CN105551707A - Neodymium iron boron magnet raw material powder and treatment process therefor - Google Patents
Neodymium iron boron magnet raw material powder and treatment process therefor Download PDFInfo
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- CN105551707A CN105551707A CN201610104827.6A CN201610104827A CN105551707A CN 105551707 A CN105551707 A CN 105551707A CN 201610104827 A CN201610104827 A CN 201610104827A CN 105551707 A CN105551707 A CN 105551707A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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Abstract
The invention provides neodymium iron boron magnet raw material powder. The neodymium iron boron magnet raw material powder comprises neodymium iron boron raw material thin powder and a nickel layer coating the surface of the neodymium iron boron raw material thin powder. According to the treatment process, the milled neodymium iron boron magnet raw material powder is adopted; the powder milled by an airflow mill is directly coated and plated with nickel; the surfaces of the powder granules are coated with a nano-scale nickel-plated layer, so that the oxidization resistance of the neodymium iron boron powder is improved, granular groups formed by powder agglomeration are prevented in the subsequent process, the orientated forming of the powder is facilitated, and the corrosion resistance of the sintered neodymium iron boron magnet is greatly improved.
Description
Technical field
The invention belongs to permanent magnet preparing technical field, particularly relate to a kind of neodymium iron boron magnetic body material powder and treatment process thereof.
Background technology
Permanent magnet and hard magnetic body, can keep the magnet of its magnetic for a long time, not easily loss of excitation, is also not easily magnetized.Thus, be no matter in industrial production or in daily life, one of muscle material that hard magnetic body is the most frequently used.Hard magnetic body can be divided into natural magnet and artificial magnet, and artificial magnet refers to that the alloy by synthesizing different materials can reach the effect identical with natural magnet (magnet), but also can improve magnetic force.Just occurred artificial magnet as far back as 18th century, but the process manufacturing more strong magnetic material is very slow, until produce alnico magnet (AlNiCo) thirties in 20th century, just makes the large-scale application of magnet become possibility.Subsequently, produce ferrite (Ferrite) the 1950's, the sixties, the appearance of rare earth permanent magnet, then for the application of magnet opens a New Times, first generation samarium cobalt permanent magnet SmCo
5, second generation precipitation hardenable samarium cobalt permanent magnet Sm
2co
17, up to now, develop into third generation Nd-Fe-Bo permanent magnet material (NdFeB).Although ferrimagnet remains the maximum permanent magnetic material of consumption at present, the output value of neodymium iron boron magnetic body substantially exceeds ferrite permanent-magnet materials, has developed into a large industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymiummagnet), and its chemical formula is Nd
2fe
14b is a kind of artificial permanent magnet, is also the permanent magnet so far with the strongest magnetic force, and its maximum magnetic energy product (BHmax) exceeds more than 10 times, ferrite, and under the state of naked magnetic, its magnetic force can reach 3500 Gauss.The advantage of neodymium iron boron magnetic body is that cost performance is high, the mechanical property that volume is little, lightweight, good and the feature such as magnetic is strong, the advantage of high-energy-density like this makes Nd-Fe-Bo permanent magnet material obtain a wide range of applications in modern industry and electronic technology, is described as magnetic king in magnetics circle.Thus, neodymium iron boron magnetic body preparation and expansion be the focus given more sustained attention in the industry always.
At present, industry often adopts sintering process to make neodymium iron boron magnetic body, in " key process parameter and alloying element are on the impact of Sintered NdFeB magnetic property and mechanical property ", the technological process adopting sintering process to manufacture Nd-Fe-Bo permanent magnet material is disclosed as Wang Wei waits, mainly melting, abrasive dust, compressing, isostatic pressed and sintering five steps, specifically comprise that batching, melting, steel ingot fragmentation, powder process, oxidative deactivation, powder orientation are compressing, isostatic pressed compacting, vacuum-sintering, inspection divide and the step such as plating.
In the last few years, along with neodymium iron boron magnetic body is at multi-field high-speed expansion, Sintered NdFeB magnet is widely used in the various aspects of life with its superior performance, as obtained extensive use in fields such as Aeronautics and Astronautics, computer hardware, voice coil motor, magnetic separation technique, instrument and meter, transducer, magnetic suspension train, magnetic medical skills.Also further demand has been had to other side to while the magnetic property requirements of neodymium iron boron magnetic body, especially on corrosion resistant performance, because neodymium iron boron magnetic body principal phase is Nd in industry
2fe
14b, grain boundary is rich-Nd phase mutually, and rich Nd Grain-Boundary Phase current potential is lower than basic phase Nd
2fe
14b and rich B phase, make material show as intercrystalline corrosion in corrosive medium, so that cause the corrosion-resistant of magnet material, naturally greatly limit the application of Nd-Fe-B material.
Thus, how can by the improvement in Sintered NdFeB magnet preparation process, on the basis ensureing magnet magnetic property, improve decay resistance, widen its range of application, be the focus of forward-looking manufacturer and technical staff's extensive concern always.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of neodymium iron boron magnetic body material powder and treatment process thereof, treatment process provided by the invention can improve the non-oxidizability of powder, and then improves product corrosion resistance, and magnet also has higher magnetic property.
The invention provides a kind of neodymium iron boron magnetic body material powder, comprise neodymium iron boron raw material fine powder and be coated on the nickel dam on its surface.
Preferably, described neodymium iron boron raw material fine powder is the fine powder after airflow milling grinds;
The granularity of described neodymium iron boron raw material fine powder is 3 ~ 5 μm.
Preferably, the thickness of described nickel dam is 30 ~ 70nm.
Preferably, described neodymium iron boron magnetic body raw material, composition comprises by mass percentage: Pr-Nd:28% ~ 33%; Dy:0 ~ 10%; Tb:0 ~ 10%; Nb:0 ~ 5%; Al:0 ~ 1%; B:0.5% ~ 2.0%; Cu:0 ~ 1%; Co:0 ~ 3%; Ga:0 ~ 2%; Gd:0 ~ 2%; Ho:0 ~ 2%; Zr:0 ~ 2%; Surplus is Fe.
The invention provides a kind for the treatment of process of neodymium iron boron magnetic body material powder, comprise the following steps:
Under the condition of protective gas, by the neodymium iron boron raw material fine powder after grinding, after carrying out plating nickel on surface, obtain neodymium iron boron magnetic body material powder.
Preferably, the temperature of described plating nickel on surface is 75 ~ 85 DEG C, and the time of described plating nickel on surface is 20 ~ 30min.
Preferably, described plating nickel on surface be specially immerse nickel plating solution carry out plating nickel on surface;
The volume ratio of described neodymium iron boron raw material fine powder quality and described nickel plating solution is (30 ~ 50) g:1L.
Preferably, described nickel plating solution comprises nickelous sulfate, reducing agent, complexing agent, stabilizer, buffer and water.
Preferably, described reducing agent is sodium hypophosphite, and described complexing agent is natrium citricum, and described stabilizer is sweet nitrilo acetic acid, and described buffer is sodium lactate;
In described nickel plating solution, the concentration of described nickelous sulfate is 25 ~ 30g/L; The concentration of described reducing agent is 25 ~ 30g/L; The concentration of described complexing agent is 20 ~ 25g/L; The concentration of described stabilizer is 0.001 ~ 0.004g/L; The concentration of described buffer is 20 ~ 25g/L.
Present invention also offers a kind of neodymium iron boron magnetic body, by the neodymium iron boron magnetic body material powder prepared by the neodymium iron boron magnetic body material powder described in technique scheme any one or technique scheme any one treatment process, through compressing and sintering after obtain.
The invention provides a kind of neodymium iron boron magnetic body material powder, comprise neodymium iron boron raw material fine powder and be coated on the nickel dam on its surface.Compared with existing air or oxygen passivating technique; the present invention is based on characteristic and the corrosion mechanism of neodymium iron boron magnetic body; Van der Waals force between micron dimension neodymium iron boron magnetic body material powder; the interaction of London power and magnetic force; make agglomerates be polymerized to secondary powder particle, form granule group, cause the poor fluidity of powder; orientation difficulty, and corrosion-resistant.The present invention starts with from the neodymium iron boron magnetic body material powder after grinding; the direct coated nickel plating of the powder that airflow milling is ground; the nano level nickel coating of the coated one deck of powder particle surface; improve the oxidation resistance of neodymium iron boron powder; agglomerates in subsequent process is prevented to be polymerized to particle group; be conducive to the oriented moulding of powder, increase substantially the corrosion resisting property of Sintered NdFeB magnet.Experimental result shows, neodymium iron boron magnetic body prepared by neodymium iron boron magnetic body material powder provided by the invention is while the magnetic property that maintenance is higher, and hot demagnetize is minimum is only 0.4%, and aging weightlessness is minimum is down to 0.2mg/cm
2, corrosion-resistant rank can reach 9 grades.
Accompanying drawing explanation
Fig. 1 is that the present invention adopts nickel plating flouring technology to prepare the process schematic of neodymium iron boron magnetic body.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, instead of the restriction to invention claim.
The all raw materials of the present invention, be not particularly limited its source, commercially buy or prepare according to conventional method well known to those skilled in the art.
The all raw materials of the present invention, are not particularly limited its purity, and the present invention preferably adopts analysis pure.
The invention provides a kind of neodymium iron boron magnetic body material powder, comprise neodymium iron boron raw material fine powder and be coated on the nickel dam on its surface.
The present invention is not particularly limited described neodymium iron boron magnetic body raw material fine powder, and with the neodymium iron boron magnetic body raw material fine powder in neodymium-iron-boron production procedure well known to those skilled in the art, the present invention preferably refers to the raw material fine powder after airflow milling grinds; The source of the present invention to described neodymium iron boron material powder is not particularly limited, originate with neodymium iron boron material powder well known to those skilled in the art, can be selected from commercially available or conventionally prepare, the present invention is preferably and obtains after the step of neodymium iron boron raw material through batching, melting, hydrogen in quick-fried and abrasive dust or multistep.
The charge ratio of the present invention to described neodymium iron boron raw material is not particularly limited, with neodymium iron boron feed proportioning ratio well known to those skilled in the art, and neodymium iron boron magnetic body raw material of the present invention, composition preferably includes by mass percentage: Pr-Nd:28% ~ 33%; Dy:0 ~ 10%; Tb:0 ~ 10%; Nb:0 ~ 5%; Al:0 ~ 1%; B:0.5% ~ 2.0%; Cu:0 ~ 1%; Co:0 ~ 3%; Ga:0 ~ 2%; Gd:0 ~ 2%; Ho:0 ~ 2%; Zr:0 ~ 2%; Surplus is Fe.The mass percentage content of wherein said Pr-Nd is preferably 29% ~ 33%, is more preferably 29.5% ~ 32%, most preferably is 30% ~ 31.2%; The mass percentage content of described Dy is preferably 1.0% ~ 8.0%, is more preferably 3.0% ~ 7.0%, most preferably is 4.0% ~ 6.0%; The mass percentage content of described Tb is preferably 1.0% ~ 8.0%, is more preferably 3.0% ~ 7.0%, most preferably is 4.0% ~ 6.0%; The mass percentage content of described Nb is preferably 1.0% ~ 4.0%, is more preferably 1.5% ~ 3.5%, most preferably is 1.8% ~ 3.2%; The mass percentage content of described Al is preferably 0.2% ~ 0.8%, is more preferably 0.4% ~ 0.5%, most preferably is 0.42% ~ 0.48%; The mass percentage content of described B is preferably 0.97% ~ 1.5%, is more preferably 0.98% ~ 1.4%, is more preferably 0.99% ~ 1.2%, most preferably is 1.0% ~ 1.1%; The mass percentage content of described Cu is preferably 0.1% ~ 0.8%, is more preferably 0.3% ~ 0.7%, most preferably is 0.4% ~ 0.6%; The mass percentage content of described Co is preferably 0.5% ~ 2.0%, is more preferably 0.7% ~ 1.5%, most preferably is 1.0% ~ 1.2%; The mass percentage content of described Ga is preferably 0.3% ~ 1.5%, is more preferably 0.5% ~ 1.2%, is more preferably 0.7% ~ 1.0%, most preferably is 0.8% ~ 0.9%; The mass percentage content of described Gd is preferably 0.3% ~ 1.5%, is more preferably 0.5% ~ 1.2%, is more preferably 0.7% ~ 1.0%, most preferably is 0.8% ~ 0.9%; The mass percentage content of described Ho is preferably 0.3% ~ 1.5%, is more preferably 0.5% ~ 1.2%, is more preferably 0.7% ~ 1.0%, most preferably is 0.8% ~ 0.9%; The mass percentage content of described Zr is preferably 0.3% ~ 1.5%, is more preferably 0.5% ~ 1.2%, is more preferably 0.7% ~ 1.0%, most preferably is 0.8% ~ 0.9%.
The present invention is not particularly limited the fusion process of described neodymium iron boron raw material and equipment, with the fusion process of neodymium iron boron raw material well known to those skilled in the art and equipment; The present invention is not particularly limited the quick-fried process of hydrogen of described neodymium iron boron raw material and equipment, with the quick-fried process of hydrogen of neodymium iron boron raw material well known to those skilled in the art and equipment; The present invention is not particularly limited the milling process of described neodymium iron boron raw material and equipment, and with the milling process of neodymium iron boron raw material well known to those skilled in the art and equipment, the present invention is preferably airflow milling; Process choice and the order of the present invention's and abrasive dust quick-fried to above-mentioned batching, melting, hydrogen are not particularly limited, with process choice well known to those skilled in the art and order, also can carry out selecting or changing according to practical condition, product quality requirement and characteristic requirements.
The granularity of the present invention to described neodymium iron boron raw material fine powder is not particularly limited, with the granularity of neodymium iron boron material powder well known to those skilled in the art, the particle mean size of neodymium iron boron raw material fine powder of the present invention is preferably 3.0 ~ 5.0 μm, be more preferably 3.25 ~ 4.75 μm, be more preferably 3.5 ~ 4.5 μm, most preferably be 3.75 ~ 4.25 μm.The thickness of the present invention to described nickel dam is not particularly limited, with the thickness of coating well known to those skilled in the art, those skilled in the art can carry out selecting or adjusting according to practical condition, product quality requirement and product type, the present invention is for ensureing anticorrosion effect, the thickness of described nickel dam is preferably 30 ~ 70nm, be more preferably 35 ~ 65nm, be more preferably 40 ~ 60nm, most preferably be 45 ~ 55nm.
The present invention to be coatedly not particularly limited described, and with coated concept well known to those skilled in the art, can be understood as, part is coated, coating, plating, compound or drip the concepts such as painting.
The present invention is at the nano level metallic nickel of neodymium iron boron raw material fine powder Surface coating one deck, the particle size efficiently solving neodymium iron boron powder is tiny, the Nd of particle surface is very easily oxidized, cause rich Nd to reduce, thus the magnetic property effectively solving the magnet caused thus reduce and the problem of magnet product corrosion resistance difference.Meanwhile, prevent agglomerates in subsequent forming process to be polymerized to particle group, be conducive to the oriented moulding of powder.
The invention provides a kind for the treatment of process of neodymium iron boron magnetic body material powder, comprise the following steps:
Under the condition of protective gas, by the neodymium iron boron raw material fine powder after grinding, after carrying out plating nickel on surface, obtain neodymium iron boron magnetic body material powder.
The optimum principle of the optimum principle such as source, composition, character of raw material described in preparation method of the present invention or concrete preferred version and aforementioned neodymium iron boron magnetic body material powder and specifically preferred version is all consistent, this is no longer going to repeat them.
The present invention is not particularly limited described protective gas; with well known to those skilled in the art for the protective gas in neodymium iron boron powder compaction process; protective gas of the present invention is preferably inert gas and/or nitrogen, is more preferably argon gas and/or nitrogen, most preferably is nitrogen.
The mode of effects on surface nickel plating of the present invention is not particularly limited, and those skilled in the art can carry out selecting or adjusting according to practical condition, product quality requirement and product purpose, and the present invention is specifically preferably immersion nickel plating solution and carries out plating nickel on surface.The temperature that the temperature and time of plating nickel on surface of the present invention is specifically preferably nickel plating solution and the time of flooding in nickel plating solution; The temperature of described plating nickel on surface is specifically preferably 75 ~ 85 DEG C, is more preferably 77 ~ 83 DEG C, most preferably is 79 ~ 81 DEG C; The time of described plating nickel on surface is specifically preferably 20 ~ 30min, is more preferably 22 ~ 28min, most preferably is 24 ~ 26min.The ratio of the present invention to described nickel plating solution and neodymium iron boron raw material fine powder is not particularly limited, with both conventional ratio in the plated journey of solution surface well known to those skilled in the art, those skilled in the art can carry out selecting or adjusting according to practical condition, product quality requirement and product purpose, the volume ratio of neodymium iron boron raw material fine powder quality of the present invention and described nickel plating solution is preferably (30 ~ 50) g:1L, be more preferably (33 ~ 47) g:1L, be more preferably (35 ~ 45) g:1L, most preferably be (37 ~ 42) g:1L.
The concrete composition of the present invention to described nickel plating solution is not particularly limited, form with the routine of nickel plating solution well known to those skilled in the art, those skilled in the art can carry out selecting or adjusting according to practical condition, product quality requirement and product purpose, and nickel plating solution of the present invention preferably includes nickelous sulfate, reducing agent, complexing agent, stabilizer, buffer and water; Described reducing agent is preferably sodium hypophosphite, and described complexing agent is preferably natrium citricum, and described stabilizer is preferably sweet nitrilo acetic acid, and described buffer is preferably sodium lactate.The concrete ratio of the present invention to mentioned component is not particularly limited, those skilled in the art can carry out selecting or adjusting according to practical condition, product quality requirement and product purpose, in nickel plating solution of the present invention, the concentration of described nickelous sulfate is preferably 25 ~ 30g/L, be more preferably 26 ~ 29g/L, most preferably be 27 ~ 28g/L; The concentration of described reducing agent is preferably 25 ~ 30g/L, is more preferably 26 ~ 29g/L, most preferably is 27 ~ 28g/L; The concentration of described complexing agent is preferably 20 ~ 25g/L, is more preferably 21 ~ 24g/L, most preferably is 22 ~ 23g/L; The concentration of described stabilizer is preferably 0.001 ~ 0.004g/L, is more preferably 0.0015 ~ 0.0035g/L, most preferably is 0.002 ~ 0.003g/L; The concentration of described buffer is preferably 20 ~ 25g/L, is more preferably 26 ~ 29g/L, most preferably is 27 ~ 28g/L.
The present invention, after plating nickel on surface, for consolidating coating effect, preferably also after reprocessing, obtains neodymium iron boron magnetic body material powder.The concrete steps of the present invention to described reprocessing are not particularly limited, and with post-processing step well known to those skilled in the art, the present invention is specifically preferably washing, filters and drying.The process of the present invention to described washing and filtering is not particularly limited, and in washing and filtering mode well known to those skilled in the art, the present invention specifically preferably spends deionized water and filters 2 ~ 5 times; The process of the present invention to described drying is not particularly limited, and with drying course well known to those skilled in the art, the present invention is specifically preferably constant temperature 90 ~ 110 DEG C drying process 3 ~ 6h, then is cooled to room temperature.
The present invention will obtain a kind of neodymium iron boron magnetic body material powder through above-mentioned steps; i.e. a kind of neodymium iron boron magnetic body material powder of plating nickel on surface modification; the present invention is based on characteristic and the corrosion mechanism of neodymium iron boron magnetic body; Van der Waals force between micron dimension neodymium iron boron magnetic body material powder, the interaction of London power and magnetic force, makes agglomerates be polymerized to secondary powder particle; form granule group; cause the poor fluidity of powder, orientation difficulty, and corrosion-resistant.The present invention starts with from the neodymium iron boron magnetic body material powder after grinding; the direct coated nickel plating of the powder that airflow milling is ground; the nano level nickel coating of the coated one deck of powder particle surface; improve the oxidation resistance of neodymium iron boron powder; agglomerates in subsequent process is prevented to be polymerized to particle group; be conducive to the oriented moulding of powder, increase substantially the corrosion resisting property of Sintered NdFeB magnet.Experimental result shows, neodymium iron boron magnetic body prepared by neodymium iron boron magnetic body material powder provided by the invention is while the magnetic property that maintenance is higher, and hot demagnetize is minimum is only 0.4%, and aging weightlessness is minimum is down to 0.2mg/cm
2, corrosion-resistant rank can reach 9 grades.
Present invention also offers a kind of neodymium iron boron magnetic body, by the neodymium iron boron magnetic body material powder prepared by the neodymium iron boron magnetic body material powder described in technique scheme any one or technique scheme any one treatment process, through compressing and sintering after obtain.
The neodymium iron boron magnetic body material powder that the present invention will be prepared through above-mentioned steps, through compressing and sintering after obtain.It will be appreciated by those skilled in the art that described neodymium iron boron magnetic body material powder also preferably again through orientation, compacting, encapsulation, isostatic cool pressing, cut the subsequent steps such as material and sintering after, finally obtain product neodymium iron boron magnetic body.The present invention is not particularly limited the concrete technology flow process of above-mentioned subsequent step and Parameter Conditions, with the concrete technology flow process of neodymium-iron-boron preparation step well known to those skilled in the art and Parameter Conditions, the present invention is specifically preferably: neodymium iron boron magnetic body material powder above-mentioned steps prepared, the pressed compact of density 3.9 ~ 4.3g/cm3 is pressed into through the mo(u)ldenpress orientation that magnetizes, cold isostatic press compresses pressed compact further, green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree to below 0.3Pa, be warming up to about 200 DEG C insulation draining gas, be warming up to about 500 DEG C insulation row organic substances, be warming up to 800 DEG C of insulation row H
2be warming up to i.e. 1020 DEG C ~ 1050 DEG C temperature liquid-phase sinterings of below principal phase fusing point, now the rich neodymium of crystal boundary is in liquid phase state mutually, continue insulation 60 ~ 120min at this temperature, close heater, applying argon gas to 85 ~ 100Kpa, the machine that blows in is cooled to 60 DEG C ~ 80 DEG C and comes out of the stove, obtain blank, then after processing and surface treatment, obtain neodymium iron boron magnetic body product.
In order to further illustrate the present invention, be described in detail to a kind of neodymium iron boron magnetic body material powder provided by the invention and treatment process thereof, neodymium iron boron magnetic body below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
With the checking that 38SH sintered neodymium iron boron material does, composition of raw material is as shown in table 1 below:
| Element | PrNd | Dy | Ho | Al | B | Cu | Co | Zr | Ga | Fe |
| wt％ | 25.1 | 2 | 4 | 0.44 | 0.94 | 0.15 | 1.5 | 0.15 | 0.2 | 65.52 |
First, by above-mentioned formula, allot 600Kg raw material, wherein iron staff rust cleaning, rare earth material carries out oily, the amphidromic and rustless process of nothing, by raw material deposite metal under the condition of Frequency Induction Heating that vacuum melting (SC) will prepare, the final fast quenching Nd Fe B alloys with columnar crystal structure obtaining sheet.
Then in hydrogen broken furnace, inhale hydrogen dehydrogenation be broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then grind the micron-sized powder of epigranular by airflow milling high pressure nitrogen, powder mean particle sizes is 4.0 ~ 5.0 μm.
Then carry out chemical nickel plating by electroless plating tank to airflow milling powder particle, chemical nickel-plating solution formula is as follows:
Containing nickelous sulfate 23g, reducing agent sodium hypophosphite 29g, complexing agent natrium citricum 25g in often liter of solution, the sweet nitrilo acetic acid 0.003g of stabilizer, buffer sodium lactate 23g, all the other are deionized water.
Neodymium iron boron raw material fine powder through airflow milling is immersed in above-mentioned chemical nickel-plating solution, bath temperature 76 DEG C, pH value is 5, directly carry out chemical nickel plating, thickness of coating is about 35nm, process applies the uniform stirring of 20 revs/min, plating time is 20min, neodymium iron boron material powder after chemical plating is through 4 washed with de-ionized water, filter, by the powder constant temperature 110 DEG C drying process 5h filtered, be cooled to room temperature, the mo(u)ldenpress orientation that magnetizes is pressed into the pressed compact of density 4.0g/cm3, cold isostatic press compresses pressed compact further, green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree to below 0.3Pa, be warming up to about 200 DEG C insulation draining gas, be warming up to about 500 DEG C insulation row organic substances, be warming up to 800 DEG C of insulation row H
2be warming up to the i.e. 1020 DEG C of temperature liquid-phase sinterings of below principal phase fusing point, now the rich neodymium of crystal boundary is in liquid phase state mutually, insulation 60min is continued at this temperature, close heater, applying argon gas is to 85Kpa, and the machine that blows in is cooled to 60 DEG C and comes out of the stove, and obtaining specification is 51.2*51*29mm (direction of orientation is 29 sizes) blank.
Finally, with surface grinding machine, oriented surface one side 60% is shown in light, is glued on iron staff, is cut into 9.59*6.69*0.88 (M) black-film with inside diameter slicer, with adding the solution oil removing of cleaning agent except glue, fall the radian of 0.2mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtains the finished product being of a size of 9.95*6.69*0.88 (M).
Carry out Performance Detection to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, see table 2, table 2 is the magnetic property of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
The magnetic property of finished product neodymium iron boron magnetic body prepared by table 2 embodiment of the present invention 1
As shown in Table 2, adopt powder depositing process provided by the invention, Br and Hcj of magnet there is no change, and this shows that treatment process of the present invention does not affect magnetic property and the temperature stability of material.
Demagnetize is tested, and see table 3, table 3 is the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Demagnetize condition: 120 DEG C × 2h; Equipment: high temperature drying case.
The demagnetize situation of finished product neodymium iron boron magnetic body prepared by table 3 embodiment of the present invention 1
| Demagnetize | |
| Powder depositing process | 0.5％～2.8％ |
| Normal process | 5％～10％ |
As shown in Table 3, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet demagnetize situation obviously declines.
Weightless test, see table 4, table 4 is the reduced gravity situations of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar.
Equipment: HAST ageing oven
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by table 4 embodiment of the present invention 1
| Weightlessness/mg/cm 2 | |
| Powder depositing process | 0.8～1.5 |
| Normal process | 2.0～8.0 |
As shown in Table 4, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet is weightless obviously to be reduced.
Salt air corrosion is tested, and see table 5, table 5 is the decay resistance of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1.
Salt fog condition:
A. sodium chloride concentration: 50g/lPH value: 6.5 ~ 7.2;
B. spray amount: (ml/80cm2/h)=1.0 ~ 2.0;
C. pressure measuring cylinder temperature: (DEG C)=47 ± 2 brine temp (DEG C)=35 ± 2 test temperatures: (DEG C)=35 ± 2;
D. spray: spray continuously
Equipment: salt spray test chamber
The decay resistance of finished product neodymium iron boron magnetic body prepared by table 5 embodiment of the present invention 1
| Rank | |
| Powder depositing process | 8～9 |
| Normal process | 3～7 |
As shown in Table 5, the decay resistance of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet decay resistance obviously promotes, and rank can reach 8 ~ 9.
Embodiment 2
With the checking that 42SH sintered neodymium iron boron material does, composition of raw material is as shown in table 6 below:
| Element | PrNd | Dy | Al | B | Cu | Co | Zr | Ga | Fe |
| wt％ | 30 | 2 | 0.4 | 0.93 | 0.15 | 1.2 | 0.1 | 0.2 | 65.02 |
First, by above-mentioned formula, allot 600Kg raw material, wherein iron staff rust cleaning, rare earth material carries out oily, the amphidromic and rustless process of nothing, by raw material deposite metal under the condition of Frequency Induction Heating that vacuum melting (SC) will prepare, the final fast quenching Nd Fe B alloys with columnar crystal structure obtaining sheet.
Then in hydrogen broken furnace, inhale hydrogen dehydrogenation be broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then grind the micron-sized powder of epigranular by airflow milling high pressure nitrogen, powder mean particle sizes is 3.7 ~ 4.7 μm.
Then carry out chemical nickel plating by electroless plating tank to airflow milling powder particle, chemical nickel-plating solution formula is as follows:
Containing nickelous sulfate 28g, reducing agent sodium hypophosphite 26g, complexing agent natrium citricum 23g in often liter of solution, the sweet nitrilo acetic acid 0.003g of stabilizer, buffer sodium lactate 22g, all the other are deionized water.
Neodymium iron boron raw material fine powder through airflow milling is immersed in above-mentioned chemical nickel-plating solution, bath temperature 80 DEG C, pH value is 6, directly carry out chemical nickel plating, thickness of coating is about 50nm, process applies the uniform stirring of 18 revs/min, plating time is 25min, neodymium iron boron material powder after chemical plating is through 5 washed with de-ionized water, filter, by the powder constant temperature 100 DEG C drying process 5h filtered, be cooled to room temperature, the mo(u)ldenpress orientation that magnetizes is pressed into the pressed compact of density 4.3g/cm3, cold isostatic press compresses pressed compact further, green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree to below 0.3Pa, be warming up to about 200 DEG C insulation draining gas, be warming up to about 500 DEG C insulation row organic substances, be warming up to 800 DEG C of insulation row H
2be warming up to the i.e. 1050 DEG C of temperature liquid-phase sinterings of below principal phase fusing point, now the rich neodymium of crystal boundary is in liquid phase state mutually, insulation 120min is continued at this temperature, close heater, applying argon gas is to 95Kpa, and the machine that blows in is cooled to 80 DEG C and comes out of the stove, and obtaining specification is 51*47*32mm (direction of orientation is 32 sizes) blank.
Finally, with surface grinding machine, oriented surface one side 80% is shown in light, is glued on iron staff, is cut into 9.59*6.69*0.88 (M) black-film with inside diameter slicer, with adding the solution oil removing of cleaning agent except glue, fall the radian of 0.3mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtains the finished product being of a size of 9.95*6.69*0.88 (M).
Carry out Performance Detection to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, see table 7, table 7 is the magnetic property of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
The magnetic property of finished product neodymium iron boron magnetic body prepared by table 7 embodiment of the present invention 2
As shown in Table 7, adopt powder depositing process provided by the invention, Br and Hcj of magnet there is no change, and promotes by a small margin in addition, and this shows that treatment process of the present invention does not affect magnetic property and the temperature stability of material.
Demagnetize is tested, and see table 8, table 8 is the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Demagnetize condition: 120 DEG C × 2h; Equipment: high temperature drying case.
The demagnetize situation of finished product neodymium iron boron magnetic body prepared by table 8 embodiment of the present invention 2
| Demagnetize | |
| Powder depositing process | 0.6％～3％ |
| Normal process | 6％～10％ |
As shown in Table 8, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet demagnetize situation obviously declines.
Weightless test, see table 9, table 9 is the reduced gravity situations of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar.
Equipment: HAST ageing oven
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by table 9 embodiment of the present invention 2
| Weightlessness/mg/cm 2 | |
| Powder depositing process | 0.2～1.6 |
| Normal process | 2.0～8.0 |
As shown in Table 9, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet is weightless obviously to be reduced.
Salt air corrosion is tested, and see table 10, table 10 is the decay resistance of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 2.
Salt fog condition:
A. sodium chloride concentration: 50g/lPH value: 6.5 ~ 7.2;
B. spray amount: (ml/80cm2/h)=1.0 ~ 2.0;
C. pressure measuring cylinder temperature: (DEG C)=47 ± 2 brine temp (DEG C)=35 ± 2 test temperatures: (DEG C)=35 ± 2;
D. spray: spray continuously
Equipment: salt spray test chamber
The decay resistance of finished product neodymium iron boron magnetic body prepared by table 10 embodiment of the present invention 2
| Rank | |
| Powder depositing process | 8～9 |
| Normal process | 2～7 |
As shown in Table 10, the decay resistance of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet decay resistance obviously promotes, and rank can reach 8 ~ 9.
Embodiment 3
With the checking that 45UH sintered neodymium iron boron material does, composition of raw material is as shown in table 11 below:
| Element | PrNd | Tb | Al | B | Cu | Co | Zr | Ga | Fe |
| wt％ | 30 | 0.8 | 0.1 | 0.93 | 0.15 | 1.2 | 0.1 | 0.2 | 66.52 |
First, by above-mentioned formula, allot 600Kg raw material, wherein iron staff rust cleaning, rare earth material carries out oily, the amphidromic and rustless process of nothing, by raw material deposite metal under the condition of Frequency Induction Heating that vacuum melting (SC) will prepare, the final fast quenching Nd Fe B alloys with columnar crystal structure obtaining sheet.
Then in hydrogen broken furnace, inhale hydrogen dehydrogenation be broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then grind the micron-sized powder of epigranular by airflow milling high pressure nitrogen, powder mean particle sizes is 3.5 ~ 4.5 μm.
Then carry out chemical nickel plating by electroless plating tank to airflow milling powder particle, chemical nickel-plating solution formula is as follows:
Containing nickelous sulfate 26g, reducing agent sodium hypophosphite 27g, complexing agent natrium citricum 22g in often liter of solution, the sweet nitrilo acetic acid 0.002g of stabilizer, buffer sodium lactate 21g, all the other are deionized water.
Neodymium iron boron raw material fine powder through airflow milling is immersed in above-mentioned chemical nickel-plating solution, bath temperature 85 DEG C, pH value is 6, directly carry out chemical nickel plating, thickness of coating is about 70nm, process applies the uniform stirring of 19 revs/min, plating time is 25min, neodymium iron boron material powder after chemical plating is through 4 washed with de-ionized water, filter, by the powder constant temperature 100 DEG C drying process 6h filtered, be cooled to room temperature, the mo(u)ldenpress orientation that magnetizes is pressed into the pressed compact of density 4.0g/cm3, cold isostatic press compresses pressed compact further, green compact are loaded vacuum sintering furnace, be evacuated to vacuum degree to below 0.3Pa, be warming up to about 200 DEG C insulation draining gas, be warming up to about 500 DEG C insulation row organic substances, be warming up to 800 DEG C of insulation row H
2be warming up to the i.e. 1040 DEG C of temperature liquid-phase sinterings of below principal phase fusing point, now the rich neodymium of crystal boundary is in liquid phase state mutually, insulation 100min is continued at this temperature, close heater, applying argon gas is to 90Kpa, and the machine that blows in is cooled to 80 DEG C and comes out of the stove, and obtaining specification is 51*47*32mm (direction of orientation is 32 sizes) blank.
Finally, with surface grinding machine, oriented surface one side 70% is shown in light, is glued on iron staff, is cut into 9.59*6.69*0.88 (M) black-film with inside diameter slicer, with adding the solution oil removing of cleaning agent except glue, fall the radian of 0.5mm with automatic chamfering machine, remove burrs on edges, pass through ultrasonic oil removal, pickling, passivation, automatic zincincation, obtains the finished product being of a size of 9.95*6.69*0.88 (M).
Carry out Performance Detection to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, see table 12, table 12 is the magnetic property of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
The magnetic property of finished product neodymium iron boron magnetic body prepared by table 12 embodiment of the present invention 3
As shown in Table 12, adopt powder depositing process provided by the invention, Br and Hcj of magnet there is no change, and promotes by a small margin in addition, and this shows that treatment process of the present invention does not affect magnetic property and the temperature stability of material.
Demagnetize is tested, and see table 13, table 13 is the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Demagnetize condition: 120 DEG C × 2h; Equipment: high temperature drying case.
The demagnetize situation of finished product neodymium iron boron magnetic body prepared by table 13 embodiment of the present invention 3
| Demagnetize | |
| Powder depositing process | 0.4％～2.5％ |
| Normal process | 4％～10％ |
As shown in Table 13, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet demagnetize situation obviously declines.
Weightless test, see table 14, table 14 is the reduced gravity situations of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Below-G conditions: temperature 130 DEG C, humidity 100%, time 240h, pressure 2.7Bar.
Equipment: HAST ageing oven
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by table 14 embodiment of the present invention 3
As shown in Table 14, the demagnetize situation of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet is weightless obviously to be reduced.
Salt air corrosion is tested, and see table 15, table 15 is the decay resistance of finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 3.
Salt fog condition:
A. sodium chloride concentration: 50g/lPH value: 6.5 ~ 7.2;
B. spray amount: (ml/80cm2/h)=1.0 ~ 2.0;
C. pressure measuring cylinder temperature: (DEG C)=47 ± 2 brine temp (DEG C)=35 ± 2 test temperatures: (DEG C)=35 ± 2;
D. spray: spray continuously
Equipment: salt spray test chamber
The decay resistance of finished product neodymium iron boron magnetic body prepared by table 15 embodiment of the present invention 3
| Rank | |
| Powder depositing process | 8～9 |
| Normal process | 2～8 |
As shown in Table 15, the decay resistance of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet decay resistance obviously promotes, and rank can reach 8 ~ 9.
Above a kind of neodymium iron boron magnetic body material powder provided by the present invention and treatment process thereof, neodymium iron boron magnetic body are described in detail.Apply a concrete example herein to set forth principle of the present invention and execution mode, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection range of the claims in the present invention.
Claims (10)
1. a neodymium iron boron magnetic body material powder, is characterized in that, comprises neodymium iron boron raw material fine powder and is coated on the nickel dam on its surface.
2. material powder according to claim 1, is characterized in that, described neodymium iron boron raw material fine powder is the fine powder after airflow milling grinds;
The granularity of described neodymium iron boron raw material fine powder is 3 ~ 5 μm.
3. material powder according to claim 1, is characterized in that, the thickness of described nickel dam is 30 ~ 70nm.
4. material powder according to claim 1, is characterized in that, described neodymium iron boron magnetic body raw material, and composition comprises by mass percentage: Pr-Nd:28% ~ 33%; Dy:0 ~ 10%; Tb:0 ~ 10%; Nb:0 ~ 5%; Al:0 ~ 1%; B:0.5% ~ 2.0%; Cu:0 ~ 1%; Co:0 ~ 3%; Ga:0 ~ 2%; Gd:0 ~ 2%; Ho:0 ~ 2%; Zr:0 ~ 2%; Surplus is Fe.
5. a treatment process for neodymium iron boron magnetic body material powder, is characterized in that, comprises the following steps:
Under the condition of protective gas, by the neodymium iron boron raw material fine powder after grinding, after carrying out plating nickel on surface, obtain neodymium iron boron magnetic body material powder.
6. treatment process according to claim 5, is characterized in that, the temperature of described plating nickel on surface is 75 ~ 85 DEG C, and the time of described plating nickel on surface is 20 ~ 30min.
7. treatment process according to claim 5, is characterized in that, described plating nickel on surface is specially immersion nickel plating solution and carries out plating nickel on surface;
The volume ratio of described neodymium iron boron raw material fine powder quality and described nickel plating solution is (30 ~ 50) g:1L.
8. treatment process according to claim 7, is characterized in that, described nickel plating solution comprises nickelous sulfate, reducing agent, complexing agent, stabilizer, buffer and water.
9. treatment process according to claim 8, is characterized in that, described reducing agent is sodium hypophosphite, and described complexing agent is natrium citricum, and described stabilizer is sweet nitrilo acetic acid, and described buffer is sodium lactate;
In described nickel plating solution, the concentration of described nickelous sulfate is 25 ~ 30g/L; The concentration of described reducing agent is 25 ~ 30g/L; The concentration of described complexing agent is 20 ~ 25g/L; The concentration of described stabilizer is 0.001 ~ 0.004g/L; The concentration of described buffer is 20 ~ 25g/L.
10. a neodymium iron boron magnetic body, is characterized in that, by the neodymium iron boron magnetic body material powder prepared by the neodymium iron boron magnetic body material powder described in Claims 1 to 4 any one or claim 5 ~ 9 any one treatment process, through compressing and sintering after obtain.
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