-2h and 500-650 ℃ of second annealing 0.5-1h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
The atomic percent of described main-phase alloy composition is Nd
xfe
100-x-y-zb
ym
z, 11≤x≤16 wherein, 5.5≤y≤7,0.1≤z≤10, M is one or more in Pr, Dy, Tb, Ho, Co, Ni, Al, Cu, Ga, Mg, Zn, Nb, Zr, Ti, Mo, W, V element.
The atomic percent of described crystal-boundary phase alloy composition is Nd
afe
100-a-b-cb
br
c, 12≤a≤30 wherein, 5≤b≤7,0.1≤c≤20, R is one or more in Pr, Dy, Tb, Ho, Gd, Ce, Co, Ni, Al, Cu, Ga, Mg, Zn, Si, Nb, Zr, Ti, Mo, W, V element.
The diameter of described graphene nanometer sheet powder is distributed in 0.5-2 μ m, and thickness distribution is at 0.6-1.2nm.
In described crystal-boundary phase alloy powder, the addition of graphene nanometer sheet powder is 1-10wt%.
Described resonance sound incorporation time is 2-10min.
Described dispersant is stearic acid, and addition is 1-6wt%.
Described discharge plasma sintering parameter is: sintering temperature is 600-900 ℃, and sintering time is 5-30min, and pressure is 5-50MPa.
The invention has the advantages that: adopt the nano combined intensifying method of pairing Jin Jing circle to prepare Sintered NdFeB magnet, be convenient to introduce nanometer reinforcing phase in Grain-Boundary Phase, regulation and control Grain-Boundary Phase the Nomenclature Composition and Structure of Complexes, is guaranteeing, under the prerequisite of high magnetic characteristics, to significantly improve the obdurability of magnet.Two alloyages make principal phase and Grain-Boundary Phase separate preparation, can under the prerequisite that does not affect Hard Magnetic principal phase composition and magnetic property, change structure and the mechanical property of Grain-Boundary Phase, and the crystal-boundary phase alloy powder of nano combined strengthening still can promote liquid-phase sintering, crystal boundary liquid phase is uniformly distributed, guarantees the high magnetic property of magnet.Nano combined strengthening is the effective ways that improve Fracture of Material And, and Graphene has excellent mechanical property, is introduced in the Grain-Boundary Phase of neodymium iron boron magnetic body, can effectively improve the obdurability of Grain-Boundary Phase, suppresses intercrystalline britftleness fracture, thereby improves the obdurability of magnet.Resonance sound hybrid technology is a kind of new-type technology that mixes, and low frequency, high sound intensity wave energy can produce uniform shearing field in whole container, and graphene nanometer sheet powder is distributed in Grain-Boundary Phase more equably, improves strengthening effect.The efficient sintering feature in short-term of discharge plasma sintering can effectively be avoided nanometer reinforcing phase Graphene and Grain-Boundary Phase generation interfacial reaction, and then guarantees nano combined strengthening effect.Therefore, the present invention can realize the matched well of high magnetic characteristics and high-strength tenacity keeping, under the prerequisite of high magnetic characteristics, significantly improving the obdurability of magnet, further expands its range of application.Technical process of the present invention is simple, easy to operate, is suitable for large-scale batch production, therefore, by the present invention, can prepare the high tough Sintered NdFeB magnet of high magnetic characteristics.
Embodiment
In the present invention, the nano combined strengthening neodymium iron boron magnetic body of crystal boundary is prepared by the nano combined intensifying method of pairing Jin Jing circle.First main-phase alloy and crystal-boundary phase alloy are prepared respectively to also powder process, then by the mixing of resonance sound and ball-milling technology, graphene nanometer sheet powder is dispersed in crystal-boundary phase alloy powder, and it is evenly mixed with main-phase alloy powder, in magnetic field, be orientated die mould and make green compact, finally green compact are carried out to discharge plasma sintering and final magnet is made in tempering.The Sintered NdFeB magnet density that adopts the present invention to prepare is high, and Grain-Boundary Phase is evenly distributed, and is the composite construction of nanometer enhancing, significantly improved the obdurability of Grain-Boundary Phase, suppressed along brilliant brittle fracture, and then improved the obdurability of Sintered NdFeB magnet, further expanded its practical application.
Embodiment 1:
1) main-phase alloy Nd
11pr
2fe
balzr
0.1b
5.5adopt rapid hardening belt-rejecting technology to make rapid hardening strip, copper roller degree of turning is 2m/s, crystal-boundary phase alloy Nd
12pr
20fe
balco
2cu
0.5b
7adopt rapid quenching technique to make rapid tempering belt, fast quenching speed is 16m/s;
2) main-phase alloy and crystal-boundary phase alloy are carried out to coarse crushing by Mechanical Crushing respectively, then under nitrogen protection, by airflow milling, make respectively the powder that average particulate diameter is 6 μ m and 5 μ m;
3) by 1wt% graphene nanometer sheet powder with after crystal-boundary phase alloy powder resonance sound mixing 2min, add 1wt% stearic acid to carry out vacuum ball milling, it is dispersed in crystal-boundary phase alloy powder;
4), after the crystal-boundary phase alloy powder graphene nano of 7wt% being strengthened evenly mixes with main-phase alloy powder, in the magnetic field of 2.0T, be orientated die mould and make green compact;
5) by green compact 600 ℃ with 50MPa pressure under discharge plasma sintering 30min, then through 1000 ℃ of one-level tempering 1h and 500 ℃ of second annealing 1h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
Adopt three-point bending test and SENB method to test respectively bending strength and the fracture toughness of not strengthening and strengthen magnet, result is as follows:
Embodiment 2:
1) main-phase alloy Nd
16dy
1fe
balga
0.3b
7adopt casting technique to make ingot casting, crystal-boundary phase alloy Nd
30dy
5fe
balni
3al
1nb
0.1b
6.5adopt rapid quenching technique to make rapid tempering belt, fast quenching speed is 18m/s;
2) main-phase alloy and crystal-boundary phase alloy are carried out to coarse crushing by hydrogen explosion is broken respectively, then under nitrogen protection, by ball milling, make respectively the powder that average particulate diameter is 2 μ m and 1 μ m;
3) by 10wt% graphene nanometer sheet powder with after crystal-boundary phase alloy powder resonance sound mixing 10min, add 6wt% stearic acid to carry out vacuum ball milling, it is dispersed in crystal-boundary phase alloy powder;
4), after the crystal-boundary phase alloy powder graphene nano of 3wt% being strengthened evenly mixes with main-phase alloy powder, in the magnetic field of 1.2T, be orientated die mould and make green compact;
5) by green compact 900 ℃ with 5MPa pressure under discharge plasma sintering 10min, then through 950 ℃ of one-level tempering 1.5h and 650 ℃ of second annealing 0.5h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
Adopt three-point bending test and SENB method to test respectively bending strength and the fracture toughness of not strengthening and strengthen magnet, result is as follows:
Embodiment 3:
1) main-phase alloy Nd
12pr
10fe
balco
0.5cu
0.5nb
0.1b
6adopt rapid hardening belt-rejecting technology to make rapid hardening strip, copper roller degree of turning is 1.6m/s, crystal-boundary phase alloy Nd
20dy
2ho
2fe
balmg
2ti
0.5b
5adopt rapid quenching technique to make rapid tempering belt, fast quenching speed is 18m/s;
2) main-phase alloy and crystal-boundary phase alloy are carried out to coarse crushing by Mechanical Crushing respectively, then under nitrogen protection, by airflow milling, make respectively the powder that average particulate diameter is 3.8 μ m and 3 μ m;
3) by 3wt% graphene nanometer sheet powder with after crystal-boundary phase alloy powder resonance sound mixing 5min, add 4wt% stearic acid to carry out vacuum ball milling, it is dispersed in crystal-boundary phase alloy powder;
4), after the crystal-boundary phase alloy powder graphene nano of 1wt% being strengthened evenly mixes with main-phase alloy powder, in the magnetic field of 1.8T, be orientated die mould and make green compact;
5) by green compact 850 ℃ with 40MPa pressure under discharge plasma sintering 20min, then through 900 ℃ of one-level tempering 2h and 600 ℃ of second annealing 0.5h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
Adopt three-point bending test and SENB method to test respectively bending strength and the fracture toughness of not strengthening and strengthen magnet, result is as follows:
Embodiment 4:
1) main-phase alloy Nd
14ho
1fe
balal
0.2mo
0.1b
6.5adopt casting technique to make ingot casting, crystal-boundary phase alloy Nd
25gd
3fe
balco
2ga
0.3si
0.5w
0.1b
6adopt rapid quenching technique to make rapid tempering belt, fast quenching speed is 16m/s;
2) main-phase alloy and crystal-boundary phase alloy are carried out to coarse crushing by hydrogen explosion is broken respectively, then under nitrogen protection, by airflow milling, make respectively the powder that average particulate diameter is 4.5 μ m and 4 μ m;
3) by 6wt% graphene nanometer sheet powder with after crystal-boundary phase alloy powder resonance sound mixing 7min, add 5wt% stearic acid to carry out vacuum ball milling, it is dispersed in crystal-boundary phase alloy powder;
4), after the crystal-boundary phase alloy powder graphene nano of 5wt% being strengthened evenly mixes with main-phase alloy powder, in the magnetic field of 1.6T, be orientated die mould and make green compact;
5) by green compact 800 ℃ with 30MPa pressure under discharge plasma sintering 5min, then through 1000 ℃ of one-level tempering 1h and 550 ℃ of second annealing 1h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
Adopt three-point bending test and SENB method to test respectively bending strength and the fracture toughness of not strengthening and strengthen magnet, result is as follows:
| Test magnet kind | Bending strength (MPa) | Fracture toughness (MPam 1/2) |
| Do not strengthen magnet | 288 | 2.90 |
| Strengthening magnet | 372 | 3.15 |
Claims (8)
1. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of crystal boundary, it is characterized in that, adopt the nano combined intensifying method of pairing Jin Jing circle to prepare high tough Sintered NdFeB magnet, two alloyages and nano combined reinforcement technique are organically combined, in crystal-boundary phase alloy magnetic, by resonance sound, mix with ball milling method and evenly introduce graphene nanometer sheet powder, form the crystal boundary composite construction that nanometer strengthens, improve the obdurability of Grain-Boundary Phase, suppress intercrystalline britftleness fracture, improve magnet obdurability; Concrete steps are:
A) main-phase alloy adopts casting method or rapid hardening to get rid of band method and makes ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts quick-quenching method to make rapid tempering belt;
B) by main-phase alloy and crystal-boundary phase alloy respectively by Mechanical Crushing or hydrogen explosion is broken carries out coarse crushing, coarse crushing is carried out fine grinding by ball milling or airflow milling, and making average particulate diameter is the main-phase alloy powder of 2-6 μ m and the crystal-boundary phase alloy powder of 1-5 μ m;
C) after graphene nanometer sheet powder is mixed with crystal-boundary phase alloy powder resonance sound, add dispersant to carry out vacuum or protective atmosphere ball milling, graphene nanometer sheet powder is dispersed in crystal-boundary phase alloy powder, obtains the crystal-boundary phase alloy powder that graphene nano strengthens;
D) by step C) after the crystal-boundary phase alloy powder that strengthens of the graphene nano that obtains evenly mixes with main-phase alloy powder, in the magnetic field of 1.2-2.0T, be orientated die mould and make green compact;
E) green compact are carried out to discharge plasma sintering, and through 900-1000 ℃ of one-level tempering 1-2h and 500-650 ℃ of second annealing 0.5-1h, make the high tough nano combined strengthening neodymium iron boron magnetic body of crystal boundary.
2. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described steps A) the atomic percent of main-phase alloy composition be Nd
xfe
100-x-y-zb
ym
z, 11≤x≤16 wherein, 5.5≤y≤7,0.1≤z≤10, M is one or more in Pr, Dy, Tb, Ho, Co, Ni, Al, Cu, Ga, Mg, Zn, Nb, Zr, Ti, Mo, W, V element.
3. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described steps A) the atomic percent of crystal-boundary phase alloy composition be Nd
afe
100-a-b-cb
br
c, 12≤a≤30 wherein, 5≤b≤7,0.1≤c≤20, R is one or more in Pr, Dy, Tb, Ho, Gd, Ce, Co, Ni, Al, Cu, Ga, Mg, Zn, Si, Nb, Zr, Ti, Mo, W, V element.
4. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described step C) the diameter of graphene nanometer sheet powder be distributed in 0.5-2 μ m, thickness distribution is at 0.6-1.2nm.
5. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described step C) crystal-boundary phase alloy powder in the addition of graphene nanometer sheet powder be 1-10wt%.
6. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described step C) resonance sound incorporation time be 2-10min.
7. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, is characterized in that described step C) dispersant be stearic acid, addition is 1-6wt%.
8. the preparation method of the nano combined strengthening neodymium iron boron magnetic body of a kind of crystal boundary according to claim 1, it is characterized in that, described step e) discharge plasma sintering parameter is: sintering temperature is 600-900 ℃, and sintering time is 5-30min, and pressure is 5-50MPa.
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Application publication date: 20140319 |