CN101982855A - Sintered Nd-Fe-B permanent-magnet material and preparation method thereof - Google Patents
Sintered Nd-Fe-B permanent-magnet material and preparation method thereof Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 19
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 16
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 7
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- 230000005291 magnetic effect Effects 0.000 claims description 39
- 239000000696 magnetic material Substances 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 28
- 239000010949 copper Substances 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 21
- 230000008018 melting Effects 0.000 claims description 21
- 238000003801 milling Methods 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 239000004615 ingredient Substances 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000013022 venting Methods 0.000 claims description 7
- 238000005275 alloying Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000000956 alloy Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 229910052742 iron Inorganic materials 0.000 description 16
- 229910052777 Praseodymium Inorganic materials 0.000 description 15
- 229910052796 boron Inorganic materials 0.000 description 15
- 239000007789 gas Substances 0.000 description 10
- 229910052779 Neodymium Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005662 electromechanics Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
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Abstract
The invention discloses a sintered Nd-Fe-B permanent-magnet material and a preparation method thereof. The molecular formula of the sintered Nd-Fe-B permanent-magnet material is (NdPr)aFe[100%-a-b-c]BbMc, wherein M is one or a plurality of Dy, Ho, Nb, Zr, Co, Ga, Al and Cu; a, b and c represent the mass percentages of the corresponding elements; a is greater than or equal to 20% and smaller than or equal to 32%, b is greater than or equal to 0.9% and smaller than or equal to 1.2%, and c is greater than or equal to 0% and smaller than or equal to 6%; and the mass of the element Pr accounts for 20-49% of the mass of PrNd alloy. Compared with the prior art, the sintered Nd-Fe-B permanent-magnet material has the following advantage: the content of the element Pr in the Nd-Fe-B permanent-magnet material is increased by adjusting the composition and content of the Nd-Fe-B permanent-magnet material, so that the mass percentage of the element Pr in the light rare earth Nd is increased to 20-49%. Compared with the prior Nd-Fe-B permanent-magnet material, the Nd-Fe-B permanent-magnet material obtained by the invention has the advantages that the high coercive force can be maintained and simultaneously the cost is greatly lowered without reducing the remanence.
Description
Technical field
The present invention relates to the permanent magnetic material technical field, relate in particular to a kind of sintered Nd-Fe-B permanent magnetic material and preparation method thereof.
Background technology
At present, permanent magnetic material is widely used in various fields such as electronics, automobile, computer, the energy, machinery and medicine equipment.Wherein, rare-earth Nd-Fe-B permanent magnetic material is a most important permanent magnetic material in the long duration now and from now on, and the new beginning of rare earth permanent-magnetic material has been opened up in his appearance.
At present, nearly 50% Nd-Fe-Bo permanent magnet material is applied to electromechanics trade.The development of The Development of Permanent Magnet Machine and permanent magnetic material is closely-related.The sintered Nd-Fe-B permanent magnetic material that uses in the motor generally all needs higher coercive force, generally about 20kOe.The anti-demagnetization capability of coercive force and motor, promptly overload magnification is relevant with indexs such as air gap flux densities, and coercivity value is big more, the anti-demagnetization capability of motor is strong more, overload magnification is big more, and is strong more to the adaptive capacity of strong demagnetization dynamic duty environment, and the air gap flux density of motor also can increase simultaneously.At present, domestic preparation high-coercive force magnet generally by adding heavy rare earth element Tb and Dy, especially adds heavy rare earth element Tb.But,, therefore can significantly increase the cost of Nd-Fe-Bo permanent magnet material by the coercive force that adds heavy rare earth element raising Nd-Fe-Bo permanent magnet material because heavy rare earth element costs an arm and a leg.In addition, because heavy rare earth element and iron dust antiferromagnetic coupling can reduce the iron atom magnetic moment, thereby cause the magnetic flux Bs of Nd-Fe-Bo permanent magnet material and remanent magnetism Br to descend.
Summary of the invention
The objective of the invention is provides a kind of sintered Nd-Fe-B permanent magnetic material and preparation method thereof at the above-mentioned state of the art, and this sintered Nd-Fe-B permanent magnetic material has the advantage of low cost, high-coercive force and high remanent magnetism.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is: a kind of sintered Nd-Fe-B permanent magnetic material, represent that the ingredient formula of its component and content is (NdPr)
aFe
100%-a-b-cB
bM
cExpression, wherein M be in Dy, Ho, Nb, Zr, Co, Ga, Al and the Cu element one or more, a, b and c represent the mass percent of each corresponding element respectively, and 20%≤a≤32%, 0.9%≤b≤1.2%, 0≤c≤6%, the quality of Pr element account for 20%~49% of PrNd alloying element quality.
As preferably, each component and the content of above-mentioned a kind of sintered Nd-Fe-B permanent magnetic material are:
PrNd alloying element 20%~32%;
Fe element 55%~70%;
B element 0.9%~1.1%;
Dy element 0~8%;
Ho element 0~5%;
Co element 0~2%;
Cu element 0~0.2%;
Ga element 0~0.2%;
Al element 0~1%;
Zr element 0~1%;
Nb element 0~1%.
The preparation method of a kind of sintered Nd-Fe-B permanent magnetic material of the present invention comprises the steps:
Step 1: according to ingredient formula (NdPr)
aFe
100%-a-b-cB
bM
cShown component and mass percentage content preparation raw material, wherein M be in Dy, Ho, Nb, Zr, Co, Ga, Al and the Cu element one or more, a, b and c represent the mass percent of each corresponding element respectively, and 20%≤a≤32%, 0.9%≤b≤1.2%, 0≤c≤6%, the quality of Pr element account for 20%~49% of PrNd alloying element quality.:
Step 2: the raw material of step 1 preparation is dropped into the rapid hardening stove, carry out melting in inert gas shielding atmosphere, after the melting melting liquid is watered roller speed on the copper roller of 0.5m/s~2m/s, getting rid of into average thickness is the rapid hardening strip of 0.25mm~0.4mm;
Step 3: the rapid hardening strip that step 2 is obtained carries out the broken technology of hydrogen, and the broken laggard capable airflow milling of hydrogen obtains magnetic, with magnetic oriented moulding in magnetic field, obtains molded blank;
Step 4: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, carry out the dehydrogenation venting in the sintering process, regulate sintering temperature to 1050 ℃~1110 ℃ then, charge into inert gas after being incubated 2 hours~5 hours and be cooled to below 100 ℃, carried out Ageing Treatment 3 hours~5 hours at 450 ℃~600 ℃ then.
In order to optimize technique scheme, the measure of taking also comprises:
The particle mean size of the magnetic in the step 3 is 3 μ m~4 μ m, and the density of molded blank is more than the 4.0g/cm3.
The magnetic field intensity in magnetic field is 1.5T~2T in the step 3.
Dehydrogenation deflation course in the step 4 carries out between 300 ℃~800 ℃.
Compared with prior art, the advantage of a kind of sintered Nd-Fe-B permanent magnetic material of the present invention is: by adjusting the component and the content of Nd-Fe-Bo permanent magnet material, improve the content of Pr element in the Nd-Fe-Bo permanent magnet material, the percentage that makes the quality of Pr element account for light rare earth Nd element quality brings up to 20%~49%, the Nd-Fe-Bo permanent magnet material that obtains is compared with existing Nd-Fe-Bo permanent magnet material, can when keeping high-coercive force, reduce cost greatly, and remanent magnetism not reduce.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1:
In the present embodiment, the ingredient formula of sintered Nd-Fe-B permanent magnetic material is:
Nd
18..5%Pr
10%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%, its preparation method comprises the steps:
Step 1: with Nd, Pr, Fe, B, Dy, Cu, Al, Zr and Co element according to ingredient formula Nd
18..5%Pr
10%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%The mass percentage content preparation raw material of expression, confected materials drops in the rapid hardening stove, is 2 * 10 in vacuum degree
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the melting melting liquid is watered roller speed on the copper roller of 1m/s, getting rid of into average thickness is the rapid hardening strip of 0.33mm;
Step 2: the rapid hardening strip that step 1 is obtained is packed into and is carried out the broken technology of hydrogen in the hydrogenation furnace, magnetic after hydrogen is broken carries out airflow milling, the particle mean size of the magnetic after the airflow milling is 3.5 μ m, is oriented moulding in the magnetic field of 2T with the magnetic after the airflow milling in magnetic field, and obtaining density is the above molded blank of 4.0g/cm3;
Step 3: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, in the sintering process, be incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ and carry out the dehydrogenation venting, regulate sintering temperature to 1065 ℃ then, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, then respectively carried out Ageing Treatment 3 hours at 900 ℃ and 500 ℃.
Embodiment 2:
In the present embodiment, the ingredient formula of sintered Nd-Fe-B permanent magnetic material is:
Nd
18..5%Pr
10%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%, its preparation method comprises the steps:
Step 1: with Nd, Pr, Fe, B, Dy, Cu, Al, Zr and Co element according to ingredient formula Nd
18..5%Pr
10%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%The mass percentage content preparation raw material of expression, confected materials drops in the rapid hardening stove, is 2 * 10 in vacuum degree
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the melting melting liquid is watered roller speed on the copper roller of 1m/s, getting rid of into average thickness is the rapid hardening strip of 0.37mm;
Step 2: the rapid hardening strip that step 1 is obtained is packed into and is carried out the broken technology of hydrogen in the hydrogenation furnace, magnetic after hydrogen is broken carries out airflow milling, the particle mean size of the magnetic after the airflow milling is 3.8 μ m, is oriented moulding in the magnetic field of 2T with the magnetic after the airflow milling in magnetic field, and obtaining density is the above molded blank of 4.0g/cm3;
Step 3: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, in the sintering process, be incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ and carry out the dehydrogenation venting, regulate sintering temperature to 1085 ℃ then, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, then respectively carried out Ageing Treatment 3 hours at 900 ℃ and 500 ℃.
Embodiment 3:
In the present embodiment, the ingredient formula of sintered Nd-Fe-B permanent magnetic material is:
Nd
16..5%Pr
12%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%, its preparation method comprises the steps:
Step 1: with Nd, Pr, Fe, B, Dy, Cu, Al, Zr and Co element according to ingredient formula Nd
16..5%Pr
12%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%The mass percentage content preparation raw material of expression, confected materials drops in the rapid hardening stove, is 2 * 10 in vacuum degree
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the melting melting liquid is watered roller speed on the copper roller of 1m/s, getting rid of into average thickness is the rapid hardening strip of 0.33mm;
Step 2: the rapid hardening strip that step 1 is obtained is packed into and is carried out the broken technology of hydrogen in the hydrogenation furnace, magnetic after hydrogen is broken carries out airflow milling, the particle mean size of the magnetic after the airflow milling is 3.5 μ m, is oriented moulding in the magnetic field of 2T with the magnetic after the airflow milling in magnetic field, and obtaining density is the above molded blank of 4.0g/cm3;
Step 3: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, in the sintering process, be incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ and carry out the dehydrogenation venting, regulate sintering temperature to 1065 ℃ then, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, then respectively carried out Ageing Treatment 3 hours at 900 ℃ and 500 ℃.
Embodiment 4:
In the present embodiment, the ingredient formula of sintered Nd-Fe-B permanent magnetic material is:
Nd
15%Pr
13.5%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%, its preparation method comprises the steps:
Step 1: with Nd, Pr, Fe, B, Dy, Cu, Al, Zr and Co element according to ingredient formula Nd
15%Pr
13.5%Fe
66.3%B
1%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%The mass percentage content preparation raw material of expression, confected materials drops in the rapid hardening stove, is 2 * 10 in vacuum degree
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the melting melting liquid is watered roller speed on the copper roller of 1m/s, getting rid of into average thickness is the rapid hardening strip of 0.33mm;
Step 2: the rapid hardening strip that step 1 is obtained is packed into and is carried out the broken technology of hydrogen in the hydrogenation furnace, magnetic after hydrogen is broken carries out airflow milling, the particle mean size of the magnetic after the airflow milling is 3.5 μ m, is oriented moulding in the magnetic field of 2T with the magnetic after the airflow milling in magnetic field, and obtaining density is the above molded blank of 4.0g/cm3;
Step 3: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, in the sintering process, be incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ and carry out the dehydrogenation venting, regulate sintering temperature to 1065 ℃ then, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, then respectively carried out Ageing Treatment 3 hours at 900 ℃ and 500 ℃.
Embodiment 5:
In the present embodiment, the ingredient formula of sintered Nd-Fe-B permanent magnetic material is:
Nd
14%Pr
12.5%Fe
66.3%B
1%Ho
2%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%, its preparation method comprises the steps:
Step 1: with Nd, Pr, Fe, B, Ho, Dy, Cu, Al, Zr and Co element according to ingredient formula Nd
14%Pr
12.5%Fe
66.3%B
1%Ho
2%Dy
2.5%Cu
0.1%Al
0.4%Zr
0.2%Co
1%The mass percentage content preparation raw material of expression, confected materials drops in the rapid hardening stove, is 2 * 10 in vacuum degree
-2Add heat drying furnace under the vacuum of Pa, charge into Ar gas then and carry out melting, after the melting melting liquid is watered roller speed on the copper roller of 1m/s, getting rid of into average thickness is the rapid hardening strip of 0.3mm;
Step 2: the rapid hardening strip that step 1 is obtained is packed into and is carried out the broken technology of hydrogen in the hydrogenation furnace, magnetic after hydrogen is broken carries out airflow milling, the particle mean size of the magnetic after the airflow milling is 3.5 μ m, is oriented moulding in the magnetic field of 2T with the magnetic after the airflow milling in magnetic field, and obtaining density is the above molded blank of 4.0g/cm3;
Step 3: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, in the sintering process, be incubated 2 hours respectively at 300 ℃, 560 ℃ and 800 ℃ and carry out the dehydrogenation venting, regulate sintering temperature to 1065 ℃ then, be incubated and charge into high-purity Ar gas after 4 hours and be cooled to below 100 ℃, then respectively carried out Ageing Treatment 3 hours at 900 ℃ and 500 ℃.
The performance of each sintered Nd-Fe-B permanent magnetic material that obtains according to the preparation method in the foregoing description 1 to embodiment 5 is as shown in the table:
Most preferred embodiment of the present invention is illustrated, and various variations or the remodeling made by those of ordinary skills can not depart from the scope of the present invention.
Claims (6)
1. sintered Nd-Fe-B permanent magnetic material is characterized in that: the ingredient formula of described sintered Nd-Fe-B permanent magnetic material is (NdPr)
aFe
100%-a-b-cB
bM
cWherein M is one or more in Dy, Ho, Nb, Zr, Co, Ga, Al and the Cu element, a, b and c represent the mass percent of each corresponding element respectively, and 20%≤a≤32%, 0.9%≤b≤1.2%, 0≤c≤6%, the quality of Pr element account for 20%~49% of PrNd alloying element quality.
2. a kind of sintered Nd-Fe-B permanent magnetic material according to claim 1 is characterized in that: the component of described sintered Nd-Fe-B permanent magnetic material and content are: PrNd alloying element, content are 20%~32%; Fe element, content are 55%~70%; B element, content are 0.9%~1.1%; Dy element, content are 0~8%; Ho element, content are 0~5%; Co element, content are 0~2%; Cu element, content are 0~0.2%; Ga element, content are 0~0.2%; Al element, content are 0~1%; Zr element, content are 0~1%; Nb element, content are 0~1%.
3. the preparation method of a kind of sintered Nd-Fe-B permanent magnetic material as claimed in claim 1 is characterized in that: comprise the steps:
Step 1: according to described component and mass percentage content preparation raw material:
Step 2: the raw material of step 1 preparation is dropped into the rapid hardening stove, carry out melting in inert gas shielding atmosphere, after the melting melting liquid is watered roller speed on the copper roller of 0.5m/s~2m/s, getting rid of into average thickness is the rapid hardening strip of 0.25mm~0.4mm;
Step 3: the rapid hardening strip that step 2 is obtained carries out the broken technology of hydrogen, and the broken laggard capable airflow milling of hydrogen obtains magnetic, with magnetic oriented moulding in magnetic field, obtains molded blank;
Step 4: the sintering furnace that the molded blank that step 3 is obtained is put into high vacuum carries out sintering, carry out the dehydrogenation venting in the sintering process, regulate sintering temperature to 1050 ℃~1110 ℃ then, charge into inert gas after being incubated 2 hours~5 hours and be cooled to below 100 ℃, carried out Ageing Treatment 3 hours~5 hours at 450 ℃~600 ℃ then.
4. the preparation method of a kind of sintered Nd-Fe-B permanent magnetic material according to claim 3, it is characterized in that: the particle mean size of the magnetic in the described step 3 is 3 μ m~4 μ m, and the density of molded blank is 4.0g/cm
3More than.
5. the preparation method of a kind of sintered Nd-Fe-B permanent magnetic material according to claim 3, it is characterized in that: the magnetic field intensity in magnetic field is 1.5T~2T in the described step 3.
6. the preparation method of a kind of sintered Nd-Fe-B permanent magnetic material according to claim 3, it is characterized in that: the dehydrogenation deflation course in the described step 4 carries out between 300 ℃~800 ℃.
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