CN108269669B - A method of preparing neodymium iron boron magnetic body - Google Patents
A method of preparing neodymium iron boron magnetic body Download PDFInfo
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Abstract
A kind of method preparing neodymium iron boron magnetic body includes that ingredient, slab, hydrogen is broken, gas sub-sieve, powder processed, compression moulding, sintering;The neodymium iron boron magnetic body produced has the following performance, 20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 275MPa or more, remanent magnetism (Br) >=1.27T, intrinsic coercivity (Hcj) >=1670kA/m, magnetic energy product (BHmax) are >=335kJ/m3;20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 280MPa or more, and remanent magnetism (Br) >=1.32T, intrinsic coercivity (Hcj) >=1750kA/m, magnetic energy product (BHmax) is >=363kJ/m3.It is an advantage of the current invention that passing through the method for pyrogenic process gold metallurgy, the neodymium iron boron magnetic body of high-quality is produced, and there is strong high bending strength (275MPa).
Description
Technical field
The present invention relates to a kind of high-performance neodymium-iron-boron magnet methods, and in particular to a kind of pyrometallurgy and crystal boundary add two-phase
The method that alloy legal system technology prepares high-performance neodymium-iron-boron magnet.
Background technique
In recent years, with the rapid expansion of the application of NdFeB magnets, the demand of neodymium iron boron magnetic body has been become to get over
Come bigger, domestic Sintered NdFeB magnet constantly narrows the gap in the performance of magnetic property with overseas enterprise, but due to equipment and
The backwardness of technology also needs to further increase in terms of the stability of performance and consistency, especially in operating temperature one
As less than 140 degrees Celsius, be unable to satisfy more than 140 degree Celsius operational requirements, especially operating temperature 150 degrees Celsius the case where
Domestic existing Sintered NdFeB magnet can not work substantially.High-quality neodymium iron boron magnet is produced using pyrometallurgy, it can be effective
It avoids generating waste water, reduces the pressure to environment.
Summary of the invention
It is an object of the invention to be directed to the deficiencies in the prior art, a kind of side for preparing neodymium iron boron magnetic body is provided
Method changes the problem of present pyrometallurgy can not produce high-quality neodymium iron boron magnet, makes neodymium by the sorting to magnetic powder particle
The bending strength of iron boron magnet greatly improves, in the new of continuous uninterrupted (temperature-controllable) the not converter of sintering process and aging technique
Type heat treatment process effectively improves intrinsic coercivity, and operating temperature is higher by 15 degrees Celsius or more than similar product, can take the photograph 150
Good working order is still remain under the conditions of family name's degree.
The purpose of the present invention is achieved through the following technical solutions, and a kind of method preparing neodymium iron boron magnetic body includes ingredient, casting
Piece, hydrogen is broken, gas sub-sieve, powder processed, compression moulding, sintering;
The ingredient, weight ratio be Nd 19~20.5%, B 0.7~0.8%, Cu 0.3~0.35%, Co 1.2~
1.5%, Ga 0.3~0.4%, Zr0.7~0.8%, Nb 0.6~0.7%, Pr 5~6%, Al 0.7~0.9%, surplus are
Fe, mixing generate mixture;
Mixture is delivered to slab furnace and carries out melting under vacuum by the slab, and smelting temperature is 1350-1480 DEG C,
And the plates being made with a thickness of 0.3-0.4mm;
The hydrogen is broken, and hydrogen crushing furnace is inputted after plates are mixed with additive and progress hydrogen is quick-fried under vacuum conditions, vacuum
Degree is 1.06-1.11Pa, and temperature is 400-600 DEG C, generates primary product;
Primary product is inputted gas screen-dividing machine by the gas sub-sieve, and the gas screen-dividing machine includes gravity box, gravity box
Height is 6-8 meter, and gravity box upper end is equipped with light phase export, lower end is equipped with heavy out, light phase export by the first Negative pressure machine and
The connection of first airflow milling, heavy out are connect by the second Negative pressure machine with the second airflow milling, and inert gas passes through among gravity box
Feed pipe primary product is blown into gravity box, the inert gas plenum speed is 0.2 to 0.3 meter per second, and the first Negative pressure machine produces
Raw negative pressure is 0.06 ± 0.01MPa, and the negative pressure that the second Negative pressure machine generates is 0.05 ± 0.01MPa;
The powder processed, the first airflow milling generate the first fine powder (preferred, the first powder material temperature is not less than 100 DEG C),
Second airflow milling generates the second fine powder (preferred, the second powder material temperature is not less than 100 DEG C);
The compression moulding, the first fine powder are delivered to the first moulding press, the first moulding press by the first fine powder static pressure at
Type,
Second fine powder directly transports the second moulding press, and the second moulding press is by the second fine powder hydrostatic profile;
The sintering, the first moulding press compacting material are input to the first vacuum sintering furnace, and the second moulding press compacting material is defeated
Enter to the second vacuum sintering furnace, the vacuum degree of the first vacuum sintering furnace is less than 8Pa, 940-1070 DEG C of sintering temperature, sintering time
Vacuum degree for 13-15h, the second vacuum sintering furnace is less than 10Pa, 940-1090 DEG C of sintering temperature, sintering time 16-17h;
By above step, the first vacuum burns the product produced of furnace and generates the first neodymium iron boron magnetic body after cooling, and second
Vacuum burns the product that furnace is produced and generates the second neodymium iron boron magnetic body after cooling;
20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 275MPa or more, and remanent magnetism (Br) >=
1.27T, intrinsic coercivity (Hcj) >=1670kA/m, magnetic energy product (BHmax) are >=335kJ/m3;
20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 278MPa or more, and remanent magnetism (Br) >=
1.32T, intrinsic coercivity (Hcj) >=1750kA/m, magnetic energy product (BHmax) are >=363kJ/m3。
Further, the additive is praseodymium, and praseodymium weight is the 0.2~0.3% of sheet body weight.
Further, first airflow milling is spiral jet pulverizer;Second airflow milling is circulating airflow milling.
Further, in first vacuum sintering furnace sintering temperature gradient be followed successively by from start to finish 960 DEG C ±
20℃—1000℃±20℃—1045℃±25℃—1000℃±20℃—960℃±20℃—1010℃±30℃—
960 DEG C ± 20 DEG C, the time be followed successively by 1h ± 10min, 2h ± 10min, 4h ± 10min, 2h ± 10min, 1h ± 10min, 2h ±
10min、1h±10min。
Further, sintering temperature gradient is to be followed successively by 960 DEG C ± 20 from start to finish in the second vacuum sintering furnace
℃—1010℃±30℃—1065℃±25℃—1010℃±30℃—970℃±10℃—990℃±10℃—1005
℃±5℃—1020℃±10℃-980℃±30℃
Time be followed successively by 1h ± 10min, 1.5h ± 10min, 5h ± 10min, 2h ± 10min, 1h ± 10min, 1h ±
10min、1h±10min、2.5h±10min、1h±10min。
Further, in the ingredient, weight ratio is Nd 20.1%, B 0.74%, Cu 0.33%, Co 1.3%, Ga
0.38%, Zr0.7%, Nb 0.6%, Pr 5%, Al 0.7%, surplus Fe.
Further, in the ingredient, weight ratio is Nd 20.2%, B 0.76%, Cu 0.32%, Co 1.25%, Ga
0.32%, Zr0.76%, Nb 0.62%, Pr 5.6%, Al 0.75%, surplus Fe.
Further, in the ingredient, weight ratio is Nd 19.4%, B 0.73%, Cu 0.31%, Co 1.45%, Ga
0.34%, Zr0.72%, Nb 0.63%, Pr 5.8%, Al 0.78%, surplus Fe.
Further, it is static that the method includes high temperature;
The high temperature be still in slab after, hydrogen it is broken before, i.e., plates are placed in inert gas after slab and are heated
To 920-950 DEG C of static 1.5h-2h.
Further, during the compression moulding, the first 150 DEG C -170 DEG C of fine powder temperature, the second fine powder temperature 150
℃-170℃。
The present invention has the advantage that
1, pyrometallurgic methods are simple, effective, environmentally friendly.
2, neodymium iron boron magnet raw material compatibility made of present invention sintering is reasonable, and neodymium iron boron magnetic body magnetic property is high, corrosion resistance,
Inoxidizability, temperature stability are good.
3, plates (producing in slab) substantially eliminate slab static 1.5 hours to 2 hours in inert gas high temperature
In α-Fe phase, another slab reduces auxiliary alloy cast ingot oxygen content in the mode of vacuum copper mold casting, provides more for magnet
For the Nd-rich phase of intelligent richness, reduce oxygen content inside alloy.
3, praseodymium and neodymium iron boron magnet raw material carry out that hydrogen is quick-fried simultaneously, and the coarse crushing of neodymium iron boron magnet raw material powder uses hydride edge
The mode of crystalline substance fracture, is effectively protected the complete of crystal structure, while the brittleness of hydride is big, and powder processed is easy, and makes powder shape
The polyhedron pattern of rule is presented in looks, while fine powder generates reduction, effectively improves the size distribution of powder.By hydrogen it is broken and
Powder particle after air-flow milling, has monoclinic crystal structure, is not in twin crystal particle;Praseodymium produces praseodymium hydrogen during hydrogen is quick-fried
Object (praseodymium hydrogen object, which is added into neodymium iron boron magnet raw material, can make magnet crystal grain become round and smooth), compared to directly in neodymium iron boron magnetic body original
Material is directly added into praseodymium hydrogen object, and neodymium iron boron magnetic body can be made to generate bending strength and reach 265MPa or more, and bending strength is inclined
Difference is down to ± 4.5MPa, can increase substantially the consistency of magnet strength.
4, it is effectively controlled by the temperature to neodymium iron boron magnet raw material, makes neodymium iron boron magnet raw material from slab, hydrogen is broken, gas
Sub-sieve, powder processed, compression moulding, sintering are completed, and minimum temperature is not less than 90 degree or so, are conducive to discharge neodymium iron boron magnet raw material hydrogen
Gas, reduces the content of hydrogen in neodymium iron boron magnet raw material, and it is quick-fried to affecting iron boron magnet magnetic property to reduce hydrogen to greatest extent
It influences.
5, operating temperature reaches 150 degrees Celsius.
Detailed description of the invention
The SEML of plates institutional framework in Fig. 1, embodiment one after slab schemes.
By the SEML figure of the static sheet body tissue structure of high temperature in Fig. 2, embodiment one.
Fig. 3, gas screen-dividing machine structural schematic diagram.
The backscattered electron image figure of first neodymium iron boron magnetic body fracture in Fig. 4, embodiment one.
The backscattered electron image figure of second neodymium iron boron magnetic body fracture in Fig. 5, embodiment one.
The SEML of plates institutional framework in Fig. 6, embodiment two after slab schemes.
By the SEML figure of the static sheet body tissue structure of high temperature in Fig. 7, embodiment two.
The backscattered electron image figure of first neodymium iron boron magnetic body fracture in Fig. 8, embodiment two.
The backscattered electron image figure of second neodymium iron boron magnetic body fracture in Fig. 9, embodiment two.
Specific implementation
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment one:
A kind of method preparing neodymium iron boron magnetic body includes ingredient, slab, high temperature is static, hydrogen is broken, gas sub-sieve, powder processed, pressure
Type, sintering is made;
The ingredient, weight ratio be Nd 20.1%, B 0.74%, Cu 0.33%, Co 1.3%, Ga 0.38%,
Zr0.7%, Nb 0.6%, Pr 5%, Al 0.7%, surplus Fe, mixing generate mixture;
Mixture is delivered to slab furnace and carries out melting under vacuum by the slab, and smelting temperature is 1350-1390 DEG C,
And (the SEML figure of the plates institutional framework after slab as shown in figure 1, exists a large amount of the plates for being made with a thickness of 0.3-0.4mm
α-Fe phase);
The high temperature is static, after slab, before hydrogen is broken, i.e., plates is placed in inert gas after slab and is heated
To 920-950 DEG C of static 1.5h-2h, (the SEML figure such as α-Fe in Fig. 2 by the static plates institutional framework of high temperature is mutually basic
It disappears);
The hydrogen is broken, and by plates, (preferred, additive is praseodymium, and praseodymium weight is sheet body weight with additive
0.25%) hydrogen crushing furnace is inputted after mixing and progress hydrogen is quick-fried under vacuum conditions, vacuum degree 1.06-1.10Pa, temperature 450-
It 500 DEG C, generates primary product (temperature is at 400 DEG C or so);
The gas sub-sieve (sub-sieve principle is simple, but this really core of the invention protects point, by simple method,
Particle of the hydrogen after quick-fried less than 10 microns and the particle greater than 10 microns are carried out to separate processing, to prevent 1,2 micron of particle shadow
Subsequent technique is rung, total thinking is that the particle less than or equal to 10 microns is faster using lower temperature in following process
Speed is handled, and the particle greater than 10 microns is then with higher temperature that just slow speed is handled, and is very in laboratory
Above-mentioned steps are easily accomplished, but be really extremely not easy in commercial process), primary product is inputted into gas screen-dividing machine
(such as in Fig. 3), the gas screen-dividing machine include gravity box 1 (primary product is generally not less than 250 DEG C in the interior temperature of gravity box),
1 height of gravity box is 6-8 meters (low up to high score screen capacity, less than 6 meters sub-sieve effects do not reach requirement), and 1 upper end of gravity box is equipped with
Light phase export, lower end are equipped with heavy out, and (light phase export is equipped with filter screen to light phase export, and filter screen can be by being less than or equal to 10
The particle of micron, i.e. particle of the micron less than 10 microns can be also easy to produce 1-2 microns of grain in the quick-fried process of hydrogen by light phase export
Son, these particles enter subsequent powder link processed and can cause to aoxidize, and magnetic property and mechanical strength is caused to reduce) pass through the first negative pressure
Machine 2 and the first airflow milling (preferred, the first airflow milling is spiral jet pulverizer) connection, heavy out pass through the second Negative pressure machine 3
It is connect with the second airflow milling (the second airflow milling is circulating airflow milling), inert gas will by the feed pipe 4 among gravity box 1
Primary product is blown into gravity box 1, and the inert gas plenum speed is 0.25 meter per second, and the negative pressure that the first Negative pressure machine generates is 0.06
± 0.01MPa, the negative pressure that the second Negative pressure machine generates are 0.05 ± 0.01MPa;
Powder processed, the first airflow milling generate the first fine powder, and the second airflow milling generates the second fine powder;
Compression moulding, the first fine powder are delivered to the first moulding press, the first moulding press by the first fine powder hydrostatic profile,
Second fine powder directly transports the second moulding press, and the second moulding press is by the second fine powder hydrostatic profile;
The sintering, the first moulding press compacting material are input to the first vacuum sintering furnace, and the second moulding press compacting material is defeated
Enter to the second vacuum sintering furnace, the vacuum degree of the first vacuum sintering furnace is less than 8Pa, 940-1070 DEG C of sintering temperature, sintering time
For 13-15h, it is preferred that in the first vacuum sintering furnace sintering temperature gradient be followed successively by from start to finish 960 DEG C ± 20 DEG C-
1000℃±20℃—1045℃±25℃—1000℃±20℃—960℃±20℃—1010℃±30℃—960℃±
20 DEG C, the time is followed successively by 1h ± 10min, 2h ± 10min, 4h ± 10min, 2h ± 10min, 1h ± 10min, 2h ± 10min, 1h
±10min;The vacuum degree of second vacuum sintering furnace is less than 10Pa, 940-1090 DEG C of sintering temperature, sintering time 16-17h;It is excellent
Choosing, sintering temperature gradient is to be followed successively by 960 DEG C ± 20 DEG C -1010 DEG C ± 30 from start to finish in the second vacuum sintering furnace
℃—1065℃±25℃—1010℃±30℃—970℃±10℃—990℃±10℃—1005℃±5℃—1020℃
± 10 DEG C -980 DEG C ± 30 DEG C, the time be followed successively by 1h ± 10min, 1.5h ± 10min, 5h ± 10min, 2h ± 10min, 1h ±
10min、1h±10min、1h±10min、2.5h±10min、1h±10min。
In actual production, it is found that the temperature of sintering furnace is difficult to control in a homeostasis value, as have the temperature of 40-50 degree
Fluctuation, in order to ensure sintering quality, by test in 2 years, discovery can make sintering process along needs by artificial temperature control
Curve carry out, i.e., be first heated up to high temperature (1070 DEG C or 1090 DEG C) from low temperature (940 DEG C) and be then down to relative low temperature naturally again
(940 DEG C or 960 DEG C) heat again rise to relatively-high temperature (1040 DEG C or 1030 DEG C) later, are finally down to naturally and need temperature
(940 DEG C), then export logical inert gas and carry out cold really to natural temperature, above-mentioned temprature control method can make the temperature of sintering
Complete sintering in different silicon carbide, and it is also that can control that each different silicon carbides, which pour the knot time, temperature from it is low-
High-low-relatively high-low, being equivalent to the tempering of the high temperature realized during the sintering process, (i.e. sintering process and aging technique be not continuously
It is interrupted the novel thermal process technique of not converter), effectively improve neodymium iron boron magnetic body intrinsic coercivity and other parameters.
By above step, the first vacuum burns the product produced of furnace and generates the first neodymium iron boron magnetic body after cooling, and second
Vacuum burns the product that furnace is produced and generates the second neodymium iron boron magnetic body after cooling;
Such as the first neodymium iron boron magnetic body in Fig. 4, the second neodymium iron boron magnetic body in Fig. 5.
20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 275MPa ± 4.5MPa, and remanent magnetism (Br) is
1.42T, intrinsic coercivity (Hcj) are 1990kA/m, and magnetic energy product (BHmax) is 428.2kJ/m3;
80 DEG C of test temperature, the first neodymium iron boron magnetic body raw remanent magnetism (Br) is 1.39T, and intrinsic coercivity (Hcj) is 1904kA/
M, magnetic energy product (BHmax) are 418kJ/m3;
100 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.35T, and intrinsic coercivity (Hcj) is 1825kA/
M, magnetic energy product (BHmax) are 395kJ/m3;
120 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.305T, and intrinsic coercivity (Hcj) is 1645kA/
M, magnetic energy product (BHmax) are 345kJ/m3;
150 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.25T, and intrinsic coercivity (Hcj) is 1345kA/
M, magnetic energy product (BHmax) are 315kJ/m3;
20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 278MPa ± 3.5MPa, and remanent magnetism (Br) is
1.45T, intrinsic coercivity (Hcj) are 2065kA/m, and magnetic energy product (BHmax) is 432kJ/m3。
80 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.42T, and intrinsic coercivity (Hcj) is 1970kA/m,
Magnetic energy product (BHmax) is 423kJ/m3。
100 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.39T, and intrinsic coercivity (Hcj) is 1840kA/
M, magnetic energy product (BHmax) are 410kJ/m3;
120 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.32T, and intrinsic coercivity (Hcj) is 1665kA/
M, magnetic energy product (BHmax) are 385kJ/m3;
150 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.26T, and intrinsic coercivity (Hcj) is 1445kA/
M, magnetic energy product (BHmax) are 355kJ/m3;
As can be seen from the above test results that neodymium iron boron magnetic body performance is ideal, (generally requires and reach praseodymium is greatly reduced
2775MPa intensity, needs at least to add the praseodymium hydride of the 0.8-0.9% of compound total weight, but is applied in example 1 in this patent only
It is added to the praseodymium of 0.25% compound total weight, is converted into praseodymium hydride namely 0.4% or so) in the case where dosage, at least
Reach 275MPa intensity, and intrinsic coercivity, under 20 degree and 80 degree of state of temperatures, changing value is less than 18%, it is however generally that interior
Coercivity is reported at 20 degree under 80 degree of state of temperatures, changing value is greater than 25%.
Embodiment two:
A kind of method preparing neodymium iron boron magnetic body includes ingredient, slab, high temperature is static, hydrogen is broken, gas sub-sieve, powder processed, pressure
Type, sintering is made;
The ingredient, weight ratio be Nd 20.2%, B 0.76%, Cu 0.32%, Co 1.25%, Ga 0.32%,
Zr0.76%, Nb 0.62%, Pr 5.6%, Al 0.75%, surplus Fe, mixing generate mixture;
Mixture is delivered to slab furnace and carries out melting under vacuum by the slab, and smelting temperature is 1460-1480 DEG C,
And it is made and (in SEML figure such as Fig. 6 of the plates institutional framework after slab, exists a large amount of with a thickness of the plates of 0.3-0.4mm
α-Fe phase);
The high temperature is static, after slab, before hydrogen is broken, i.e., plates is placed in inert gas after slab and is heated
To 920-950 DEG C of static 2h (SEML figure α-Fe mutually basic disappearance such as in Fig. 7 by the static plates institutional framework of high temperature);
The hydrogen is broken, and by plates, (preferred, additive is praseodymium, and praseodymium weight is sheet body weight with additive
0.27%) hydrogen crushing furnace is inputted after mixing and progress hydrogen is quick-fried under vacuum conditions, vacuum degree 1.06-1.08Pa, temperature 450-
It 500 DEG C, generates primary product (temperature is at 420 DEG C or so);
The gas sub-sieve (sub-sieve principle is simple, but this really core of the invention protects point, by simple method,
Particle of the hydrogen after quick-fried less than 10 microns and the particle greater than 10 microns are carried out to separate processing, to prevent 1,2 micron of particle shadow
Subsequent technique is rung, total thinking is that the particle less than or equal to 10 microns is faster using lower temperature in following process
Speed is handled, and the particle greater than 10 microns is then with higher temperature that just slow speed is handled, and is very in laboratory
Above-mentioned steps are easily accomplished, but be really extremely not easy in commercial process), primary product is inputted into gas screen-dividing machine
(such as in Fig. 3), the gas screen-dividing machine include gravity box 1 (primary product is generally not less than 260 DEG C in the interior temperature of gravity box),
1 height of gravity box is 6-8 meters (low up to high score screen capacity, less than 6 meters sub-sieve effects do not reach requirement), and 1 upper end of gravity box is equipped with
Light phase export, lower end are equipped with heavy out, and (light phase export is equipped with filter screen to light phase export, and filter screen can be by being less than or equal to 10
The particle of micron, i.e. particle of the micron less than 10 microns can be also easy to produce 1-2 microns of grain in the quick-fried process of hydrogen by light phase export
Son, these particles enter subsequent powder link processed and can cause to aoxidize, and magnetic property and mechanical strength is caused to reduce) pass through the first negative pressure
Machine 2 and the first airflow milling (preferred, the first airflow milling is spiral jet pulverizer) connection, heavy out pass through the second Negative pressure machine 3
It is connect with the second airflow milling (the second airflow milling is circulating airflow milling), inert gas will by the feed pipe 4 among gravity box 1
Primary product is blown into gravity box 1, and the inert gas plenum speed is 0.25 meter per second, and the negative pressure that the first Negative pressure machine generates is 0.06
± 0.01MPa, the negative pressure that the second Negative pressure machine generates are 0.05 ± 0.01MPa;
Powder processed, the first airflow milling generate the first fine powder, and the second airflow milling generates the second fine powder;
Compression moulding, the first fine powder are delivered to the first moulding press, the first moulding press by the first fine powder hydrostatic profile,
Second fine powder directly transports the second moulding press, and the second moulding press is by the second fine powder hydrostatic profile;
The sintering, the first moulding press compacting material are input to the first vacuum sintering furnace, and the second moulding press compacting material is defeated
Enter to the second vacuum sintering furnace, the vacuum degree of the first vacuum sintering furnace is less than 8Pa, 940-1070 DEG C of sintering temperature, sintering time
For 13-15h, it is preferred that in the first vacuum sintering furnace sintering temperature gradient be followed successively by from start to finish 960 DEG C ± 20 DEG C-
1000℃±20℃—1045℃±25℃—1000℃±20℃—960℃±20℃—1010℃±30℃—960℃±
20 DEG C, the time is followed successively by 1h ± 10min, 2h ± 10min, 4h ± 10min, 2h ± 10min, 1h ± 10min, 2h ± 10min, 1h
±10min;The vacuum degree of second vacuum sintering furnace is less than 10Pa, 940-1090 DEG C of sintering temperature, sintering time 16-17h;It is excellent
Choosing, sintering temperature gradient is to be followed successively by 960 DEG C ± 20 DEG C -1010 DEG C ± 30 from start to finish in the second vacuum sintering furnace
℃—1065℃±25℃—1010℃±30℃—970℃±10℃—990℃±10℃—1005℃±5℃—1020℃
± 10 DEG C -980 DEG C ± 30 DEG C, the time be followed successively by 1h ± 10min, 1.5h ± 10min, 5h ± 10min, 2h ± 10min, 1h ±
10min、1h±10min、1h±10min、2.5h±10min、1h±10min。
By above step, the first vacuum burns the product produced of furnace and generates the first neodymium iron boron magnetic body after cooling, and second
Vacuum burns the product that furnace is produced and generates the second neodymium iron boron magnetic body after cooling;
Such as the first neodymium iron boron magnetic body in Fig. 8, the second neodymium iron boron magnetic body in Fig. 9.
20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 280MPa ± 4.5MPa, and remanent magnetism (Br) is
1.43T, intrinsic coercivity (Hcj) are 2030kA/m, and magnetic energy product (BHmax) is 436kJ/m3;
80 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.412T, and intrinsic coercivity (Hcj) is 1962kA/
M, magnetic energy product (BHmax) are 421kJ/m3;
100 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.38T, and intrinsic coercivity (Hcj) is 1875kA/
M, magnetic energy product (BHmax) are 410kJ/m3;
120 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.33T, and intrinsic coercivity (Hcj) is 1695kA/
M, magnetic energy product (BHmax) are 379kJ/m3;
150 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.26T, and intrinsic coercivity (Hcj) is 1415kA/
M, magnetic energy product (BHmax) are 349kJ/m3;
20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 282MPa ± 3.5MPa, and remanent magnetism (Br) is
1.46T, intrinsic coercivity (Hcj) are 2120kA/m, and magnetic energy product (BHmax) is 450kJ/m3。
80 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.43T, and intrinsic coercivity (Hcj) is 2060kA/m,
Magnetic energy product (BHmax) is 430kJ/m3。
100 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.4T, and intrinsic coercivity (Hcj) is 1940kA/m,
Magnetic energy product (BHmax) is 410kJ/m3;
120 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.36T, and intrinsic coercivity (Hcj) is 1765kA/
M, magnetic energy product (BHmax) are 375kJ/m3;
150 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.3T, and intrinsic coercivity (Hcj) is 1625kA/m,
Magnetic energy product (BHmax) is 335kJ/m3;
As can be seen from the above test results that neodymium iron boron magnetic body performance is ideal, (generally requires and reach praseodymium is greatly reduced
280MPa intensity, needs at least to add about 1% praseodymium hydride of compound total weight, but applies in this patent in example 2 and only add
The praseodymium of 0.25% compound total weight, is converted into praseodymium hydride namely 0.5% or so) in the case where dosage, at least up to
277MPa intensity, and intrinsic coercivity, under 20 degree to 80 degree state of temperatures, changing value is less than 10%, it is however generally that it is intrinsic to rectify
Stupid power is greater than 15% with changing value under 80 degree of state of temperatures at 20 degree.
Embodiment three:
A kind of method preparing neodymium iron boron magnetic body includes ingredient, slab, high temperature is static, hydrogen is broken, gas sub-sieve, powder processed, pressure
Type, sintering is made;
Ingredient, weight ratio be Nd 19.4%, B 0.73%, Cu 0.31%, Co 1.45%, Ga 0.34%,
Zr0.72%, Nb 0.63%, Pr 5.8%, Al 0.78%, surplus Fe, mixing generate mixture;
Mixture is delivered to slab furnace and carries out melting under vacuum by slab, and smelting temperature is 1460-1480 DEG C, and is made
At the plates with a thickness of 0.3-0.4mm;
The high temperature is static, after slab, before hydrogen is broken, i.e., plates is placed in inert gas after slab and is heated
To 920-950 DEG C of static 1.5-2h;
The hydrogen is broken, and by plates, (preferred, additive is praseodymium, and praseodymium weight is the 0.26- of sheet body weight with additive
0.265%) hydrogen crushing furnace is inputted after mixing and progress hydrogen is quick-fried under vacuum conditions, vacuum degree 1.06-1.08Pa, and temperature is
It 450-500 DEG C, generates primary product (temperature is at 420 DEG C or so);
The gas sub-sieve (sub-sieve principle is simple, but this really core of the invention protects point, by simple method,
Particle of the hydrogen after quick-fried less than 10 microns and the particle greater than 10 microns are carried out to separate processing, to prevent 1,2 micron of particle shadow
Subsequent technique is rung, total thinking is that the particle less than or equal to 10 microns is faster using lower temperature in following process
Speed is handled, and the particle greater than 10 microns is then with higher temperature that just slow speed is handled, and is very in laboratory
Above-mentioned steps are easily accomplished, but be really extremely not easy in commercial process), primary product is inputted into gas screen-dividing machine
(such as in Fig. 3), the gas screen-dividing machine include gravity box 1 (primary product is generally not less than 260 DEG C in the interior temperature of gravity box),
1 height of gravity box is 6-8 meters (low up to high score screen capacity, less than 6 meters sub-sieve effects do not reach requirement), and 1 upper end of gravity box is equipped with
Light phase export, lower end are equipped with heavy out, and (light phase export is equipped with filter screen to light phase export, and filter screen can be by being less than or equal to 10
The particle of micron, i.e. particle of the micron less than 10 microns can be also easy to produce 1-2 microns of grain in the quick-fried process of hydrogen by light phase export
Son, these particles enter subsequent powder link processed and can cause to aoxidize, and magnetic property and mechanical strength is caused to reduce) pass through the first negative pressure
Machine 2 and the first airflow milling (preferred, the first airflow milling is spiral jet pulverizer) connection, heavy out pass through the second Negative pressure machine 3
It is connect with the second airflow milling (the second airflow milling is circulating airflow milling), inert gas will by the feed pipe 4 among gravity box 1
Primary product is blown into gravity box 1, and the inert gas plenum speed is 0.25 meter per second, and the negative pressure that the first Negative pressure machine generates is 0.06
± 0.01MPa, the negative pressure that the second Negative pressure machine generates are 0.05 ± 0.01MPa;
Powder processed, the first airflow milling generate the first fine powder, and the second airflow milling generates the second fine powder;
Compression moulding, the first fine powder are delivered to the first moulding press, the first moulding press by the first fine powder hydrostatic profile,
Second fine powder directly transports the second moulding press, and the second moulding press is by the second fine powder hydrostatic profile;
The sintering, the first moulding press compacting material are input to the first vacuum sintering furnace, and the second moulding press compacting material is defeated
Enter to the second vacuum sintering furnace, the vacuum degree of the first vacuum sintering furnace is less than 8Pa, 940-1070 DEG C of sintering temperature, sintering time
For 13-15h, it is preferred that in the first vacuum sintering furnace sintering temperature gradient be followed successively by from start to finish 960 DEG C ± 20 DEG C-
1000℃±20℃—1045℃±25℃—1000℃±20℃—960℃±20℃—1010℃±30℃—960℃±
20 DEG C, the time is followed successively by 1h ± 10min, 2h ± 10min, 4h ± 10min, 2h ± 10min, 1h ± 10min, 2h ± 10min, 1h
±10min;The vacuum degree of second vacuum sintering furnace is less than 10Pa, 940-1090 DEG C of sintering temperature, sintering time 16-17h;It is excellent
Choosing, sintering temperature gradient is to be followed successively by 960 DEG C ± 20 DEG C -1010 DEG C ± 30 from start to finish in the second vacuum sintering furnace
℃—1065℃±25℃—1010℃±30℃—970℃±10℃—990℃±10℃—1005℃±5℃—1020℃
± 10 DEG C -980 DEG C ± 30 DEG C, the time be followed successively by 1h ± 10min, 1.5h ± 10min, 5h ± 10min, 2h ± 10min, 1h ±
10min、1h±10min、1h±10min、2.5h±10min、1h±10min。
By above step, the first vacuum burns the product produced of furnace and generates the first neodymium iron boron magnetic body after cooling, and second
Vacuum burns the product that furnace is produced and generates the second neodymium iron boron magnetic body after cooling;
First neodymium iron boron magnetic body, the second neodymium iron boron magnetic body.
20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 277MPa ± 4.5MPa, and remanent magnetism (Br) is
1.419T, intrinsic coercivity (Hcj) are 2050kA/m, and magnetic energy product (BHmax) is 427kJ/m3;
80 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.39T, and intrinsic coercivity (Hcj) is 1910kA/m,
Magnetic energy product (BHmax) is 418kJ/m3;
100 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.346T, and intrinsic coercivity (Hcj) is 1823kA/
M, magnetic energy product (BHmax) are 395kJ/m3;
120 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.3T, and intrinsic coercivity (Hcj) is 1640kA/m,
Magnetic energy product (BHmax) is 342kJ/m3;
150 DEG C of test temperature, the first neodymium iron boron magnetic body remanent magnetism (Br) is 1.248T, and intrinsic coercivity (Hcj) is 1339kA/
M, magnetic energy product (BHmax) are 314J/m3;
20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 280MPa ± 3.5MPa, and remanent magnetism (Br) is
1.45T, intrinsic coercivity (Hcj) are 2075kA/m, and magnetic energy product (BHmax) is 435kJ/m3。
80 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.42T, and intrinsic coercivity (Hcj) is 1972kA/m,
Magnetic energy product (BHmax) is 423kJ/m3。
100 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.392T, and intrinsic coercivity (Hcj) is 1845kA/
M, magnetic energy product (BHmax) are 410kJ/m3;
120 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.33T, and intrinsic coercivity (Hcj) is 1698kA/
M, magnetic energy product (BHmax) are 388kJ/m3;
150 DEG C of test temperature, the second neodymium iron boron magnetic body remanent magnetism (Br) is 1.27T, and intrinsic coercivity (Hcj) is 1480kA/
M, magnetic energy product (BHmax) are 370kJ/m3;
As can be seen from the above test results that neodymium iron boron magnetic body performance is ideal, (generally requires and reach praseodymium is greatly reduced
276MPa intensity, needs at least to add the praseodymium hydride of the about 0.8-0.9% of compound total weight, but is applied in example 3 in this patent
It is only added to the praseodymium of 0.26-0.265% compound total weight, is converted into praseodymium hydride namely 0.55% or so) feelings of dosage
Under condition, at least up to 276MPa intensity, and intrinsic coercivity is under 20 degree to 80 degree state of temperatures, changing value less than 10%,
In general intrinsic coercivity is greater than 15% with changing value under 80 degree of state of temperatures at 20 degree.
In conclusion next with test result from the magnetic property of the neodymium iron boron magnetic body in embodiment one, two, three, high-temperature behavior
It sees, the neodymium iron boron magnetic body magnetic property with higher that the present invention is produced with this method, preferable temperature stability, and passes through change
The addition manner of praseodymium, the dosage for considerably reducing praseodymium simultaneously, also improve neodymium iron boron magnetic body bending strength and generally reach
275MPa intensity also greatly improves the stability of neodymium iron boron magnetic body bending strength, strong from the bending resistance for not adding praseodymium compound originally
Degree fluctuation 15MPa drop to fluctuation 4.5MPa, the dosage that another reason reduces praseodymium compound can prevent neodymium-iron-boron volume density and
The too fast decline of magnetic energy product numerical value, reducing influence of the praseodymium compound to the other physicochemical properties of neodymium iron boron magnetic body, (the addition of praseodymium compound the how high
Neodymium-iron-boron volume density and magnetic energy product numerical value can decline, for the neodymium iron boron magnetic body of no addition praseodymium compound), this hair
It is bright, make neodymium iron boron magnetic body with preferable magnetic energy product (BHmax), while also having compared with high-flexural strength.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can do various modifications or supplement or is substituted in a similar manner to described specific embodiment, but simultaneously
Spirit or beyond the scope defined by the appended claims of the invention is not deviated by.
Claims (10)
1. a kind of method for preparing neodymium iron boron magnetic body, it is characterised in that: the method includes ingredient, slab, hydrogen is broken, gas point
It sieves, powder processed, compression moulding, sintering;
The ingredient, weight ratio be Nd 19~20.5%, B 0.7~0.8%, Cu 0.3~0.35%, Co 1.2~1.5%,
Ga 0.3~0.4%, Zr0.7~0.8%, Nb 0.6~0.7%, Pr 5~6%, Al 0.7~0.9%, surplus Fe are mixed
Symphysis is at mixture;
Mixture is delivered to slab furnace and carries out melting under vacuum by the slab, and smelting temperature is 1350-1480 DEG C, and is made
At the plates with a thickness of 0.3-0.4mm;
The hydrogen is broken, and hydrogen crushing furnace is inputted after plates are mixed with additive and progress hydrogen is quick-fried under vacuum conditions, vacuum degree is
1.06-1.11Pa, temperature are 400-600 DEG C, generate primary product;
Primary product is inputted gas screen-dividing machine by the gas sub-sieve, and the gas screen-dividing machine includes gravity box, gravity box height
It is 6-8 meters, gravity box upper end is equipped with light phase export, lower end is equipped with heavy out, and light phase export passes through the first Negative pressure machine and first
Airflow milling connection, heavy out are connect by the second Negative pressure machine with the second airflow milling, inert gas pass through among gravity box into
Primary product is blown into gravity box by expects pipe, and the inert gas plenum speed is 0.2 to 0.3 meter per second, what the first Negative pressure machine generated
Negative pressure is 0.06 ± 0.01MPa, and the negative pressure that the second Negative pressure machine generates is 0.05 ± 0.01MPa;
The powder processed, the first airflow milling generate the first fine powder, and the second airflow milling generates the second fine powder;
The compression moulding, the first fine powder are delivered to the first moulding press, the first moulding press by the first fine powder hydrostatic profile,
Second fine powder directly transports the second moulding press, and the second moulding press is by the second fine powder hydrostatic profile;
The sintering, the first moulding press compacting material are input to the first vacuum sintering furnace, and the second moulding press compacting material is input to
The vacuum degree of second vacuum sintering furnace, the first vacuum sintering furnace is less than 8Pa, 940-1070 DEG C of sintering temperature, sintering time 13-
The vacuum degree of 15h, the second vacuum sintering furnace are less than 10Pa, 940-1090 DEG C of sintering temperature, sintering time 16-17h;
By above step, the first vacuum burns the product that furnace is produced and generates the first neodymium iron boron magnetic body, the second vacuum after cooling
It burns the product that furnace is produced and generates the second neodymium iron boron magnetic body after cooling;
20 DEG C of test temperature, the first neodymium iron boron magnetic body generates bending strength and reaches 275MPa or more, and remanent magnetism (Br) >=1.27T is interior
Coercivity (Hcj) >=1670kA/m is reported, magnetic energy product (BHmax) is >=335kJ/m3;
20 DEG C of test temperature, the second neodymium iron boron magnetic body generates bending strength and reaches 278MPa or more, and remanent magnetism (Br) >=1.32T is interior
Coercivity (Hcj) >=1750kA/m is reported, magnetic energy product (BHmax) is >=363kJ/m3。
2. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: the additive is praseodymium, praseodymium
Weight is the 0.2~0.3% of sheet body weight.
3. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: first airflow milling is flat
Flat airflow milling;Second airflow milling is circulating airflow milling.
4. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: first vacuum sintering furnace
Interior sintering temperature gradient be followed successively by from start to finish 960 DEG C ± 20 DEG C -1000 DEG C ± 20 DEG C -1045 DEG C ± 25 DEG C -
1000 DEG C ± 20 DEG C -960 DEG C ± 20 DEG C -1020 DEG C ± 30 DEG C -960 DEG C ± 20 DEG C, the time be followed successively by 1h ± 10min, 2h ±
10min、4h±10min、2h±10min、1h±10min、2h±10min、1h±10min。
5. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: second vacuum sintering furnace
Interior sintering temperature gradient be followed successively by from start to finish 960 DEG C ± 20 DEG C -1010 DEG C ± 30 DEG C -1065 DEG C ± 25 DEG C -
1010℃±30℃—970℃±10℃—990℃±10℃—1005℃±5℃—1020℃±10℃-980℃±30℃
Time be followed successively by 1h ± 10min, 1.5h ± 10min, 5h ± 10min, 2h ± 10min, 1h ± 10min, 1h ± 10min,
1h±10min、2.5h±10min、1h±10min。
6. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: in the ingredient, weight ratio
For Nd20.1%, B0.74%, Cu0.33%, Co1.3%, Ga0.38%, Zr0.7%, Nb0.6%, Pr5%, Al0.7%, remaining
Amount is Fe.
7. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: in the ingredient, weight ratio
For Nd20.2%, B0.76%, Cu0.32%, Co1.25%, Ga0.32%, Zr0.76%, Nb0.62%, Pr5.6%,
Al0.75%, surplus Fe.
8. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: in the ingredient, weight ratio
For Nd19.4%, B0.73%, Cu0.31%, Co1.45%, Ga0.34%, Zr0.72%, Nb0.63%, Pr5.8%,
Al0.78%, surplus Fe.
9. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: that the method includes high temperature is quiet
Only;
The high temperature be still in slab after, hydrogen it is broken before, i.e., plates are placed in inert gas after slab and are heated up to
920-950 DEG C of static 1.5h-2h.
10. a kind of method for preparing neodymium iron boron magnetic body according to claim 1, it is characterized in that: the compression moulding process
In, the first powder material temperature is not less than 100 DEG C, and the second powder material temperature is not less than 100 DEG C.
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