CN103805826B - NdFeB iron-based composite diphase material sintering process - Google Patents
NdFeB iron-based composite diphase material sintering process Download PDFInfo
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- CN103805826B CN103805826B CN201410019305.7A CN201410019305A CN103805826B CN 103805826 B CN103805826 B CN 103805826B CN 201410019305 A CN201410019305 A CN 201410019305A CN 103805826 B CN103805826 B CN 103805826B
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Abstract
A kind of NdFeB iron-based composite diphase material sintering process disclosed by the invention, in the process, neodymium iron boron blank steps d made first carries out microwave sintering process by step e, from inside to outside heats blank; And then carry out conventional sintering technique by step f, blank is heated from outside to inside; By this kind of mode sintered Nd Fe B iron-based composite diphase material, there is following characteristics: the NdFeB iron-based composite diphase material internal stress sintered by this kind of mode is little, homogeneous grain size, make in punching, ground finish not cracked; Solve the problem that microwave sintering can only be used for processing miscellaneous goods; Significantly can reduce sintering temperature; Significantly reduce energy consumption; Shorten sintering time; Significantly improve dense structure's degree, crystal grain thinning, improve material property.
Description
Technical field
The present invention relates to NdFeB(Sintered NdFeB magnet) iron-based composite diphase material sintering process.
Background technology
In the conventional sintering technique of NdFeB iron-based composite diphase material, heating utilizes resistive heating, by convection current, radiation and conduction three kinds of modes, the heat of heating element is passed to product, direction of heat flow points to heart portion from product surface, forms product surface temperature high, the temperature field that heart portion temperature is low.When product size is comparatively large or thermal conductivity is poor, easily in product, produce larger internal stress.Once internal stress higher than the yield strength of product material or tensile strength, product can deform in heat-processed, even ftractures.
Microwave sintering utilizes microwave heating to sinter material, and it is different from traditional type of heating.Microwave sintering is then that the basic fine particle of special wave band and the material utilizing microwave to have is coupled and makes molecule strenuous exercise produce heat, and the dielectric loss of material makes its material monolithic be heated to sintering temperature and realize the method for densification.Microwave sintering is a kind of novel method of material sintering process, it has that heat-up rate is fast, energy utilization rate is high, high thermal efficiency is high and the feature such as safety and sanitation are pollution-free, and homogeneity and the yield rate of product can be improved, improve the microstructure and properties being sintered material, become study hotspot new in material sintering art.But easily there is the phenomenon (restriction by wavelength) of non-uniform heating for large size, complex-shaped sample in microwave sintering, is applied to by microwave sintering in sintered Nd Fe B iron-based composite diphase material, can only be used for processing small dimension, little weight product.
Summary of the invention
Technical problem to be solved by this invention is, there is provided a kind of NdFeB iron-based composite diphase material sintering process, the NdFeB iron-based composite diphase material internal stress of sintering is little, preparation technology is simple and convenient, energy consumption is low, sintering time is short, safety and sanitation are pollution-free and sintering is not limited to size and the weight of NdFeB iron-based composite diphase material.
For solving the problems of the technologies described above, the invention provides a kind of NdFeB iron-based composite diphase material sintering process, it comprises the following steps:
A, be by weight percentage Nd26.4-28.6%, Dy7.44-5.42%, Fe59.74-60.75%, Co4.45-3.55%, B0.98-1.08%, Ga0.9-1.8% ratio batching, above-mentioned each weight percentages of components sum is 100%; Joined material is loaded smelting furnace, through vacuumizing, be vented, argon filling, refining procedure, refine into slab;
B, the slab made by step a carry out hydrogen treatment: feed, vacuumize, inhale that hydrogen, hydrogen are broken, dehydrogenation, cooling come out of the stove; Obtain below 0.5mm powder;
C, the powder made by step b join airflow milling, carry out powder process processing, obtain the powder of 3-4um;
D, the powder made by step c obtain blank through die-filling, the orientation that magnetizes, pressurization, then improve density through isostatic pressed;
E, blank steps d made carry out sabot, then put into the sintering oven being provided with microwave device, carry out microwave sintering process: open microwave device, vacuumize, be heated to 310-400 DEG C of insulation, insulation 30-120 minute, exit, be heated to 855-900 DEG C of insulation, insulation 1-4 hour, dehydrogenation, the fixed crystalline substance of product;
F, close microwave device, the blank that step e is burned in advance proceeds to vacuum sintering technology: be 10 in vacuum tightness
-2be heated to 960-1020 DEG C of insulation under the high vacuum of more than Pa, soaking time 1-2 hour, cooling come out of the stove, complete NdFeB iron-based composite diphase material sintering process.
After adopting above structure, NdFeB iron-based composite diphase material sintering process of the present invention compared with prior art, has the following advantages:
In NdFeB iron-based composite diphase material sintering process of the present invention, neodymium iron boron blank steps d made first carries out microwave sintering process by step e, from inside to outside heats blank; And then carry out conventional sintering technique by step f, blank is heated from outside to inside; By this kind of mode sintered Nd Fe B iron-based composite diphase material, there is following characteristics: the NdFeB iron-based composite diphase material internal stress sintered by this kind of mode is little, homogeneous grain size, make in punching, ground finish not cracked; Solve the problem that microwave sintering can only be used for processing miscellaneous goods; Significantly can reduce sintering temperature; Significantly reduce energy consumption; Shorten sintering time; Significantly improve dense structure's degree, crystal grain thinning, improve material property.
Accompanying drawing explanation
Fig. 1 is the metallograph of the NdFeB iron-based composite diphase material that conventional sintering processes.
Fig. 2 is the metallograph of the NdFeB iron-based composite diphase material that NdFeB iron-based composite diphase material sintering process of the present invention processes.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in more detail.
NdFeB iron-based composite diphase material sintering process of the present invention, it comprises the following steps:
A, be by weight percentage Nd26.4-28.6%, Dy7.44-5.42%, Fe59.74-60.75%, Co4.45-3.55%, B0.98-1.08%, Ga0.9-1.8% ratio batching, above-mentioned each weight percentages of components sum is 100%; Joined material is loaded smelting furnace, through vacuumizing, be vented, argon filling, refining procedure, refine into slab;
B, the slab made by step a carry out hydrogen treatment: feed, vacuumize, inhale that hydrogen, hydrogen are broken, dehydrogenation, cooling come out of the stove; Obtain below 0.5mm powder;
C, the powder made by step b join airflow milling, carry out powder process processing, obtain the powder of 3-4um;
D, the powder made by step c obtain blank through die-filling, the orientation that magnetizes, pressurization, then improve density through isostatic pressed;
E, blank steps d made carries out sabot, then the sintering oven being provided with microwave device is put into, carry out microwave sintering process: open microwave device, vacuumize, be heated to 310-400 DEG C of insulation, insulation 30-120 minute, (venting refers in the course of processing in venting, argon gas is had in the gap of powder, nitrogen, the shielding gas such as anti-oxidation gas, can discharge in the process of heating, the gas these discharged is needed to release), be heated to 855-900 DEG C of insulation, insulation 1-4 hour, (powder is in the broken process of hydrogen in dehydrogenation, hydrogen can react with rich neodymium phase and principal phase and form hydride, residual hydrogen is removed further) in the process of microwave sintering, product is fixed brilliant (in sintering process, keep the orientation degree of die mould orientation),
F, closedown microwave device, the blank that step e is burned in advance proceeds to vacuum sintering technology, is 10 in vacuum tightness
-2be heated to 960-1020 DEG C of insulation under the high vacuum of more than Pa, soaking time 1-2 hour, cooling come out of the stove, complete NdFeB iron-based composite diphase material sintering process.
Traditional NdFeB iron-based composite diphase material sintering process is compared with NdFeB iron-based composite diphase material sintering process of the present invention, the mode of sintering is different: in the sintering step of traditional NdFeB iron-based composite diphase material microwave sintering process, the blank made by above-mentioned steps d carries out sabot, then put into gas to quench vacuum sintering furnace, vacuumize, be heated to 320 DEG C, insulation venting, be heated to 855 DEG C, insulation dehydrogenation, be heated to 1020-1100 DEG C under high vacuum, insulation 4-8 hour, cooling come out of the stove.
The NdFeB iron-based composite diphase material sintering out by the NdFeB iron-based composite diphase material sintering out by microwave sintering process of the present invention and traditional sintering process carries out the comparison of magnetic property and machining property etc.:
Embodiment:
A, be by weight percentage Nd26.4%, Dy5.42%, Fe62.3%, Co4.0%, B0.98%, Ga0.9% ratio batching; Joined material is loaded smelting furnace, through vacuumizing, be vented, argon filling, refining procedure, refine into slab;
B, the slab made by step a carry out hydrogen treatment: feed, vacuumize, inhale that hydrogen, hydrogen are broken, dehydrogenation, cooling come out of the stove; Obtain below 0.5mm powder;
C, the powder made by step b join airflow milling, carry out powder process processing, obtain the powder of 3.6um;
D, the powder made by step c obtain blank through die-filling, the orientation that magnetizes, pressurization, then improve density through isostatic pressed;
E, blank steps d made carry out sabot, then put into the sintering oven being provided with microwave device, carry out microwave sintering process: open microwave device, vacuumize, be heated to 380 DEG C of insulations, insulation 40 minutes, exit, be heated to 890 DEG C of insulations, insulation 1 hour, dehydrogenation, the fixed crystalline substance of product;
F, closedown microwave device, the blank that step e is burned in advance proceeds to vacuum sintering technology, is 8*10 in vacuum tightness
-2be heated to 1000 DEG C of insulations, soaking time 1 hour under the high vacuum of Pa, cool and come out of the stove, complete NdFeB iron-based composite diphase material sintering process.
One, conventional sintering processing
Performance index:
Br：1.328T
Hcj：1272.8kA/m
(BH)max：345.54kJ/m3
Hk：1248.9kA/m
Hk/Hcj：98%
Fig. 1 is the metallograph of the NdFeB iron-based composite diphase material that conventional sintering processes, and grain size is uneven, frangible in punching, ground finish, makees smallclothes yield rate extremely low.
Two, the present invention sinters processing
Performance index:
Br：1.351
Hcj：1355.2kA/m
(BH)max：363.2kJ/m3
Hk：1332.9kA/m
Hk/Hcj：98.5%
Fig. 2 is the metallograph of the NdFeB iron-based composite diphase material that present invention process processes, homogeneous grain size, not cracked in punching, ground finish, can make the smallclothes finished product of 0.5mm wall thickness, improves Application Areas.
Sintering process of the present invention, compared with traditional sintering process, has the following advantages:
1, the NdFeB iron-based composite diphase material internal stress sintered by this kind of mode is little, homogeneous grain size, makes in punching, ground finish not cracked;
2, the problem that microwave sintering can only be used for miscellaneous goods is solved;
3, significantly can reduce sintering temperature, maximum amplitude can reach 200 DEG C;
4, significantly energy consumption is reduced, energy-conservation up to 50-60%;
5, shorten sintering time, can more than 50% be reached;
6, significantly improve dense structure's degree, crystal grain thinning, improve material property.
Remarks: in the microwave sintering process in NdFeB iron-based composite diphase material sintering process of the present invention, use metal sintering boat meeting microwave reflection; Therefore non-metal kind sintering boat must be adopted, as the sintering boat such as graphite, quartz can be adopted.
Claims (1)
1. a NdFeB iron-based composite diphase material sintering process, it comprises the following steps:
A, be by weight percentage Nd26.4-28.6%, Dy7.44-5.42%, Fe59.74-60.75%, Co4.45-3.55%, B0.98-1.08%, Ga0.9-1.8% ratio batching, above-mentioned each weight percentages of components sum is 100%; Joined material is loaded smelting furnace, through vacuumizing, be vented, argon filling, refining procedure, refine into slab;
B, the slab made by step a carry out hydrogen treatment: feed, vacuumize, inhale that hydrogen, hydrogen are broken, dehydrogenation, cooling come out of the stove; Obtain below 0.5mm powder;
C, the powder made by step b join airflow milling, carry out powder process processing, obtain the powder of 3-4um;
D, the powder made by step c obtain blank through die-filling, the orientation that magnetizes, pressurization, then improve density through isostatic pressed;
E, blank steps d made carry out sabot, then put into the sintering oven being provided with microwave device, carry out microwave sintering process: open microwave device, vacuumize, be heated to 310-400 DEG C of insulation, insulation 30-120 minute, exit, be heated to 855-900 DEG C of insulation, insulation 1-4 hour, dehydrogenation, the fixed crystalline substance of product;
F, close microwave device, the blank that step e is burned in advance proceeds to vacuum sintering technology: be 10 in vacuum tightness
-2be heated to 960-1020 DEG C of insulation under the high vacuum of more than Pa, soaking time 1-2 hour, cooling come out of the stove, complete NdFeB iron-based composite diphase material sintering process.
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| CN104934212B (en) * | 2015-02-15 | 2017-04-05 | 宁波招宝磁业有限公司 | A kind of preparation method of thermally-stabilised neodymium iron boron magnetic body |
| CN108749207A (en) * | 2018-03-28 | 2018-11-06 | 天长市蓝天复合材料有限公司 | A kind of double glazing steel grating and preparation method |
| CN111370219B (en) * | 2020-04-22 | 2021-07-20 | 安徽吉华新材料有限公司 | Preparation process for producing new permanent magnet by full-cycle recycling of neodymium iron boron waste magnetic steel |
| CN114334422A (en) * | 2021-12-31 | 2022-04-12 | 湖南稀土新能源材料有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
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