CN103187133A - Rare earth permanent magnetic alloy and magnetic phase composite preparation method thereof - Google Patents
Rare earth permanent magnetic alloy and magnetic phase composite preparation method thereof Download PDFInfo
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- CN103187133A CN103187133A CN2013100903282A CN201310090328A CN103187133A CN 103187133 A CN103187133 A CN 103187133A CN 2013100903282 A CN2013100903282 A CN 2013100903282A CN 201310090328 A CN201310090328 A CN 201310090328A CN 103187133 A CN103187133 A CN 103187133A
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Abstract
The invention relates to the technical field of a rare earth permanent magnetic material and relates to a magnetic phase composite rare earth permanent magnetic alloy and a preparation method thereof. The permanent magnetic alloy comprises the following chemical components in mass percentage: REaFe99-a-bB1Mb, wherein a is more than or equal to 28, but less than or equal to 32, b is more than 0, but less than or equal to 10, RE comprises at least two selected rare earth elements from La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu, and M is one or more from Co, AL, Cu, Ga, Nb, Mo, Ti, Zr and V. Magnetic phase composite preparation is performed on the permanent magnetic alloy by crushing, mixing, sintering and thermally treating at least two rapid hardening strips with different components, wherein the rapid hardening strips are at least two 2-14-1-type magnetic main phases (RE) 2Fe14B containing different rare earths respectively. Through mutual proportioning of different proportions of rapid hardening strips, a magnet containing designed components is prepared; the magnet comprises two or more 2-14-1-type magnetic phases consisting of different rare earths, including a 2-14-1-type magnetic phase consisting of a single rare earth; and good comprehensive magnetic property is obtained on the premise of reducing the heavy rare earth content.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, relate to a kind of RE permanent magnetic alloy and magnetic phase composite preparation process thereof.
Background technology
Nd-Fe-Bo permanent magnet material is widely used in high-tech sectors such as Aero-Space, information and new forms of energy, is one of important foundation material of modern industry.Rare earth element is the key of Nd-Fe-B series permanent magnetic material, and accounts for more than 80% of cost of material.Since the rare earth element resource-constrained, and demand progressively increases in recent years, and price escalates, therefore improve the magnetic property of rare earth permanent-magnetic material, reducing the consumption of rare earth consumption, especially heavy rare earth, is one of focus of our times various countries rare earth permanent magnet industry concern.
In recent years, the rare earth especially high materialization of heavy rare earth utilizes technology progressively to obtain paying close attention to and development, mode by initial compounds such as interpolation Dy, Tb is oozed the Dy technology to nearest crystal boundary diffusion, by improving rare earth element in the distribution of crystal boundary, reduce the content of heavy rare earth in principal phase, obtain high magnetic property, especially improve coercive force, realize the preparation of the low rare-earth Nd-Fe-B permanent magnetic material of high-performance.But Dy technical matters complexity, equipment cost height are oozed in diffusion, also are subjected to restrictions such as size, thermal deformation, and its capital equipment, technology and patent be that Japan has, and seriously limit this The Application of Technology and popularization.China's researcher is in the low high materialization utilization of heavy rare earth of research and substitute technology, resources characteristic according to China, the especially utilizations of light rare earth such as Ce, La of technology such as rare earth balanced use have been developed, in magnet, add low-cost rare earth elements such as part Ce, La, in conjunction with the technology such as high materialization utilization of rare earth element, keep magnet to have better comprehensive performance and rational cost advantage.
Summary of the invention
At the problems referred to above, the invention provides a kind of RE permanent magnetic alloy and magnetic phase composite preparation process thereof, the 2-14-1 type magnetic phase that they 2-14-1 type magnetic two or more different rare earth elements mutually that comprise that the single rare earth element is formed are formed, when reducing heavy rare earth content, obtained good comprehensive magnetic property.
For achieving the above object, the invention provides following technical scheme:
A kind of RE permanent magnetic alloy, wherein, the chemical composition of described permanent-magnet alloy is by mass percentage: RE
aFe
99-a-bB
1M
bWherein, 28≤a≤32,0<b≤10, RE is selected from least two kinds among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu, and M is one or more among Co, Al, Cu, Ga, Nb, Mo, Ti, Zr, the V;
Described permanent-magnet alloy carries out the mutually compound preparation of magnetic by the quick setting belt of at least 2 kinds of heterogeneities through fragmentation, mixing, sintering and heat treatment step, and described quick setting belt is respectively at least two kinds of 2-14-1 type magnetic principal phases (RE) that contain different rare earths
2Fe
14B.
In the described quick setting belt, the composition of first quick setting belt is the RE ' of single rare earth
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE ')
2Fe
14B; The composition of second quick setting belt is mishmetal (RE ', RE ")
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE ', RE ")
2Fe
14B.
Described quick setting belt further comprises the 3rd quick setting belt, and its composition is RE " '
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE " ')
2Fe
14B, RE " ' for can reducing the rare earth element of permanent-magnet alloy fusing point, for being selected from least a among La, Ce, Pr, Nd, Pm, Sm, the Eu.
RE comprises at least a light rare earth RE ' and at least a heavy rare earth RE ", described light rare earth RE ' is selected from La, Ce, Pr, Nd, Pm, Sm, Eu, heavy rare earth RE " be selected from Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
Described RE is Nd, Ce and Dy.
The magnetic property of described magnetic phase composite permanent-magnet alloy is as follows: remanent magnetism B
rBe 12~15kGs, HCJ H
CjBe 8~30kOe, maximum magnetic energy product (BH)
mBe 35~55MGOe.
A kind of magnetic phase composite preparation process of RE permanent magnetic alloy, wherein,
The chemical formula of this permanent-magnet alloy is by mass percentage: RE
aFe
99-a-bB
1M
bWherein, 28≤a≤32,0<b≤10, RE is selected from least two kinds among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu, and M is one or more among Co, Al, Cu, Ga, Nb, Mo, Ti, Zr, the V;
Its magnetic phase composite preparation process comprises the steps:
Step 1: prepare at least two kinds of different quick setting belt raw materials respectively according to the composition design: the composition of first quick setting belt is RE '
aFe
99-a-bB
1M
bThe composition of second quick setting belt is (RE ', RE ")
aFe
99-a-bB
1M
b
Step 2: with respectively melting of the raw material in the step 1, and make at least two kinds of different quick setting belts that thickness is 0.2~0.4mm respectively, its magnetic principal phase is respectively (RE ')
2Fe
14B and (RE ', RE ")
2Fe
14B;
Step 3: broken powder process; Prepared two or more rapid-hardening flake in the step 2 is respectively charged into carries out the hydrogen fragmentation in the hydrogen broken furnace, then, in the powder of dehydrogenation, add antioxidant, make the magnetic of particle mean size 2~5 μ m respectively through airflow milling;
Step 4: mixed-powder, oriented moulding; According to the composition designing requirement, at least two kinds of different powder are mixed according to different ratios, then with mixed magnetic oriented moulding in the Magnetic field press of 1~3T, to make density be 3~5g/cm carrying out isostatic cool pressing
3Blank;
Step 5: sintering and heat treatment; The sintering furnace of blank being put into high vacuum carries out sintering, and wherein, sintering temperature is 900 ℃~1100 ℃, is incubated 1~6 hour, then respectively 800~950 ℃ and 400~600 ℃ of heat treatment 2 hours.
In described step 2; at first raw material are put into rapid hardening stove crucible; under argon shield, carry out vacuum induction melting; after treating that raw material fully melts the formation alloy; keep 1400~1600 ℃ of temperature; alloy liquid is poured on the water-cooled copper roller that linear velocity is 1~5 meter per second, and preparation thickness is at least two kinds of different rapid-hardening flake of 0.2~0.4mm.
In the hydrogen shattering process in step 3, inhale hydrogen under room temperature 0.1~0.5MPa pressure, carry out dehydrogenation then and handle, desorption temperature is 500~600 ℃, 2~6 hours time.
Compared with prior art, beneficial effect of the present invention is:
(1) mixing of the made powder of the quick setting belt of the present invention by heterogeneity realizes having the compound of 2-14-1 type principal phase that different rare earth elements form, thereby obtains comprehensive magnetic property preferably in alloy;
(2) the present invention is by the adjustment to rapid-hardening flake middle rare earth element kind, quantity and ratio, kind and the distribution of the rare earth element in the control principal phase, by adjusting the content of heavy rare earth in the quick setting belt, and with the proportioning of the quick setting belt that does not contain heavy rare earth, can realize adjustment and optimization to heavy rare earth content and distribution in the magnet easily, realize the efficient utilization of heavy rare earth;
(3) the present invention is by adjusting kind and the content that has the different melting points rare earth element in the quick setting belt, can realize adjustment and control to the liquid phase fusing point, and then realization is to the adjusting of sintering temperature, especially the formation of low melting point rare earth element (light rare earth) and liquid phase thereof can obviously reduce sintering temperature, obtain lower optimal sintering temperature, thereby being lower than the temperature densified sintering product of conventional method, obtain less crystallite dimension, improve the coercive force of magnet;
(4) the present invention adopts 2~4 kinds of quick setting belts, according to different ratio combinations, substantially can realize the production of multiple trade mark magnet, and pass through the efficient utilization of heavy rare earth and reduce sintering temperature, reduce production costs, enhance productivity, and need not equipment just transformed and to realize large-scale production.
Description of drawings
Fig. 1 is the Nd that has of first embodiment
2Fe
14B and (Nd, Dy)
2Fe
14The SEM pattern of the RE permanent magnetic alloy of two kinds of magnetic phases of B;
Fig. 2 is the (Nd of second embodiment
0.8Ce
0.2)
30Fe
BalB
1The density of magnet is with the variation of sintering temperature;
Fig. 3 is the second embodiment low temperature sintering (Nd
0.8Ce
0.2)
30Fe
BalB
1The fracture surface SEM pattern of magnet;
Fig. 4 is RE of the present invention
aFe
99-a-bB
1M
bThe magnetic phase distribution schematic diagram of magnetic phase built-up magnet.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated, to explain the present invention better.But it should be noted that following examples only for the purpose of illustration, protection scope of the present invention is not limited to following examples.
The chemical formula of magnetic phase composite permanent-magnet alloy of the present invention is by mass percentage: RE
aFe
99-a-bB
1M
bWherein, 28≤a≤32,0<b≤10, RE is selected from least two kinds among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu, and M is one or more among Co, Al, Cu, Ga, Nb, Mo, Ti, Zr, the V; Described magnetic phase composite permanent-magnet alloy comprises (RE
1)
2Fe
14B is at interior at least two kinds of 2-14-1 type magnetic principal phases, wherein RE
1A kind of among the described RE.
Wherein, Fig. 4 is magnetic phase composite permanent-magnet alloy RE of the present invention
aFe
99-a-bB
1M
bMagnetic phase distribution schematic diagram, as can be seen from the figure, magnet of the present invention namely comprises the single rare earth elements RE
1(the RE that forms
1)
2Fe
14B magnetic phase also comprises RE
1Mix (the RE that forms with other rare earth elements
1, RE
2, RE
3)
2Fe
14B magnetic phase, and RE
1(the RE that one or more rare earth elements of in addition other are formed
4, RE
5, RE
6)
2Fe
14B magnetic phase.Wherein, RE
1, RE
2, RE
3, RE
4, RE
5, RE
6Be selected from a kind of among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu.
Embodiment 1
Adopt method of the present invention to prepare chemical composition and be (Nd
0.9Dy
0.1)
30Fe
BalB
1Have composite magnetic phase RE permanent magnetic alloy, wherein bal is surplus, and the mass percent of heavy rare earth Dy is 3%.
Step 1: respectively according to mass percent Nd
30Fe
BalB
1(Nd
0.8Dy
0.2)
30Fe
BalB
1The difference preparation raw material.
Step 2: with confected materials respectively melting prepare quick setting belt.At first raw material are put into rapid hardening stove crucible; under argon shield, carry out vacuum induction melting, treat raw material fully melt form alloy after, keep 1500 ℃ of temperature; alloy liquid is poured on the water-cooled copper roller that linear velocity is 3 meter per seconds, and preparation thickness is two kinds of rapid-hardening flake of 0.3mm.
Step 3: broken powder process: the Nd that makes in institute's step 2
30Fe
BalB
1(Nd
0.8Dy
0.2)
30Fe
BalB
1Rapid-hardening flake is respectively charged into carries out the hydrogen fragmentation in the hydrogen broken furnace, inhale hydrogen under room temperature 0.2MPa pressure, carries out dehydrogenation then and handles, and desorption temperature is 600 ℃, 6 hours time.The powder of dehydrogenation is added antioxidant, make the magnetic of particle mean size 3 μ m respectively through airflow milling.
Step 4: according to mass ratio 1:1 ratio with Nd
30Fe
BalB
1(Nd
0.8Dy
0.2)
30Fe
BalB
1Powder evenly mixes, and its actual constituent is (Nd
0.9Dy
0.1)
30Fe
BalB
1Then, will mix magnetic oriented moulding in the Magnetic field press of 2T, and make blank carrying out isostatic cool pressing, its density is 4g/cm
3
Step 5: sintering and heat treatment: the sintering furnace of blank being put into high vacuum carries out sintering, and sintering temperature is 900 ℃~1100 ℃, is incubated 4 hours, then respectively 800~950 ℃ and 400~600 ℃ of heat treatment 2 hours.
Adopt scanning electron microscopy (SEM) to observe the heterogeneous microstructure of present embodiment magnet, typical SEM pattern as shown in Figure 1.As can be seen, the crystal grain in the magnet is made up of two kinds of crystal grain with different contrasts.Because the atomic weight of Dy is that the atomic weight of 162.50, Nd is 144.24, therefore, the crystal grain that contains Dy has higher brightness at SEM in mutually, is light grey in SEM, and the crystal grain that does not contain Dy then is Dark grey.Simultaneously, the energy spectrum analysis that obtains from scanning electron microscopy shows: the Dy quality percentage composition of light gray areas is about 5~7%, approaches with Dy content in the quick setting belt that designs.Therefore, adopt method of the present invention to prepare to have the hybrid magnet of the magnetic phase of different rare earth kinds, content, thereby realize the efficient utilization of heavy rare earth.
Embodiment 2
It is (Nd that low-temperature sintering prepares design mix
0.8Ce
0.2)
30Fe
BalB
1Magnet, wherein rare earth Nd quality percentage composition is that the quality percentage composition of 24%, Ce is 6%, total rare earth content is 30%.
Step 1: respectively according to mass percent Nd
30Fe
BalB
1(Nd
0.7Ce
0.3)
30Fe
BalB
1The difference preparation raw material.
Step 2: with confected materials respectively melting prepare quick setting belt.At first raw material are put into rapid hardening stove crucible; under argon shield, carry out vacuum induction melting, treat raw material fully melt form alloy after, keep 1400 ℃ of temperature; alloy liquid is poured on the water-cooled copper roller that linear velocity is 3 meter per seconds, and preparation thickness is two kinds of rapid-hardening flake of 0.3mm.
Step 3: broken powder process: prepared Nd
30Fe
BalB
1(Nd
0.7Ce
0.3)
30Fe
BalB
1Rapid-hardening flake is respectively charged into carries out the hydrogen fragmentation in the hydrogen broken furnace, inhale hydrogen under room temperature 0.2MPa pressure, carries out dehydrogenation then and handles, and desorption temperature is 600 ℃, 6 hours time.The powder of dehydrogenation is added antioxidant, make the magnetic of particle mean size 3 μ m respectively through airflow milling.
Step 4: according to mass ratio 1:2 ratio with Nd
30Fe
BalB
1(Nd
0.7Ce
0.3)
30Fe
BalB
1Powder evenly mixes, and its actual constituent is (Nd
0.8Ce
0.2)
30Fe
BalB
1To mix magnetic oriented moulding in the Magnetic field press of 2T, and make blank carrying out isostatic cool pressing, its density is 4g/cm
3
Step 5: sintering and heat treatment: the sintering furnace of blank being put into high vacuum carries out sintering, and sintering temperature is 1020 ℃, is incubated 2 hours, then respectively 800~900 ℃ and 400~600 ℃ of heat treatment 2 hours.
Adopt NIM-2000HF rare earth permanent magnet standard measuring equipment to survey the magnetic property of magnet, performance such as table 1.
Table 1 present embodiment (Nd
0.8Ce
0.2)
30Fe
BalB
1The performance of magnet
Fig. 2 is present embodiment (Nd
0.8Ce
0.2)
30Fe
BalB
1The situation that the density of magnet changes with sintering temperature.As can be seen, when sintering temperature reached 1020 ℃, the density of sintered magnet all can reach 7.62g/cm
3More than.And for the Nd of same powder granularity
30Fe
BalB
1The optimal sintering temperature of magnet is between 1050~1060 ℃.The analysis showed that: adopted (Nd just because of this method
0.7Ce
0.3)
30Fe
BalB
1Quick setting belt and powder because the fusing point of Ce is 798 ℃, than low 218 ℃ approximately of the fusing points of neodymium metal, reduce the fusing point of the liquid phase in the magnet, therefore can obtain the higher magnet of density at lower temperature sintering.Because sintering temperature is lower, is conducive to suppress grain growth, thereby has obtained higher coercive force in addition.Fig. 3 is present embodiment (Nd
0.8Ce
0.2)
30Fe
BalB
1The SEM pattern of the fracture surface of magnet, as can be seen, the crystal grain of magnet is 3~4 μ m, and distribution of sizes is very even, is significantly less than the crystallite dimension of commercial magnet 6~10 μ m.As shown in table 1, the prepared composition of present embodiment is (Nd
0.8Ce
0.2)
30Fe
BalB
1The remanent magnetism B of magnet
rBe 13.71kGs, HCJ H
CjBe 12.03kOe, maximum magnetic energy product (BH)
mBeing 45MGOe, having excellent comprehensive performances, is the peak of reporting at present.And because the alternative of Ce reaches 20%, can reduce the cost of raw material significantly, have the good application development prospect.
Claims (9)
1. RE permanent magnetic alloy, it is characterized in that: the chemical composition of described permanent-magnet alloy is by mass percentage: RE
aFe
99-a-bB
1M
bWherein, 28≤a≤32,0<b≤10, RE is selected from least two kinds among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu, and M is one or more among Co, Al, Cu, Ga, Nb, Mo, Ti, Zr, the V;
Described permanent-magnet alloy carries out the mutually compound preparation of magnetic by the quick setting belt of at least 2 kinds of heterogeneities through fragmentation, mixing, sintering and heat treatment step, and described quick setting belt is respectively at least two kinds of 2-14-1 type magnetic principal phases (RE) that contain different rare earths
2Fe
14B.
2. RE permanent magnetic alloy as claimed in claim 1, it is characterized in that: in the described quick setting belt, the composition of first quick setting belt is the RE ' of single rare earth
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE ')
2Fe
14B; The composition of second quick setting belt is mishmetal (RE ', RE ")
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE ', RE ")
2Fe
14B.
3. RE permanent magnetic alloy as claimed in claim 1, it is characterized in that: described quick setting belt further comprises the 3rd quick setting belt, its composition is RE " '
aFe
99-a-bB
1M
b, the magnetic principal phase is (RE " ')
2Fe
14B, RE " ' for can reducing the rare earth element of permanent-magnet alloy fusing point, for being selected from least a among La, Ce, Pr, Nd, Pm, Sm, the Eu.
4. RE permanent magnetic alloy as claimed in claim 1, it is characterized in that: RE comprises at least a light rare earth RE ' and at least a heavy rare earth RE "; described light rare earth RE ' is selected from La, Ce, Pr, Nd, Pm, Sm, Eu, heavy rare earth RE " be selected from Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
5. RE permanent magnetic alloy as claimed in claim 4, it is characterized in that: described RE is Nd, Ce and Dy.
6. RE permanent magnetic alloy as claimed in claim 1, it is characterized in that: the magnetic property of described magnetic phase composite permanent-magnet alloy is as follows: remanent magnetism B
rBe 12~15kGs, HCJ H
CjBe 8~30kOe, maximum magnetic energy product (BH)
mBe 35~55MGOe.
7. the magnetic phase composite preparation process of a RE permanent magnetic alloy as claimed in claim 1 is characterized in that:
The chemical formula of this permanent-magnet alloy is by mass percentage: RE
aFe
99-a-bB
1M
bWherein, 28≤a≤32,0<b≤10, RE is selected from least two kinds among rare-earth elements La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, the Lu, and M is one or more among Co, Al, Cu, Ga, Nb, Mo, Ti, Zr, the V;
Its magnetic phase composite preparation process comprises the steps:
Step 1: prepare at least two kinds of different quick setting belt raw materials respectively according to the composition design: the composition of first quick setting belt is RE '
aFe
99-a-bB
1M
bThe composition of second quick setting belt is (RE ', RE ")
aFe
99-a-bB
1M
b
Step 2: with respectively melting of the raw material in the step 1, and make at least two kinds of different quick setting belts that thickness is 0.2~0.4mm respectively, its magnetic principal phase is respectively (RE ')
2Fe
14B and (RE ', RE ")
2Fe
14B;
Step 3: broken powder process; Prepared two or more rapid-hardening flake in the step 2 is respectively charged into carries out the hydrogen fragmentation in the hydrogen broken furnace, then, in the powder of dehydrogenation, add antioxidant, make the magnetic of particle mean size 2~5 μ m respectively through airflow milling;
Step 4: mixed-powder, oriented moulding; According to the composition designing requirement, at least two kinds of different powder are mixed according to different ratios, then with mixed magnetic oriented moulding in the Magnetic field press of 1~3T, to make density be 3~5g/cm carrying out isostatic cool pressing
3Blank;
Step 5: sintering and heat treatment; The sintering furnace of blank being put into high vacuum carries out sintering, and wherein, sintering temperature is 900 ℃~1100 ℃, is incubated 1~6 hour, then respectively 800~950 ℃ and 400~600 ℃ of heat treatment 2 hours.
8. preparation method as claimed in claim 7; it is characterized in that: in described step 2; at first raw material are put into rapid hardening stove crucible; under argon shield, carry out vacuum induction melting; after treating that raw material fully melts the formation alloy; keep 1400~1600 ℃ of temperature, alloy liquid is poured on the water-cooled copper roller that linear velocity is 1~5 meter per second, preparation thickness is at least two kinds of different rapid-hardening flake of 0.2~0.4mm.
9. preparation method as claimed in claim 7 is characterized in that: in the hydrogen shattering process in step 3, inhale hydrogen under room temperature 0.1~0.5MPa pressure, carry out dehydrogenation then and handle, desorption temperature is 500~600 ℃, 2~6 hours time.
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