CN103903824A - Rare earth permanent magnetic material and preparation method thereof - Google Patents
Rare earth permanent magnetic material and preparation method thereof Download PDFInfo
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- CN103903824A CN103903824A CN201210578663.2A CN201210578663A CN103903824A CN 103903824 A CN103903824 A CN 103903824A CN 201210578663 A CN201210578663 A CN 201210578663A CN 103903824 A CN103903824 A CN 103903824A
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Abstract
The invention discloses a rare earth permanent magnetic material which comprises a main phase and an auxiliary phase. The rare earth permanent magnetic material is characterized in that the main phase constitutes R1xR2yFe100-x-y-z-uCozBu, the auxiliary phase constitutes R1aR2bFe100-a-b-c-n-vCocBnMv, total mass of the main phase and the auxiliary phase serves as a reference, and the mass content of the auxiliary phase is larger than 0 and smaller than or equal to 20%. The invention further provides a preparation method of the rare earth permanent magnetic material and the rare earth permanent magnetic material prepared in the method. The rare earth permanent magnetic material has high coercivity and a low temperature coefficient under the condition that loss of residual magnetism is little, effectively raises work temperature, obviously reduces content of arrowhead and / or terbium and reduces production cost of the permanent magnetic material.
Description
Technical field
The present invention relates to a kind of rare earth permanent-magnetic material, the preparation method of this rare earth permanent-magnetic material, and the rare earth permanent-magnetic material of being prepared by the method.
Background technology
Sintered NdFeB permanent magnets, compared with other types permanent magnetic material, has magnetic property high, and the low outstanding advantages that waits of price, makes its development and application obtain unconventional development.Its comprehensive magnetic can reach higher level at present, and application has related to the every field of national economy.
But current new forms of energy and environmental protection are concerned and become the trend of inevitable development day by day, used permanent magnetic material have also been proposed to the requirement of high-coercive force and high remanent magnetism.High-coercive force magnet needs dysprosium and/or the terbium element of more cost costliness, but the magnet that adds more these two kinds of elements cannot meet again the demand of high remanent magnetism preferably, is unfavorable for motor lightweight and high-power and utilize efficiently electric energy and wind energy.
CN102534358A discloses a kind of manufacture method of high-coercivity R-Fe-B sintered permanent magnet material, it is characterized in that, said method comprising the steps of: step 1, raw material are prepared in proportion, in the Strip casting stove of 200-700Kg/ time, melt, and being cast into alloy sheet with the roller speed of 1m/s-10m/s, its alloy sheet thickness is 0.1-0.4mm; Step 2, enters hydrogen by prepared alloy sheet in step 1 and processes in stove and carry out hydrogen pulverizing, and at the temperature of 400-600 ℃ dehydrogenation to hydrogen pressure <10Pa; In the oxygen-free environment under inert gas shielding, the alloy sheet after broken hydrogen is sent into middle grinding machine and be crushed to granularity <0.5mm, then carry out Crushing of Ultrafine through airflow milling, the classified Nd Fe B alloys powder of making particle diameter d=2-4um; Step 3, in the oxygen-free environment under inert gas shielding, at least one that particle diameter is less than in the nano oxidized dysprosium of 100nm, nano oxidized terbium, nano oxidized holmium joins in the Nd Fe B alloys powder preparing, and its adding proportion is the 1-3% of NdFeB alloy powder weight, and mixes; Step 4, in the oxygen-free environment under inert gas shielding, the powder mixing in step 3 is through the magnetic field orientating of 1.5-3T and be pressed into pressed compact; Step 5; in the oxygen-free environment under inert gas shielding; prepared pressed compact in step 4 is sent in vacuum sintering furnace; carry out 600-700 ℃ × 2-4hr once sintered; then carry out double sintering, the rapid cooling of 800-900 ℃ × 2-4hr; carry out again three high temperature sinterings, the rapid cooling of 1000-1100 ℃ × 1-2hr, finally carry out successively the Ageing Treatment of 850-950 ℃ × 1-6hr and 450-600 ℃ × 1-6hr, make the high-temperature resisting R-Fe-B agglomeration permanent magnetic material of high-coercive force.The remanent magnetism of permanent magnetic material prepared by the method is 13.6-14.5(kGs), coercive force is 14.5-18(kOe).
Also there is very large gap apart from coercitive theoretical boundary 80kOe in the coercive force of the permanent magnetic material making at present, and the content of the raising needed dysprosium of coercive force and/or terbium is still higher.In addition, improve the coercitive while of permanent magnetic material, remanent magnetism will inevitably reduce, how when the decline of assurance remanent magnetism is lower, to improve coercive force (, guarantee high-coercive force and high remanent magnetism simultaneously), reduce again the use amount of dysprosium and/or terbium, become the focus of current research.
Summary of the invention
The object of the invention is to solve the permanent magnetic material existing in prior art and cannot obtain higher coercivity, lower temperature coefficient and higher working temperature simultaneously, and the higher technical problem of the use amount of dysprosium and/or terbium, a kind of have higher coercivity, lower temperature coefficient and higher working temperature are provided, the lower rare earth permanent-magnetic material of use amount of dysprosium and/or terbium, and the preparation method of this rare earth permanent-magnetic material and the rare earth permanent-magnetic material prepared by the method.
The present inventor notices that magnet only adopts the rare earth element of Pr and/or Nd composition, on substantive characteristics, be difficult to obtain the magnet such as the high-coercive force such as electric motor of automobile, wind-driven generator and adaptation elevated operating temperature, therefore need to there is heavy rare earth Dy and/or the Tb of certain content in principal phase, to improve coercive force, but the existence of Dy and/or Tb inevitably causes the reduction of remanent magnetism and the increase of cost.
But, the present inventor finds that by many experiments the principal phase cooperation with definite composition and content has definite composition and content and Dy and/or the higher auxiliary phase of Tb content finally, effectively reduce the loss of the magnetic flux density of final magnet, under the condition of lower magnetic strength loss, obtain high coercive force.Although auxiliary middle Dy mutually and/or Tb content are higher, but due to the amount of the auxiliary phase of adding in rare earth permanent-magnetic material less in the situation that with regard to obtainable good effect, so, compared with prior art, still can be at Dy and/or Tb content lower in the situation that, under the condition of lower magnetic strength loss, obtain high coercive force, lower temperature coefficient and higher working temperature.In addition, when the performance of the rare earth permanent-magnetic material providing when rare earth permanent-magnetic material provided by the invention and prior art is close, the dysprosium of rare earth permanent-magnetic material provided by the invention and/or the content of terbium are obviously lower with respect to existing rare earth permanent-magnetic material.
To achieve these goals, the invention provides a kind of rare earth permanent-magnetic material, this material comprises principal phase and auxiliary phase, wherein, and the consisting of of described principal phase: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%; Consisting of of described auxiliary phase: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%; Take the gross mass of described principal phase and auxiliary phase as benchmark, the mass content of described auxiliary phase is greater than 0 and be less than or equal to 20%.
The present invention also provides a kind of preparation method of rare earth permanent-magnetic material, and the method comprises carries out mixed-forming, sintering and tempering successively to main-phase alloy raw material and auxiliary phase alloy raw material, wherein, and the consisting of of described main-phase alloy raw material: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%; Consisting of of described auxiliary phase alloy raw material: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%; With respect to the described main-phase alloy raw material of 100 weight portions and total consumption of described auxiliary phase alloy raw material, the consumption of described auxiliary phase alloy raw material is greater than 0 weight portion and is less than or equal to 20 weight portions.
The present invention also provides the rare earth permanent-magnetic material of being prepared by said method.
Compared with prior art, rare earth permanent-magnetic material provided by the invention guarantee remanent magnetism reduce there is higher coercive force little in the situation that, lower temperature coefficient and higher working temperature, and reduced the consumption of dysprosium and/or terbium.
Other features and advantages of the present invention are described in detail the embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides a kind of rare earth permanent-magnetic material, this material comprises principal phase and auxiliary phase, wherein, and the consisting of of described principal phase: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%; Consisting of of described auxiliary phase: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%; Take the gross mass of described principal phase and auxiliary phase as benchmark, the mass content of described auxiliary phase is greater than 0 and be less than or equal to 20%.
According to rare earth permanent-magnetic material provided by the invention, under preferable case, in the composition of described principal phase, the mass percent of x, y, z, u is: 28%≤x+y≤32%, 1.5%≤y≤4%, 1%≤z≤2.5%, 0.9%≤u≤1.1%.In the time that the composition of described principal phase is in above-mentioned scope, be more conducive to reduce little in the situation that at remanent magnetism, obtain there is higher coercive force, the rare earth permanent-magnetic material of lower temperature coefficient and higher working temperature.
According to rare earth permanent-magnetic material provided by the invention, under preferable case, in the composition of described auxiliary phase, the mass percent of a, b, c, n, v is: 38%≤a+b≤67%, 10%≤b≤25%, 0%≤c≤17%, 0%≤n≤1%, 8%≤v≤28%.In the time that the composition of described auxiliary phase is in above-mentioned scope, be more conducive to reduce little in the situation that at remanent magnetism, obtain there is higher coercive force, the rare earth permanent-magnetic material of lower temperature coefficient and higher working temperature.
According to rare earth permanent-magnetic material provided by the invention, under preferable case, take the gross mass of described principal phase and auxiliary phase as benchmark, the mass content of described auxiliary phase is greater than 0 and be less than or equal to 15%, for example can be for being greater than 1% and be less than or equal to 15%.In the time that the auxiliary phase mass content of rare earth permanent-magnetic material is in above-mentioned scope, be more conducive to realize object of the present invention.
The invention provides a kind of preparation method of rare earth permanent-magnetic material, the method comprises carries out mixed-forming, sintering and tempering successively to main-phase alloy raw material and auxiliary phase alloy raw material, wherein, and the consisting of of described main-phase alloy raw material: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%; Consisting of of described auxiliary phase alloy raw material: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%; With respect to the described main-phase alloy raw material of 100 weight portions and total consumption of described auxiliary phase alloy raw material, the consumption of described auxiliary phase alloy raw material is greater than 0 weight portion and is less than or equal to 20 weight portions.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, under preferable case, in the composition of described main-phase alloy raw material, the mass percent of x, y, z, u is: 28%≤x+y≤32%, 1.5%≤y≤4%, 1%≤z≤2.5%, 0.9%≤u≤1.1%.In the time that the composition of described main-phase alloy raw material is in above-mentioned scope, adopt the method to be more conducive to reduce little in the situation that at remanent magnetism, prepare there is higher coercive force, the rare earth permanent-magnetic material of lower temperature coefficient and higher working temperature.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, under preferable case, in the composition of described auxiliary phase alloy raw material, the mass percent of a, b, c, n, v is: 38%≤a+b≤67%, 10%≤b≤25%, 0%≤c≤17%, 0%≤n≤1%, 8%≤v≤28%.In the time that the composition of described auxiliary phase alloy raw material is in above-mentioned scope, adopt the method to be more conducive to reduce little in the situation that at remanent magnetism, prepare there is higher coercive force, the rare earth permanent-magnetic material of lower temperature coefficient and higher working temperature.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, under preferable case, with respect to the described main-phase alloy raw material of 100 weight portions and auxiliary phase alloy raw material total consumption, the consumption of described auxiliary phase alloy raw material is greater than 0 weight portion and is less than or equal to 15 weight portions, for example can be for being greater than 1 weight portion and being less than or equal to 15 weight portions.In the time adopting the auxiliary phase mass content of rare earth permanent-magnetic material in above-mentioned scope, be more conducive to realize object of the present invention.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, adopt two alloyages (main-phase alloy raw material and auxiliary phase alloy raw material to be carried out respectively to melting, the final rare earth permanent-magnetic material forming) and single alloyage (be a kind of alloying component, carry out melting, in the material obtaining, containing two kinds of things is principal phase and auxiliary phase mutually) prepare rare earth permanent-magnetic material and all can realize object of the present invention.
In the time that the present invention adopts single alloyage to prepare rare earth permanent-magnetic material, a kind of alloy of composition is carried out to melting, obtain ingot casting or the rapid hardening thin slice of this alloy raw material, the ingot casting of alloy raw material or rapid hardening thin slice are carried out to fragmentation, powder process, then carry out moulding.
In the time that the present invention adopts pairing gold legal system for rare earth permanent-magnetic material, main-phase alloy raw material and auxiliary phase alloy raw material are carried out respectively to melting, obtain the ingot casting of main-phase alloy raw material or ingot casting or the rapid hardening thin slice of rapid hardening thin slice and auxiliary phase alloy raw material, ingot casting or the rapid hardening thin slice of the ingot casting to main-phase alloy raw material or rapid hardening thin slice and auxiliary phase alloy raw material mixes, the order of fragmentation and powder process does not have special requirement, can first mix, more broken, powder process; Also first fragmentation, mixing, powder process; First broken, powder process, then mix; Then the fine powder of the main-phase alloy raw material making and auxiliary phase alloy raw material is carried out to moulding.
Under preferable case, the present invention adopts pairing gold legal system for rare earth permanent-magnetic material.,, before main-phase alloy raw material and auxiliary phase alloy raw material are carried out to moulding, respectively main-phase alloy raw material and auxiliary phase alloy raw material are carried out to melting.The present inventor finds to adopt the standby rare earth permanent-magnetic material of pairing gold legal system more excellent than the performance of the rare earth permanent-magnetic material that adopts single alloyage to prepare.This may be because auxiliary phase alloy raw material reacts and obtains the principal phase of high anisotropy field and form rich rare-earth phase at crystal boundary, and the trace element in auxiliary phase alloy raw material can well improve microstructure at crystal boundary simultaneously.In addition because auxiliary phase alloy raw material adds separately, therefore avoided Dy in auxiliary phase alloy raw material and/or Tb and trace element to enter principal phase completely, but be positioned at epitaxial loayer and the crystal boundary of principal phase.Therefore, compared with rare earth permanent-magnetic material prepared by standby rare earth permanent-magnetic material single alloyage close with performance of pairing gold legal system, obviously reduce Dy and/or Tb content.
The method of described melting is method of smelting conventional in this area, and the alloy of acquisition is ingot casting or gets rid of band forms.Smelting temperature is 1200-1500 ℃, and smelting time is 20min-1h.
The method of described fragmentation is the breaking method of various routines in this area, as long as can, by fully broken to the ingot casting of the ingot casting of main-phase alloy raw material or rapid hardening thin slice, auxiliary phase alloy raw material or rapid hardening thin slice, preferably adopt the broken method of hydrogen.The condition that the broken condition of hydrogen also can be known in the art, preferably by ingot casting or rapid hardening thin slice under 0.02-1.5Mpa hydrogen pressure, inhale hydrogen 0.1-5h normal temperature (20 ± 5 ℃) is lower, and at 300-650 ℃ of dehydrogenase 12-10h, obtain hydrogen flour.
The method of described powder process is the milling method of various routines in this area, as long as hydrogen flour can be made to the fine powder of target grain size, preferably adopts airflow milling method, is carrying out adding antioxidant before airflow milling.Described antioxidant can be neodymium iron boron special antioxidant arbitrarily, for example, can be purchased from Beijing Jun Cefeng development in science and technology Co., Ltd the neodymium iron boron special antioxidant that the trade mark is KM-01.Take the total weight of hydrogen flour as benchmark, the addition of described antioxidant is 0.02-0.15 % by weight.By airflow milling, hydrogen flour is made to the fine powder that average grain diameter is 1.0-4.5 μ m, (in the time adopting two alloyage, preferably the average grain diameter of the fine powder of main-phase alloy raw material be 2.5-4.5 μ m).
Under preferable case, in the fine powder obtaining, add lubricant after powder process, described lubricant is preferably one or more in gasoline, oleic acid, stearic acid, polyethylene glycol, anhydro sorbitol and tristerin.Take the weight of fine powder as benchmark, the addition of described lubricant is 0.02-0.15 % by weight.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, the method of described moulding can adopt method conventional in this area, under preferable case, described in be molded over and in the permanent magnetic field of 1.5-4T or pulsed magnetic field, be orientated compressingly, and keep 30-120s through static pressure such as 170-220MPa.
According to the preparation method of rare earth permanent-magnetic material provided by the invention, the condition of described sintering and the step of tempering can be well known by persons skilled in the art any one, under preferable case, the condition of described sintering is: sintering temperature is 1040-1120 ℃, and sintering time is 3-8 hour; The step of described tempering is: first carry out one-level tempering at 860-940 ℃, and keep 1-5h, then carry out second annealing at 470-560 ℃, and keep 1-8h.
The present invention also provides the rare earth permanent-magnetic material being prepared by the preparation method of above-mentioned rare earth permanent-magnetic material.
Below will describe the present invention by embodiment.
In following examples, according to GB/T 3217-1992 testing standard, at 22 ℃, adopt remanent magnetism (Br), coercive force (Hcj), maximum magnetic energy product ((BH) max), maximum operating temperature and the β temperature coefficient of the Chinese science metering NIM-10000H of institute test (or test and calculate) rare earth permanent-magnetic material;
Wherein β temperature coefficient calculates by following formula:
Wherein, β (Hcj): HCJ temperature coefficient, %/℃;
T
1: basal temperature, ℃; T
2: the ceiling temperature of variations in temperature, ℃;
Hcj(T
1): temperature T
1time HCJ, kA/m;
Hcj(T
2): temperature T
2time HCJ, kA/m.
Embodiment 1
To fill a prescription as Pr
5nd
23dy
3tb
0.5fe
66.5co
1b
1raw material get rid of tape handling with the copper roller linear resonance surface velocity of 1.8m/s, prepare and get rid of strap, as main-phase alloy raw material.Described main-phase alloy raw material, under 0.15Mpa hydrogen pressure, is inhaled to hydrogen 2h at 15 ℃, then dehydrogenation 6h at 560 ℃, thus make the hydrogen flour of main-phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described main-phase alloy raw material of 100 weight portions and 0.05 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the main-phase alloy raw material fine powder of 3.2um, then the main-phase alloy raw material fine powder obtaining is mixed with the gasoline of 0.03 weight portion of the main-phase alloy raw material fine powder in 100 weight portions, obtain principal phase presoma.
To fill a prescription as Pr
9.6nd
29.3dy
10fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7raw material under 1300 ℃, the condition of 25min, carry out melting ingot casting, prepare ingot casting, as auxiliary phase alloy raw material.Described auxiliary phase alloy raw material, under 0.15Mpa hydrogen pressure, is inhaled to hydrogen 2h at 15 ℃, then dehydrogenation 6h at 560 ℃, thus make the hydrogen flour of auxiliary phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described auxiliary phase alloy raw material of 100 weight portions and 0.05 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the auxiliary phase alloy raw material fine powder of 3um, then the auxiliary phase alloy raw material fine powder obtaining is mixed with the gasoline of 0.03 weight portion of the auxiliary phase alloy raw material fine powder in 100 weight portions, obtain auxiliary phase presoma.
Above-mentioned principal phase presoma and auxiliary phase presoma are evenly mixed, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 1.5 weight portions.The moulding in the permanent magnetic field of 2T by the principal phase presoma mixing and auxiliary phase presoma, then keep 70s through static pressure such as 190MPa, then at 1090 ℃ of sintering 5h, and carry out one-level tempering at 920 ℃, keep 1.5h; Then carry out second annealing at 480 ℃, keep 3.5h.Final acquisition rare earth permanent-magnetic material of the present invention.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Comparative example 1
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, do not add auxiliary phase alloy raw material.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 2
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 3.5 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 3
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 5 weight portions.Always consisting of of main-phase alloy raw material and auxiliary phase alloy raw material: Pr
5.23nd
23.315dy
3.35tb
0.475fe
63.95co
1.775b
0.998al
0.275cu
0.16zr
0.12ga
0.35.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 4
Adopt trace element (being Co, B, Al, Cu, Zr, the Ga) content of embodiment 3, and adjust the content of rare earth and iron, adopt preparation method's (being equivalent to single alloy preparation method) that main-phase alloy raw material can be prepared into rare earth permanent-magnetic material in embodiment 1, make the performance of the performance of the rare earth permanent-magnetic material making and the rare earth permanent-magnetic material of embodiment 3 close.Consisting of of raw material: Pr
4.5nd
22dy
5.35tb
0.475fe
64co
1.775b
1al
0.275cu
0.16zr
0.12ga
0.35.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 5
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 8 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 6
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 15 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Embodiment 7
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 18 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Comparative example 2
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, the Dy in auxiliary phase alloy raw material is all replaced with to Pr and Nd composition, auxiliary phase alloy raw material is Pr
12.1nd
36.8fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Comparative example 3
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, the Dy in auxiliary phase alloy raw material is all replaced with to Pr and Nd composition, auxiliary phase alloy raw material is Pr
12.1nd
36.8fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 3.5 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Comparative example 4
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, the Dy in auxiliary phase alloy raw material is all replaced with to Pr and Nd composition, auxiliary phase alloy raw material is Pr
12.1nd
36.8fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 5 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 1.
Table 1
Embodiment 8
To fill a prescription as Pr
7nd
21dy
3.7tb
0.3fe
65.6co
1.5b
0.9raw material get rid of tape handling with the copper roller linear resonance surface velocity of 1.8m/s, prepare and get rid of strap, as main-phase alloy raw material.Described main-phase alloy raw material, under 0.2Mpa hydrogen pressure, is inhaled to hydrogen 2.5h at 20 ℃, then dehydrogenase 35 .5h at 550 ℃, thus make the hydrogen flour of main-phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described main-phase alloy raw material of 100 weight portions and 0.04 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the main-phase alloy raw material fine powder of 3.5um, then the main-phase alloy raw material fine powder obtaining is mixed with the oleic acid of 0.02 weight portion of the main-phase alloy raw material fine powder in 100 weight portions, obtain principal phase presoma.
To fill a prescription as Pr
9.6nd
29.3dy
10fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7raw material under 1300 ℃, the condition of 25min, carry out melting ingot casting, prepare ingot casting, as auxiliary phase alloy raw material.Described auxiliary phase alloy raw material, under 0.2Mpa hydrogen pressure, is inhaled to hydrogen 2.5h at 20 ℃, then dehydrogenase 35 .5h at 550 ℃, thus make the hydrogen flour of auxiliary phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described auxiliary phase alloy raw material of 100 weight portions and 0.04 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the auxiliary phase alloy raw material fine powder of 3.2um, then the auxiliary phase alloy raw material fine powder obtaining is mixed with the oleic acid of 0.02 weight portion of the auxiliary phase alloy raw material fine powder in 100 weight portions, obtain auxiliary phase presoma.
Above-mentioned principal phase presoma and auxiliary phase presoma are evenly mixed, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 1.5 weight portions.The moulding in the permanent magnetic field at 3.5T by the principal phase presoma mixing and auxiliary phase presoma, then keep 30s through static pressure such as 220MPa, then at 1100 ℃ of sintering 3h, and carry out one-level tempering at 940 ℃, keep 1.5h; Then carry out second annealing at 500 ℃, keep 3h.Final acquisition rare earth permanent-magnetic material of the present invention.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 9
To fill a prescription as Pr
6.625nd
19.875tb
1.5fe
68.4co
2.5b
1.1raw material gets rid of tape handling with the copper roller linear resonance surface velocity of 1.8m/s, prepares and gets rid of strap, as main-phase alloy raw material.Described main-phase alloy raw material, under 0.5Mpa hydrogen pressure, is inhaled to hydrogen 3h at 25 ℃, then dehydrogenase 37 h at 500 ℃, thus make the hydrogen flour of main-phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described main-phase alloy raw material of 100 weight portions and 0.03 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the main-phase alloy raw material fine powder of 3um, then the main-phase alloy raw material fine powder obtaining is mixed with the stearic acid of 0.04 weight portion of the main-phase alloy raw material fine powder in 100 weight portions, obtain principal phase presoma.
To fill a prescription as Pr
9.6nd
29.3dy
10fe
15.5co
16.5b
0.96al
5.5cu
3.2zr
2.4ga
7raw material under 1300 ℃, the condition of 25min, carry out melting ingot casting, prepare ingot casting, as auxiliary phase alloy raw material.Described auxiliary phase alloy raw material, under 0.5Mpa hydrogen pressure, is inhaled to hydrogen 3h at 25 ℃, then dehydrogenase 37 h at 500 ℃, thus make the hydrogen flour of auxiliary phase alloy raw material.Then, by the neodymium iron boron special antioxidant of the hydrogen flour of the described auxiliary phase alloy raw material of 100 weight portions and 0.03 weight portion (purchased from Beijing Jun Cefeng development in science and technology Co., Ltd, trade mark KM-01) mix, then grind by airflow milling, making average grain diameter is the auxiliary phase alloy raw material fine powder of 2.8um, then the auxiliary phase alloy raw material fine powder obtaining is mixed with the stearic acid of 0.04 weight portion of the auxiliary phase alloy raw material fine powder in 100 weight portions, obtain auxiliary phase presoma.
Above-mentioned principal phase presoma and auxiliary phase presoma are evenly mixed, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 1.5 weight portions.The moulding in the permanent magnetic field of 3T by the principal phase presoma mixing and auxiliary phase presoma, then keep 120s through static pressure such as 170MPa, then at 1080 ℃ of sintering 6h, and carry out one-level tempering at 900 ℃, keep 2h; Then carry out second annealing at 490 ℃, keep 4h.Final acquisition rare earth permanent-magnetic material of the present invention.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 10
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, main-phase alloy raw material consists of: Pr
6.575nd
19.725dy
1tb
0.2fe
70.84co
0.8b
0.86; Auxiliary phase alloy raw material consists of: Pr
3nd
9dy
25.5fe
36.4co
18b
1.1al
2cu
1zr
2ga
2.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 11
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy raw material consists of Pr
9.6nd
29.3dy
20fe
15.5co
16.5b
1al
2.36cu
1.57zr
1.57ga
2.6.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 12
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy raw material consists of Pr
9.6nd
29.3dy
20fe
15.5co
16.5b
1al
2.36cu
1.57zr
1.57ga
2.6, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 3.5 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 13
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy raw material consists of Pr
9.6nd
29.3dy
20fe
15.5co
16.5b
1al
2.36cu
1.57zr
1.57ga
2.6, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 5 weight portions.Always consisting of of main-phase alloy raw material and auxiliary phase alloy raw material: Pr
5.23nd
23.315dy
3.85tb
0.475fe
63.95co
1.775b
1al
0.118cu
0.0785zr
0.0785ga
0.13.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 14
Adopt trace element (being Co, B, Al, Cu, Zr, the Ga) content of embodiment 13, and adjust the content of rare earth and iron, adopt preparation method's (being equivalent to single alloy preparation method) that main-phase alloy raw material can be prepared into rare earth permanent-magnetic material in embodiment 1, make the performance of the performance of the rare earth permanent-magnetic material making and the rare earth permanent-magnetic material of embodiment 13 close.Consisting of of raw material: Pr
4nd
22.7dy
5.7tb
0.475fe
63.95co
1.77b
1al
0.118cu
0.0785zr
0.0785ga
0.13.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 15
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy raw material consists of Pr
10.3nd
31.7dy
25fe
8al
6.95cu
8.1zr
6.95ga
3.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 16
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy raw material consists of Pr
10.3nd
31.7dy
25fe
8al
6.95cu
8.1zr
6.95ga
3, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 3.5 weight portions.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 17
The preparation method who adopts the rare earth permanent-magnetic material of embodiment 1, different, auxiliary phase alloy material composition is Pr
10.3nd
31.7dy
25fe
8al
6.95cu
8.1zr
6.95ga
3, and with respect to the described principal phase presoma of 100 weight portions and total consumption of described auxiliary phase presoma, the consumption of described auxiliary phase presoma is 5 weight portions.Always consisting of of main-phase alloy raw material and auxiliary phase alloy raw material: Pr
5.265nd
23.435dy
4.1tb
0.475fe
63.575co
0.95b
0.95al
0.3475cu
0.405zr
0.3475ga
0.15.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Embodiment 18
Adopt trace element (being Co, B, Al, Cu, Zr, the Ga) content of embodiment 17, and adjust the content of rare earth and iron, adopt preparation method's (being equivalent to single alloy preparation method) that main-phase alloy raw material can be prepared into rare earth permanent-magnetic material in embodiment 1, make the performance of the performance of the rare earth permanent-magnetic material making and the rare earth permanent-magnetic material of embodiment 17 close.Consisting of of raw material: Pr
4nd
22.8dy
6tb
0.475fe
63.575co
0.95b
0.95al
0.3475cu
0.405zr
0.3475ga
0.15.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Comparative example 5
Adopt the method for embodiment 2 in CN102534358A, adjust the constituent content of permanent magnetic material, make the performance of the permanent magnetic material obtaining close with embodiment 18.Consisting of of raw material: Nd
18.72pr
4.68dy
7tb
0.6fe
67.9cu
0.1b
1.The magnetic property of this rare earth permanent-magnetic material is as shown in table 2.
Table 2
Can find out from the test result of table 1, the remanent magnetism of rare earth permanent-magnetic material prepared by embodiment 1-7 is 11.3-13.18(kGs), coercive force is 21-26(kOe).That prepares with comparative example 1 does not contain compared with the rare earth permanent-magnetic material of auxiliary phase, the remanent magnetism of rare earth permanent-magnetic material prepared by embodiment 1-7 declines and is 14.4% to the maximum, but coercive force raising is 30% to the maximum, and β temperature coefficient improves very obvious, and the maximum operating temperature of rare earth permanent-magnetic material can improve 30 ℃.
In addition, in the case of obtaining the rare earth permanent-magnetic material that performance is close, adopt two alloyages to decline than the dysprosium of rare earth permanent-magnetic material that adopts single alloyage to make and/or the content of terbium.And, compared with the close rare earth permanent-magnetic material (comparative example 5) of the performance that adopts rare earth permanent-magnetic material provided by the invention (embodiment 18) to provide with prior art, dysprosium content 14.28 % by weight that declined, the content of terbium 20.83 % by weight that declined.Illustrate that thus rare earth permanent-magnetic material provided by the invention has higher coercive force in guaranteeing higher remanent magnetism, also obviously reduced the content of dysprosium and/or terbium, reduced the production cost of rare earth permanent-magnetic material.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned execution mode, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible compound modes.
In addition, also can carry out combination in any between various execution mode of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (12)
1. a rare earth permanent-magnetic material, this material comprises principal phase and auxiliary phase, it is characterized in that,
Consisting of of described principal phase: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%;
Consisting of of described auxiliary phase: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%;
Take the gross mass of described principal phase and auxiliary phase as benchmark, the mass content of described auxiliary phase is greater than 0 and be less than or equal to 20%.
2. material according to claim 1, wherein, in the composition of described principal phase, the mass percent of x, y, z, u is: 28%≤x+y≤32%, 1.5%≤y≤4%, 1%≤z≤2.5%, 0.9%≤u≤1.1%.
3. material according to claim 1, wherein, in the composition of described auxiliary phase, the mass percent of a, b, c, n, v is: 38%≤a+b≤67%, 10%≤b≤25%, 0%≤c≤17%, 0%≤n≤1%, 8%≤v≤28%.
4. according to the material described in any one in claim 1-3, wherein, take the gross mass of described principal phase and auxiliary phase as benchmark, the mass content of described auxiliary phase is greater than 0 and be less than or equal to 15%.
5. a preparation method for rare earth permanent-magnetic material, the method comprises carries out mixed-forming, sintering and tempering successively to main-phase alloy raw material and auxiliary phase alloy raw material, it is characterized in that,
Consisting of of described main-phase alloy raw material: R1
xr2
yfe
100-x-y-z-uco
zb
u, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and wherein, x, y, z, u are mass percent, and 26%≤x+y≤36%, 0.01%≤y≤6%, 0%≤z≤5%, 0.8%≤u≤1.2%;
Consisting of of described auxiliary phase alloy raw material: R1
ar2
bfe
100-a-b-c-n-vco
cb
nm
v, R1 is selected from Pr and/or Nd; R2 is selected from Dy and/or Tb, and M is selected from one or more in Zr, Ga, Cu, Nb, Sn, Mo, Al, V, W, Si, Hf, Ti, wherein, a, b, c, n, v are mass percent, and 35%≤a+b≤80%, 5%≤b≤40%, 0%≤c≤40%, 0%≤n≤1.2%, 0%≤v≤30%;
With respect to the described main-phase alloy raw material of 100 weight portions and total consumption of described auxiliary phase alloy raw material, the consumption of described auxiliary phase alloy raw material is greater than 0 weight portion and is less than or equal to 20 weight portions.
6. method according to claim 5, wherein, in the composition of described main-phase alloy raw material, the mass percent of x, y, z, u is preferably: 28%≤x+y≤32%, 1.5%≤y≤4%, 1%≤z≤2.5%, 0.9%≤u≤1.1%.
7. method according to claim 5, wherein, in the composition of described auxiliary phase alloy raw material, the mass percent of a, b, c, n, v is preferably: 38%≤a+b≤67%, 10%≤b≤25%, 0%≤c≤17%, 0%≤n≤1%, 8%≤v≤28%.
8. according to the method described in any one in claim 5-7, wherein, with respect to the described main-phase alloy raw material of 100 weight portions and auxiliary phase alloy raw material total consumption, the consumption of described auxiliary phase alloy raw material is greater than 0 weight portion and is less than or equal to 15 weight portions.
9. method according to claim 5, wherein, described main-phase alloy raw material and described auxiliary phase alloy raw material use with the form of ingot casting or rapid hardening thin slice separately, and described ingot casting or rapid hardening thin slice make by melting.
10. according to the method described in claim 5 or 9, wherein, the process of moulding comprises: in the permanent magnetic field of 1.5-4T or pulsed magnetic field, be orientated compressingly, and keep 30-120s at the inferior static pressure of 170-220MPa.
11. methods according to claim 5, wherein, the condition of described sintering comprises: sintering temperature is 1040-1120 ℃, sintering time is 3-8 hour; The step of described tempering is: first carry out one-level tempering at 860-940 ℃, and keep 1-5h, then carry out second annealing at 470-560 ℃, and keep 1-8h.
12. rare earth permanent-magnetic materials of being prepared by the method described in any one in claim 5-11.
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