CN101819841A - Neodymium iron boron magnetic material and preparation method thereof - Google Patents
Neodymium iron boron magnetic material and preparation method thereof Download PDFInfo
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Abstract
一种永磁材料技术领域的钕铁硼磁性材料及其制备方法，通过将锭块或速凝薄片进行粗破碎处理并经气流磨制成粉末，并在磁场下取向压制成型，然后将坯体进行冷等静压及高真空烧结，最后经回火处理制成钕铁硼磁性材料，获得氧含量在1500～4400ppm范围内，方形度高达98％～99％的钕铁硼磁体。通过对磁体的显微组织进行观察，结果表明：磁体中dhcp结构的富Nd相氧含量＜9at.％，fcc结构的富Nd相氧含量为10at.％～48at.％。
A neodymium-iron-boron magnetic material in the technical field of permanent magnet materials and a preparation method thereof. The ingot or the quick-setting flake is roughly crushed and then jet-milled into powder, which is orientated and pressed into shape under a magnetic field, and then the green body is Cold isostatic pressing and high-vacuum sintering are carried out, and finally NdFeB magnetic materials are made through tempering treatment to obtain NdFeB magnets with oxygen content in the range of 1500-4400ppm and squareness as high as 98%-99%. By observing the microstructure of the magnet, the results show that the oxygen content of the Nd-rich phase of the dhcp structure in the magnet is less than 9 at.%, and the oxygen content of the Nd-rich phase of the fcc structure is 10 at.% to 48 at.%.
Description
Technical field
What the present invention relates to is neodymium-iron-boron magnetic material of a kind of permanent magnetic material technical field and preparation method thereof, specifically is that a kind of demagnetization curve squareness (abbreviation squareness) is higher than neodymium-iron-boron magnetic material of 98% and preparation method thereof.
Background technology
Nd-Fe-Bo permanent magnet material is since nineteen eighty-three exploitation, because its abundant raw materials, low price, magnetic property are best, thereby are widely used in numerous areas such as automobile, motor, instrument and medicine equipment, is with fastest developing speed a kind of in the magnetic material.Along with the specification requirement of energy-saving and emission-reduction, the application of neodymium iron boron in automobile is especially noticeable, mainly is drive motor and generator.For magneto, remanent magnetism is high more, and the gap field that provides is just high more, and the moment of motor is just big more, can improve efficiency of motor; Coercive force is high more, and the anti-demagnetization capability of machine operation field is just strong more, and working range is also just wide more; Squareness is good more, and the dynamic loss of motor is just more little.Therefore neodymium iron boron not only requires it to have very high magnetic property, the temperature stability that also needs as motor material hot soak condition.But neodymium-iron-boron magnetic material exists Curie temperature lower, temperature coefficient is big, squareness is not high and repeated shortcoming such as bad, obtained very big progress about the research that how to reduce temperature coefficient and raising Curie temperature at present, but it is less about the research that how to improve squareness, therefore significant about the research that how to prepare high squareness Sintered NdFeB magnet.
Literature search through prior art is found, people such as Liu Xiang ripples are at " relation of Nd-Fe-B magnet demagnetization curve squareness and sintering process " (magnetic material and device, 2007,38 (1): the relation of once having studied magnet squareness and sintering process 46-50), he has analyzed relative density, crystallite dimension and distribution square shaped degree influence rule, this technology has been put down in writing raising density, reducing average grain size and making its grain size distribution evenly is the necessary condition of the good squareness magnet of preparation, but do not point out to prepare the process conditions of high squareness neodymium iron boron magnetic body, temperature particularly, the scope of important technical parameters such as humidity and sintering vacuum degree, and the scope of final magnet oxygen content.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of neodymium-iron-boron magnetic material and preparation method thereof is provided, obtain oxygen content in 1500～4400ppm scope, squareness is up to 98%～99% neodymium iron boron magnetic body, the rich Nd phase oxygen content＜9at.% of dhcp structure in the magnet, the rich Nd phase oxygen content of fcc structure is 10at.%～48at.%.
The present invention is achieved by the following technical solutions,
The present invention relates to a kind of neodymium-iron-boron magnetic material, its alloying component is Nd
aFe
100-a-b-cB
bM
c, wherein: 11≤a≤24,5.5≤b≤7,0≤c≤7, M be in Pr, Dy, Tb, Gd, Al, Cu, Ga, Nb, Co or the Y element one or more.
The present invention relates to the preparation method of above-mentioned neodymium-iron-boron magnetic material, comprise the steps:
The first step, employing casting ingot process are made the ingot bar of neodymium iron boron cast alloy or are made Nd Fe B alloys rapid hardening thin slice with rapid hardening thin slice technology, and the alloying component of described neodymium iron boron alloy of ingot is Nd
aFe
100-a-b-cB
bM
c, wherein: 11≤a≤24,5.5≤b≤7,0≤c≤7, M be in Pr, Dy, Tb, Gd, Al, Cu, Ga, Nb, Co or the Y element one or more;
Second goes on foot, ingot bar or rapid hardening thin slice is carried out the coarse crushing processing and make powder through airflow milling;
Described coarse crushing is handled and is meant: adopt mechanical system to be crushed to 80～100 orders ingot bar or rapid hardening thin slice;
Described airflow milling is made powder and is meant: ingot bar or rapid hardening thin slice after by the airflow milling method coarse crushing being handled are worn into the powder that average particulate diameter is 4～5 μ m.
The 3rd step, the neodymium iron boron powder is orientated compression moulding under magnetic field, then base substrate is carried out isostatic cool pressing, obtain the rare earth base substrate;
Described orientation compression moulding is meant: externally-applied magnetic field 1.6～2.0T under the environment of 10～30 ℃ of temperature and humidity 20～40%;
The pressing pressure of described isostatic cool pressing is 150～250MPa.
The 4th the step, the rare earth base substrate is carried out the high vacuum sintering, neodymium-iron-boron magnetic material is made in last tempered processing.
Described high vacuum sintering is meant: sintering vacuum degree 1.0 * 10 is set
-2～5 * 10
-4Pa, sintering temperature is 1040～1140 ℃ of sintering that carry out 1～4h.
Described temper is meant: carry out double tempering successively under 1000～800 ℃ and 500～580 ℃, each tempering time is 1～2h.
The present invention is conceived to the actual and application of production of Nd-Fe-Bo permanent magnet material, because in actual applications, only consider that these two indexs of permanent magnet magnetic energy product and coercive force are not enough, whether the demagnetization curve squareness that also must investigate magnet meets the requirements, squareness is high more to show that the performance of magnet is good more, the opposing magnetic field intensity that can bear is big more, and anti-external magnetic field interference performance is strong more.In fact the demagnetization curve squareness of a lot of permanent magnets is lower on the market, and the neodymium iron boron magnetic body of 98%～99% squareness is rarely seen especially.After the broken powder process of Nd Fe B alloys, under specific temperature and humidity, the NdFeB magnetic is carried out the magnetic field orientating die mould, sintering and heat treatment through special process, obtain oxygen content in 1500～4400ppm scope, squareness is up to 98%～99% neodymium iron boron magnetic body, and this method repeatability better in addition.
Description of drawings
The demagnetization curve figure of Fig. 1 embodiment 1 Sintered NdFeB magnet (M-1 and M-2);
The demagnetization curve figure of Fig. 2 embodiment 2 Sintered NdFeB magnets (M-4 and M-5);
The transmission electron microscope observing of Fig. 3 embodiment 1 Sintered NdFeB magnet (M-1).
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) adopt casting ingot process to make the neodymium iron boron alloy of ingot, its composition is (Nd
0.8Pr
0.2)
14.5Dy
1.2Fe
BalB
6(at.%).Alloy is carried out coarse crushing earlier in jaw crusher,, make the powder that average particulate diameter is 4～5 μ m by airflow milling at last then by middle crusher in crushing to 80～100 orders.
(2) under 10 ℃ of temperature and humidity 40% environmental condition, with the compression moulding in the magnetic field orientating forming press of neodymium iron boron powder, moulding alignment magnetic field 2.0T.After the orientation compacting base substrate is carried out isostatic cool pressing, pressure is 180MPa.
(3) base substrate is put into vacuum degree 1.0 * 10 respectively
-2Pa and vacuum degree 5.0 * 10
-2In the sintering furnace of Pa, 1040 ℃ of sintering 4h, through 900 ℃ and 500 ℃ of double temperings, tempering time 2h makes magnet M-1 and M-2 respectively again.
(4) under 35 ℃ of temperature and humidity 40% environmental condition, other preparation condition is made magnet M-3 with magnet M-1.
As shown in Figure 1, the demagnetization curve figure of the neodymium-iron-boron magnetic material for preparing for present embodiment.
Embodiment 2
(1) adopt single rod belt-rejecting technology to make neodymium iron boron rapid hardening foil alloys, copper roller speed is 2m/s, and its composition is (Nd
0.8Pr
0.2)
15.5Fe
BalB
6(at.%).Foil alloys is carried out coarse crushing earlier in jaw crusher,, make the powder that average particulate diameter is 4～5 μ m by airflow milling at last then by middle crusher in crushing to 80～100 orders.
(2) under 20 ℃ of temperature and humidity 30% environmental condition, with the compression moulding in the magnetic field orientating forming press of neodymium iron boron powder, moulding alignment magnetic field 1.8T.After the orientation compacting base substrate is carried out isostatic cool pressing, pressure is 200MPa.
(3) base substrate is put into vacuum degree 5 * 10 respectively
-4Pa and vacuum degree 9.0 * 10
-2In the Pa sintering furnace, 1100 ℃ of sintering 2h, through 900 ℃ and 530 ℃ of double temperings, tempering time 2h makes magnet M-4 and M-5 respectively again.
(4) under 10 ℃ of temperature and humidity 70% environmental condition, other preparation condition is made magnet M-6 with magnet M-4.
As shown in Figure 2, the demagnetization curve figure of the neodymium-iron-boron magnetic material for preparing for present embodiment.
Embodiment 3
(1) adopt casting ingot process to make the neodymium iron boron alloy of ingot, its composition is (Nd
0.8Pr
0.2)
14.5Nb
0.2Al
0.4Fe
BalB
6(at.%).Alloy is carried out coarse crushing earlier in jaw crusher,, make the powder that average particulate diameter is 4～5 μ m by airflow milling at last then by middle crusher in crushing to 80～100 orders.
(2) under 30 ℃ of temperature and humidity 20% environmental condition, with the compression moulding in the magnetic field orientating forming press of neodymium iron boron powder, moulding alignment magnetic field 2.0T.After the orientation compacting base substrate is carried out isostatic cool pressing, pressure is 200MPa.
(3) base substrate is put into vacuum degree 1.0 * 10 respectively
-3Pa and vacuum degree 6.0 * 10
-2In the sintering furnace of Pa, 1140 ℃ of sintering 1h, through 900 ℃ and 580 ℃ of double temperings, tempering time 2h makes magnet M-7 and M-8 respectively again.
(4) under 30 ℃ of temperature and humidity 55% environmental condition, preparation condition is made magnet M-9 with magnet M-7.
Table 1 adopts the performance of the Sintered NdFeB magnet of different process preparation
| Sample | Remanent magnetism (T) | Coercive force (kA/m) | Maximum magnetic energy product (kJ/m 3) | Density (g/cm 3) | Squareness (%) | Oxygen content (ppm) |
| ??M-1 | ??1.203 | ??1594.8 | ??276 | ??7.57 | ??98 | ??4400 |
| ??M-2 | ??1.152 | ??1546.4 | ??242 | ??7.27 | ??75 | ??6000 |
| ??M-3 | ??1.126 | ??1530.2 | ??241 | ??7.47 | ??78 | ??5000 |
| ??M-4 | ??1.133 | ??1106.8 | ??245 | ??7.47 | ??99 | ??1500 |
| ??M-5 | ??1.085 | ??838.8 | ??202 | ??7.36 | ??55 | ??6200 |
| ??M-6 | ??1.052 | ??936.2 | ??207 | ??7.37 | ??65 | ??5500 |
| ??M-7 | ??1.121 | ??1212.8 | ??245 | ??7.42 | ??99 | ??2300 |
| ??M-8 | ??1.073 | ??901.6 | ??216 | ??7.26 | ??74 | ??5200 |
| ??M-9 | ??1.098 | ??1026.9 | ??223 | ??7.30 | ??80 | ??4600 |
The performance of Sintered NdFeB magnet M-1, M-2, M-3, M-4, M-5, M-6, M-7, M-8 and M-9 among the embodiment 1,2 and 3 is listed in the table 1.By contrast M-1, M-2 and M-3, M-4, M-5 and M-6, and M-7, M-8 and M-9, as can be seen: the invention provides suitable technological parameter, particularly temperature, humidity and sintering vacuum degree, is the key of the high squareness magnet of preparation.The neodymium iron boron powder is orientated compression moulding through certain pressure under 10～30 ℃ of temperature, 20～40% humidity environment conditions, 1.0 * 10
-2～5 * 10
-4Under the Pa vacuum degree through the uniform temperature sintering, and annealing in process subsequently, prepared magnet oxygen content is between 1500～4400ppm, the squareness of magnet demagnetization curve is up to 98%～99%.
Performance evaluation
To squareness among the embodiment 1 is that 98% M-1 magnet carries out transmission electron microscope observing, sightingpiston is perpendicular to the magnet easy magnetizing axis, show by selected area electron diffraction and energy spectrum analysis, the rich Nd phase oxygen content of dhcp structure is less than 9at.% in the magnet, and the rich Nd phase oxygen content of fcc structure is between 10at.%～48at.%.The transmission electron microscopy pattern of M-1 sample is seen Fig. 3, and its energy spectrum analysis sees Table 2.Other is had 99% squareness magnet (M-4 and M-7) carries out transmission electron microscope observing and energy spectrum analysis also obtains same rule.
The energy spectrum analysis of corresponding microcell (at.%) among table 2 Fig. 3
| ??O | ??Fe | ??Pr | ??Nd | ??Dy | |
| ??Nd 2Fe 14B matrix phase | ??87.47 | ??2.59 | ??9.82 | ??0.12 | |
| Dhcp structure crystal boundary phase | ??8.04 | ??8.87 | ??25.26 | ??57.32 | ??0.51 |
| Fcc structure crystal boundary phase | ??33.07 | ??29.55 | ??8.13 | ??28.59 | ??0.65 |
Claims (8)
1. a neodymium-iron-boron magnetic material is characterized in that, its alloying component is Nd
aFe
100-a-b-cB
bM
cWherein: 11≤a≤24,5.5≤b≤7,0≤c≤7, M be in Pr, Dy, Tb, Gd, Al, Cu, Ga, Nb, Co or the Y element one or more, the squareness of described Fe-Mn magnetism material is 98%～99%, oxygen content is in 1500～4400ppm scope.
2. the preparation method of a neodymium-iron-boron magnetic material according to claim 1 is characterized in that, comprises the steps:
The first step, employing casting ingot process are made the ingot bar of neodymium iron boron cast alloy or are made Nd Fe B alloys rapid hardening thin slice with rapid hardening thin slice technology, and the alloying component of described neodymium iron boron alloy of ingot is Nd
aFe
100-a-b-cB
bM
c, wherein: 11≤a≤24,5.5≤b≤7,0≤c≤7, M be in Pr, Dy, Tb, Gd, Al, Cu, Ga, Nb, Co or the Y element one or more;
Second goes on foot, ingot bar or rapid hardening thin slice is carried out the coarse crushing processing and make powder through airflow milling;
The 3rd step, the neodymium iron boron powder is orientated compression moulding under magnetic field, then base substrate is carried out isostatic cool pressing, obtain the rare earth base substrate;
The 4th the step, the rare earth base substrate is carried out the high vacuum sintering, neodymium-iron-boron magnetic material is made in last tempered processing.
3. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, described coarse crushing is handled and is meant: adopt mechanical system to be crushed to 80～100 orders ingot bar or rapid hardening thin slice.
4. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, described airflow milling is made powder and is meant: ingot bar or rapid hardening thin slice after by the airflow milling method coarse crushing being handled are worn into the powder that average particulate diameter is 4～5 μ m.
5. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, described orientation compression moulding is meant: externally-applied magnetic field 1.6～2.0T under the environment of 10～30 ℃ of temperature and humidity 20～40%.
6. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, the pressing pressure of described isostatic cool pressing is 150～250MPa.
7. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, described high vacuum sintering is meant: sintering vacuum degree 1.0 * 10 is set
-2～5 * 10
-4Pa, sintering temperature is 1040～1140 ℃ of sintering that carry out 1～4h.
8. the preparation method of neodymium-iron-boron magnetic material according to claim 2 is characterized in that, described temper is meant: carry out double tempering successively under 1000～800 ℃ and 500～580 ℃, each tempering time is 1～2h.
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| CN102211192A (en) * | 2011-06-09 | 2011-10-12 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
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| CN102921950A (en) * | 2012-10-16 | 2013-02-13 | 山东依诺威强磁材料有限公司 | Sintering aging process for preparing neodymium-iron-boron permanent magnet material |
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| US10242779B2 (en) | 2012-12-31 | 2019-03-26 | Xiamen Tungsten Co., Ltd. | Manufacturing method of an alloy powder for rare earth magnet and the rare earth magnet based on heat treatment |
| CN103981337A (en) * | 2014-05-26 | 2014-08-13 | 上海交通大学 | Heat treatment process for sintered nd-fe-b |
| CN115700395A (en) * | 2022-11-11 | 2023-02-07 | 中钢天源股份有限公司 | Method for improving efficiency of high-temperature irreversible flux loss test of neodymium iron boron |
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