CN105551707B - A kind of neodymium iron boron magnetic body raw material powder and its treatment process - Google Patents
A kind of neodymium iron boron magnetic body raw material powder and its treatment process Download PDFInfo
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- CN105551707B CN105551707B CN201610104827.6A CN201610104827A CN105551707B CN 105551707 B CN105551707 B CN 105551707B CN 201610104827 A CN201610104827 A CN 201610104827A CN 105551707 B CN105551707 B CN 105551707B
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- iron boron
- neodymium iron
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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
Abstract
The present invention provides a kind of neodymium iron boron magnetic body raw material powder, including neodymium iron boron raw material fine powder and the nickel layer on its surface is coated on.Neodymium iron boron magnetic body raw material powder of the present invention after grinding is started with; the powder that airflow milling is ground directly coats nickel plating; powder particle surface coats one layer of nano level nickel coating; improve the oxidation resistance of neodymium iron boron powder; powder in subsequent process is prevented to be agglomerated into particle group; be conducive to the oriented moulding of powder, the corrosion resistance of Sintered NdFeB magnet is greatly improved.
Description
Technical field
The invention belongs to permanent magnet preparing technical field more particularly to a kind of neodymium iron boron magnetic body raw material powder and its processing works
Skill.
Background technology
Permanent magnet, that is, hard magnetic body, the magnet that can keep its magnetic for a long time, is not easy loss of excitation, is not easy to be magnetized.Thus, nothing
By being in industrial production or in daily life one of most common muscle material of hard magnetic body.Hard magnetic body can be divided into naturally
Magnet and artificial magnet, artificial magnet refer to reach and natural magnet (magnet) phase by the alloy for synthesizing different materials
Same effect, but also magnetic force can be improved.Early in 18th century there have been artificial magnet, but manufacture the mistake of more strong magnetic material
Journey but very slowly, alnico magnet (AlNiCo) is produced until the 1930s, just make the large-scale application of magnet into
For possibility.Then, ferrite (Ferrite), the sixties are manufactured that the 1950s, the appearance of rare earth permanent magnet is then magnetic
The application of body opens a new era, first generation samarium cobalt permanent magnet SmCo5, second generation precipitation hardenable samarium cobalt permanent magnet Sm2Co17,
So far, third generation Nd-Fe-B permanent magnet material (NdFeB) is developed to.Although current ferrimagnet is still that dosage is maximum
Permanent-magnet material, but the output value of neodymium iron boron magnetic body has substantially exceeded ferrite permanent-magnet materials, has evolved into a big industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), chemical formula Nd2Fe14B is a kind of artificial
Permanent magnet and there is the permanent magnet of most strong magnetic force so far, maximum magnetic energy product (BHmax) exceeds ferrite 10
Times or more, in the state of naked magnetic, magnetic force can reach 3500 Gauss.The advantages of neodymium iron boron magnetic body is cost-effective, body
The advantages of the features such as small, light-weight, good mechanical property of product and strong magnetism, such high-energy density, makes Nd-Fe-B permanent magnet material
It is had been widely used in modern industry and electronic technology, magnetic king is known as in magnetics circle.Thus, the system of neodymium iron boron magnetic body
The focus that standby and extension always gives more sustained attention in the industry.
At present, industry makes neodymium iron boron magnetic body frequently with sintering process, such as Wang Wei exists《Key process parameter and alloying element
Influence to Sintered NdFeB magnetic property and mechanical property》In disclose using sintering process manufacture Nd-Fe-B permanent magnet material technique
Five flow, mainly melting, milling, compression moulding, isostatic pressed and sintering steps, specifically include dispensing, melting, steel ingot are broken
It powder broken, processed, oxidative deactivation, powder orientation compression moulding, isostatic pressed compacting, vacuum-sintering, inspection point and electroplates.
In recent years, as neodymium iron boron magnetic body is in multi-field high-speed expansion, Sintered NdFeB magnet is with its superior property
The various aspects of life can be widely used in, such as in Aeronautics and Astronautics, computer hardware, voice coil motor, magnetic separation technique, instrument
The fields such as instruments and meters, sensor, magnetic suspension train, magnetic medical technology obtain extensive use.To the magnetic of neodymium iron boron magnetic body in industry
Also there is further need to other aspects while performance requirement, especially on corrosion resistant performance, due to neodymium iron boron magnetic body
Main phase is Nd2Fe14B, grain boundary are mutually rich-Nd phases, and rich Nd Grain-Boundary Phases current potential is less than basic phase Nd2Fe14B and richness B phases, make material
Material shows as intercrystalline corrosion in corrosive medium, so that causing the poor corrosion resistance of magnet material, greatly limits Nd- naturally
The application of Fe-B materials.
Thus, how by the improvement in Sintered NdFeB magnet preparation process, ensureing the base of magnet magnetic property
On plinth, corrosion resistance is improved, widens its application range, be always forward-looking manufacturer and technical staff's extensive concern
Focus.
The content 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 raw material powder and its processing
Technique, treatment process provided by the invention can improve the inoxidizability of powder, and then improve product corrosion resistance, and magnetic
Body also has higher magnetic property.
The present invention provides a kind of neodymium iron boron magnetic body raw material powders, including neodymium iron boron raw material fine powder and are coated on its surface
Nickel layer.
Preferably, the neodymium iron boron raw material fine powder is the fine powder after airflow milling is ground；
The granularity of the neodymium iron boron raw material fine powder is 3~5 μm.
Preferably, the thickness of the nickel layer is 30~70nm.
Preferably, the neodymium iron boron magnetic body raw material, form 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 present invention provides a kind for the treatment of process of neodymium iron boron magnetic body raw material powder, comprise the following steps：
Under conditions of protective gas, by the neodymium iron boron raw material fine powder after grinding, after carrying out plating nickel on surface, neodymium is obtained
Iron boron magnet raw material powder.
Preferably, the temperature of the plating nickel on surface is 75~85 DEG C, and the time of the plating nickel on surface is 20~30min.
Preferably, the plating nickel on surface is specially and immerses nickel plating solution to carry out plating nickel on surface；
The neodymium iron boron raw material fine powder quality and the volume ratio of the nickel plating solution are (30~50) g：1L.
Preferably, the nickel plating solution includes nickel sulfate, reducing agent, complexing agent, stabilizer, buffer and water.
Preferably, the reducing agent is sodium hypophosphite, and the complexing agent is sodium citrate, and the stabilizer is sweet ammonia second
Acid, the buffer are sodium lactate；
In the nickel plating solution, the concentration of the nickel sulfate is 25~30g/L；The concentration of the reducing agent is 25~30g/
L；The concentration of the complexing agent is 20~25g/L；The concentration of the stabilizer is 0.001~0.004g/L；The buffer
Concentration is 20~25g/L.
It is former as the neodymium iron boron magnetic body described in above-mentioned technical proposal any one the present invention also provides a kind of neodymium iron boron magnetic body
Neodymium iron boron magnetic body raw material powder prepared by feed powder end or above-mentioned technical proposal any one treatment process, by compression moulding and
It is obtained after sintering.
The present invention provides a kind of neodymium iron boron magnetic body raw material powders, including neodymium iron boron raw material fine powder and are coated on its surface
Nickel layer.It is micro- the present invention is based on the characteristic and corrosion mechanism of neodymium iron boron magnetic body compared with existing air or oxygen passivating technique
Van der Waals force between rice magnitude neodymium iron boron magnetic body raw material powder, the interaction of London power and magnetic force are agglomerated into powder
Secondary powder particle forms little particle group, causes the poor fluidity of powder, orientation is difficult, and poor corrosion resistance.The present invention
Neodymium iron boron magnetic body raw material powder after grinding is started with, and the powder that airflow milling is ground directly coats nickel plating, powder particle surface
One layer of nano level nickel coating is coated, improves the oxidation resistance of neodymium iron boron powder, it is therefore prevented that powder is reunited in subsequent process
Into particle group, be conducive to the oriented moulding of powder, the corrosion resisting property of Sintered NdFeB magnet is greatly improved.Experimental result
Show the neodymium iron boron magnetic body of neodymium iron boron magnetic body raw material powder preparation provided by the invention while higher magnetic property is kept,
It is only 0.4% that it is minimum, which to subtract magnetic, for heat, and aging weightlessness is minimum to be down to 0.2mg/cm2, corrosion-resistant rank can reach 9 grades.
Description of the drawings
Fig. 1 is the process schematic that the present invention prepares neodymium iron boron magnetic body using nickel plating flouring technology.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are intended merely to the feature and advantage further illustrated the present invention rather than to invention claim
Limitation.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to people in the art
Known to member prepared by conventional method.
All raw materials of the present invention, are not particularly limited its purity, pure present invention preferably employs analyzing.
The present invention provides a kind of neodymium iron boron magnetic body raw material powders, including neodymium iron boron raw material fine powder and are coated on its surface
Nickel layer.
The neodymium iron boron magnetic body raw material fine powder is not particularly limited in the present invention, with neodymium iron well known to those skilled in the art
Neodymium iron boron magnetic body raw material fine powder in boron magnet preparation process, the present invention preferably refer to the raw material after airflow milling is ground
Fine powder；The source of the neodymium iron boron raw material powder is not particularly limited in the present invention, with neodymium iron well known to those skilled in the art
Boron raw material powder source can be selected from commercially available or conventionally prepare, and the present invention is preferably to pass through neodymium iron boron raw material
Cross that dispensing, melting, hydrogen is quick-fried and milling in one or multi-step after obtain.
The charge ratio of the neodymium iron boron raw material is not particularly limited in the present invention, with neodymium iron well known to those skilled in the art
Boron feed proportioning ratio, neodymium iron boron magnetic body raw material of the present invention form preferably include 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 quality hundred of wherein described Pr-Nd
It is preferably 29%~33% to divide than content, and more preferably 29.5%~32%, it is most preferably 30%~31.2%；The matter of the Dy
It is preferably 1.0%~8.0% to measure degree, and more preferably 3.0%~7.0%, it is most preferably 4.0%~6.0%；It is described
The mass percentage content of Tb is preferably 1.0%~8.0%, more preferably 3.0%~7.0%, most preferably 4.0%~
6.0%；The mass percentage content of the Nb is preferably 1.0%~4.0%, and more preferably 1.5%~3.5%, be most preferably
1.8%~3.2%；The mass percentage content of the Al is preferably 0.2%~0.8%, and more preferably 0.4%~0.5%, most
Preferably 0.42%~0.48%；The mass percentage content of the B is preferably 0.97%~1.5%, and more preferably 0.98%
~1.4%, more preferably 0.99%~1.2% are most preferably 1.0%~1.1%；The mass percentage content of the Cu is preferred
It is most preferably 0.4%~0.6% for 0.1%~0.8%, more preferably 0.3%~0.7%；The mass percent of the Co contains
Amount is preferably 0.5%~2.0%, and more preferably 0.7%~1.5%, it is most preferably 1.0%~1.2%；The quality hundred of the Ga
It is preferably 0.3%~1.5% to divide than content, and more preferably 0.5%~1.2%, more preferably 0.7%~1.0% are most preferably
0.8%~0.9%；The mass percentage content of the Gd is preferably 0.3%~1.5%, and more preferably 0.5%~1.2%, more
Preferably 0.7%~1.0%, it is most preferably 0.8%~0.9%；The mass percentage content of the Ho is preferably 0.3%~
1.5%, more preferably 0.5%~1.2%, more preferably 0.7%~1.0% are most preferably 0.8%~0.9%；The Zr's
Mass percentage content is preferably 0.3%~1.5%, more preferably 0.5%~1.2%, more preferably 0.7%~1.0%, most
Preferably 0.8%~0.9%.
The fusion process and equipment of the neodymium iron boron raw material is not particularly limited in the present invention, ripe with those skilled in the art
The fusion process and equipment for the neodymium iron boron raw material known；The present invention does not have the quick-fried process of hydrogen and equipment of the neodymium iron boron raw material
Especially limitation, with the quick-fried process of hydrogen and equipment of neodymium iron boron raw material well known to those skilled in the art；The present invention is to the neodymium
The milling process and equipment of iron boron raw material are not particularly limited, with the milling of neodymium iron boron raw material well known to those skilled in the art
Journey and equipment, the present invention are preferably airflow milling；The present invention is to above-mentioned dispensing, melting, hydrogen are quick-fried and the process choice of milling and
Order is not particularly limited, can also be according to actual production with process choice well known to those skilled in the art and order
Situation, product quality requirement and characteristic requirements make choice or replace.
The granularity of the neodymium iron boron raw material fine powder is not particularly limited in the present invention, with neodymium well known to those skilled in the art
The granularity of iron boron raw material powder, the particle mean size of neodymium iron boron raw material fine powder of the present invention is preferably 3.0~5.0 μm, more
Preferably 3.25~4.75 μm, more preferably 3.5~4.5 μm are most preferably 3.75~4.25 μm.The present invention is to the nickel layer
Thickness is not particularly limited, and with the thickness of coating well known to those skilled in the art, those skilled in the art can basis
Practical condition, product quality requirement and product type make choice or adjust, and the present invention is to ensure anticorrosion effect, institute
The thickness for stating nickel layer is preferably 30~70nm, more preferably 35~65nm, more preferably 40~60nm, most preferably 45~
55nm。
The cladding is not particularly limited in the present invention, with cladding concept well known to those skilled in the art, with can
To be interpreted as the concepts such as part cladding, coating, plating, compound or drop coating.
The present invention coats one layer of nano level metallic nickel on neodymium iron boron raw material fine powder surface, efficiently solves neodymium iron boron powder
Particle size it is tiny, the Nd of particle surface is easily aoxidized, and rich Nd is caused to reduce, so as to effectively solve what is thereby resulted in
The problem of magnetic property of magnet reduces and magnet product corrosion resistance is poor.Meanwhile prevent agglomerates during subsequent forming
Particle group is polymerized to, is conducive to the oriented moulding of powder.
The present invention provides a kind for the treatment of process of neodymium iron boron magnetic body raw material powder, comprise the following steps：
Under conditions of protective gas, by the neodymium iron boron raw material fine powder after grinding, after carrying out plating nickel on surface, neodymium is obtained
Iron boron magnet raw material powder.
The optimum principles such as the source of raw material, composition, property described in preparation method of the present invention or specific preferred embodiment
Consistent with the optimum principle of foregoing neodymium iron boron magnetic body raw material powder and specific preferred embodiment, this is no longer going to repeat them.
The protective gas is not particularly limited in the present invention, and neodymium iron boron powder is used for well known to those skilled in the art
Protective gas in pressing process, protective gas of the present invention are preferably inert gas and/or nitrogen, more preferably argon
Gas and/or nitrogen are most preferably nitrogen.
The mode of plating nickel on surface is not particularly limited in the present invention, and those skilled in the art can be according to actual production feelings
Condition, product quality requirement and product purpose make choice or adjust, and the present invention is particularly preferred as immersing nickel plating solution carry out table
Face nickel plating.The temperature and time of plating nickel on surface of the present invention is particularly preferred as the temperature of nickel plating solution and in nickel plating solution
The time of dipping；The temperature of the plating nickel on surface is particularly preferred as 75~85 DEG C, more preferably 77~83 DEG C, most preferably 79~
81℃；The time of the plating nickel on surface is particularly preferred as 20~30min, more preferably 22~28min, most preferably 24~
26min.The ratio of the nickel plating solution and neodymium iron boron raw material fine powder is not particularly limited in the present invention, with those skilled in the art
Conventional ratio both during the plating of well known solution surface, those skilled in the art can according to practical condition,
Product quality requirement and product purpose make choice or adjust, neodymium iron boron raw material fine powder quality of the present invention and the nickel plating
The volume ratio of solution is preferably (30~50) g：1L, more preferably (33~47) g：1L, more preferably (35~45) g：1L, it is optimal
Elect (37~42) g as：1L.
The concrete composition of the nickel plating solution is not particularly limited in the present invention, with nickel plating well known to those skilled in the art
The conventional composition of solution, those skilled in the art can use according to practical condition, product quality requirement and product
Way makes choice or adjusts, and nickel plating solution of the present invention preferably includes nickel sulfate, reducing agent, complexing agent, stabilizer, buffer
And water；The reducing agent is preferably sodium hypophosphite, and the complexing agent is preferably sodium citrate, and the stabilizer is preferably sweet ammonia second
Acid, the buffer are preferably sodium lactate.The specific ratio of mentioned component is not particularly limited in the present invention, people in the art
Member can make choice or adjust according to practical condition, product quality requirement and product purpose, nickel plating of the present invention
In solution, the concentration of the nickel sulfate is preferably 25~30g/L, more preferably 26~29g/L, is most preferably 27~28g/L；Institute
The concentration for stating reducing agent is preferably 25~30g/L, more preferably 26~29g/L, is most preferably 27~28g/L；The complexing agent
Concentration be preferably 20~25g/L, more preferably 21~24g/L, be most preferably 22~23g/L；The concentration of the stabilizer is excellent
It elects 0.001~0.004g/L as, more preferably 0.0015~0.0035g/L, is most preferably 0.002~0.003g/L；It is described slow
The concentration of electuary is preferably 20~25g/L, more preferably 26~29g/L, is most preferably 27~28g/L.
The present invention is after plating nickel on surface, to consolidate coating effect, preferably also after post processing, obtains neodymium iron boron magnetic body
Raw material powder.The specific steps of the post processing are not particularly limited in the present invention, with rear place well known to those skilled in the art
Step is managed, the present invention is particularly preferred as washing, filter and drying.The present invention is not special to the process of the washing filtering
Limitation, with washing filter type well known to those skilled in the art, the present invention is particularly preferred as being washed with deionized
Filter 2~5 times；The process of the drying is not particularly limited in the present invention, is with drying course well known to those skilled in the art
Can, the present invention is particularly preferred as 90~110 DEG C of 3~6h of drying process of constant temperature, is cooled to room temperature.
The present invention will obtain a kind of neodymium iron boron magnetic body raw material powder by above-mentioned steps, i.e., what a kind of plating nickel on surface was modified
Neodymium iron boron magnetic body raw material powder, the present invention is based on the characteristic and corrosion mechanism of neodymium iron boron magnetic body, micron dimension neodymium iron boron magnetic bodies
Van der Waals force between raw material powder, the interaction of London power and magnetic force make powder be agglomerated into secondary powder particle, are formed
Little particle group causes the poor fluidity of powder, and orientation is difficult, and poor corrosion resistance.Neodymium iron boron of the present invention after grinding
Magnet raw material powder is started with, and the powder that airflow milling is ground directly coats nickel plating, and one layer of powder particle surface cladding is nano level
Nickel coating improves the oxidation resistance of neodymium iron boron powder, it is therefore prevented that powder is agglomerated into particle group in subsequent process, is conducive to
The corrosion resisting property of Sintered NdFeB magnet is greatly improved in the oriented moulding of powder.It is the experimental results showed that provided by the invention
For neodymium iron boron magnetic body prepared by neodymium iron boron magnetic body raw material powder while higher magnetic property is kept, it is minimum only that heat subtracts magnetic
0.4%, aging weightlessness is minimum to be down to 0.2mg/cm2, corrosion-resistant rank can reach 9 grades.
It is former as the neodymium iron boron magnetic body described in above-mentioned technical proposal any one the present invention also provides a kind of neodymium iron boron magnetic body
Neodymium iron boron magnetic body raw material powder prepared by feed powder end or above-mentioned technical proposal any one treatment process, by compression moulding and
It is obtained after sintering.
The neodymium iron boron magnetic body raw material powder that the present invention will be prepared by above-mentioned steps, after compression moulding and sintering
It arrives.It will be appreciated by those skilled in the art that the neodymium iron boron magnetic body raw material powder further preferably using orientation, compacting, encapsulation, it is cold
Isostatic pressed after cutting the subsequent steps such as material and sintering, finally obtains product neodymium iron boron magnetic body.The present invention is to the tool of above-mentioned subsequent step
Body technology flow and Parameter Conditions are not particularly limited, with the tool of neodymium-iron-boron preparation step well known to those skilled in the art
Body technology flow and Parameter Conditions, the present invention are particularly preferred as：Neodymium iron boron magnetic body raw material powder prepared by above-mentioned steps,
It magnetizes by mo(u)ldenpress and is orientated the green compact for being pressed into 3.9~4.3g/cm3 of density, cold isostatic press further compresses green compact, by life
Base is packed into vacuum sintering furnace, is evacuated to vacuum degree to below 0.3Pa, is warming up to 200 DEG C or so heat preservation draining gas, is warming up to
500 DEG C or so heat preservation row's organic matters are warming up to 800 DEG C of heat preservation row H2, i.e. 1020 DEG C~1050 DEG C are warming up to below main phase fusing point
Temperature liquid-phase sintering, crystal boundary richness neodymium is mutually in liquid phase state at this time, continues 60~120min of heat preservation at a temperature of this, closes heating
Device, applying argon gas to 85~100Kpa, the machine that blows in are cooled to 60 DEG C~80 DEG C and come out of the stove, and obtain blank, at processing and surface
After reason, neodymium iron boron magnetic body product is obtained.
In order to further illustrate the present invention, with reference to embodiment to a kind of neodymium iron boron magnetic body raw material powder provided by the invention
End and its treatment process, neodymium iron boron magnetic body are described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
With the verification that 38SH sintered neodymium iron boron materials are done, 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, 600Kg raw material are allotted, wherein iron staff derusts, rare earth material carry out oil-free, it is amphidromic and
The raw material prepared under conditions of Frequency Induction Heating are melted metal by vacuum melting (SC), finally obtained by rustless processing
Obtain the fast quenching Nd Fe B alloys with columnar crystal structure of sheet.
Then hydrogen dehydrogenation is inhaled in hydrogen broken furnace and is broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then led to
It crosses airflow milling and grinds the micron-sized powder of epigranular with high pressure nitrogen, powder mean particle sizes are 4.0~5.0 μm.
Then chemical nickel plating carries out airflow milling powder particle by electroless plating tank, chemical nickel-plating solution formula is as follows：
Contain nickel sulfate 23g, reducing agent sodium hypophosphite 29g, complexing agent sodium citrate 25g in every liter of solution, stabilizer is sweet
Nitrilo acetic acid 0.003g, buffer sodium lactate 23g, remaining is deionized water.
Neodymium iron boron raw material fine powder Jing Guo airflow milling is immersed in above-mentioned chemical nickel-plating solution, 76 DEG C of bath temperature, PH
It is worth for 5, directly carries out chemical nickel plating, thickness of coating is about 35nm, and process applies 20 revs/min of uniform stirring, and plating time is
20min, the neodymium iron boron raw material powder after chemical plating is cleaned by 4 deionized waters, filtering, by filtered powder constant temperature 110
DEG C drying process 5h, is cooled to room temperature, and the mo(u)ldenpress orientation that magnetizes is pressed into the green compact of density 4.0g/cm3, and cold isostatic press is into one
Step compresses green compact, and green compact are packed into vacuum sintering furnace, vacuum degree is evacuated to below 0.3Pa, is warming up to 200 DEG C or so heat preservations
Draining gas is warming up to 500 DEG C or so heat preservation row's organic matters, is warming up to 800 DEG C of heat preservation row H2, it is warming up to below main phase fusing point i.e.
1020 DEG C of temperature liquid-phase sinterings, crystal boundary richness neodymium is mutually in liquid phase state at this time, continues to keep the temperature 60min at a temperature of this, closes heating
Device, applying argon gas to 85Kpa, the machine that blows in are cooled to 60 DEG C and come out of the stove, and it is that (differently- oriented directivity is 29 rulers to 51.2*51*29mm to obtain specification
It is very little) blank.
Finally, oriented surface one side 60% is shown in into light with surface grinding machine, is glued on iron staff, is cut into inside diameter slicer
9.59*6.69*0.88 (M) black-film with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.2mm with automatic chamfering machine, removes
Burrs on edges, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 9.95*6.69*0.88's (M) to obtain size
Finished product.
Performance detection is carried out to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, referring to table 2, table 2 is real for the present invention
Apply the magnetic property of the finished product neodymium iron boron magnetic body of the preparation of example 1.
The magnetic property of finished product neodymium iron boron magnetic body prepared by 2 embodiment of the present invention 1 of table
As shown in Table 2, using powder depositing process provided by the invention, the Br and Hcj of magnet there is no variation, this shows
The treatment process of the present invention has no effect on the magnetic property and temperature stability of material.
Subtract magnetic experiment, referring to table 3, table 3 subtracts magnetic situation for the finished product neodymium iron boron magnetic body of the preparation of the embodiment of the present invention 1.
Subtract magnetic stripe part：120℃×2h；Equipment：High temperature drying case.
Finished product neodymium iron boron magnetic body prepared by 3 embodiment of the present invention 1 of table subtracts magnetic situation
| Subtract magnetic | |
| Powder depositing process | 0.5%~2.8% |
| Normal process | 5%~10% |
As shown in Table 3, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet subtracts magnetic feelings
Condition is decreased obviously.
Weightless test, referring to the reduced gravity situations for the finished product neodymium iron boron magnetic body that table 4, table 4 are prepared for the embodiment of the present invention 1.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar.
Equipment：HAST ageing ovens
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by 4 embodiment of the present invention 1 of table
| Weightlessness/mg/cm2 | |
| Powder depositing process | 0.8~1.5 |
| Normal process | 2.0~8.0 |
As shown in Table 4, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet weightlessness is bright
It is aobvious to reduce.
Salt air corrosion is tested, referring to the corrosion resistance for the finished product neodymium iron boron magnetic body that table 5, table 5 are prepared for the embodiment of the present invention 1
Energy.
Salt fog condition：
A. sodium chloride concentration:50g/l pH values:6.5~7.2；
B. spray amount:(ml/80cm2/h)=1.0~2.0；
C. pressure measuring cylinder temperature:The test temperature of the brine temp of (DEG C)=47 ± 2 (DEG C)=35 ± 2:(DEG C)=35 ± 2；
D. spray:Continuous spraying
Equipment：Salt spray test chamber
The corrosion resistance of finished product neodymium iron boron magnetic body prepared by 5 embodiment of the present invention 1 of table
| Rank | |
| Powder depositing process | 8~9 |
| Normal process | 3~7 |
As shown in Table 5, the corrosion resistance of finished product neodymium iron boron magnetic body prepared by the present invention is compared to traditional handicraft, magnet corrosion resistant
Corrosion can be obviously improved, and rank can reach 8~9.
Embodiment 2
With the verification that 42SH sintered neodymium iron boron materials are done, 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, 600Kg raw material are allotted, wherein iron staff derusts, rare earth material carry out oil-free, it is amphidromic and
The raw material prepared under conditions of Frequency Induction Heating are melted metal by vacuum melting (SC), finally obtained by rustless processing
Obtain the fast quenching Nd Fe B alloys with columnar crystal structure of sheet.
Then hydrogen dehydrogenation is inhaled in hydrogen broken furnace and is broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then led to
It crosses airflow milling and grinds the micron-sized powder of epigranular with high pressure nitrogen, powder mean particle sizes are 3.7~4.7 μm.
Then chemical nickel plating carries out airflow milling powder particle by electroless plating tank, chemical nickel-plating solution formula is as follows：
Contain nickel sulfate 28g, reducing agent sodium hypophosphite 26g, complexing agent sodium citrate 23g in every liter of solution, stabilizer is sweet
Nitrilo acetic acid 0.003g, buffer sodium lactate 22g, remaining is deionized water.
Neodymium iron boron raw material fine powder Jing Guo airflow milling is immersed in above-mentioned chemical nickel-plating solution, 80 DEG C of bath temperature, PH
It is worth for 6, directly carries out chemical nickel plating, thickness of coating is about 50nm, and process applies 18 revs/min of uniform stirring, and plating time is
25min, the neodymium iron boron raw material powder after chemical plating is cleaned by 5 deionized waters, filtering, by filtered powder constant temperature 100
DEG C drying process 5h, is cooled to room temperature, and the mo(u)ldenpress orientation that magnetizes is pressed into the green compact of density 4.3g/cm3, and cold isostatic press is into one
Step compresses green compact, and green compact are packed into vacuum sintering furnace, vacuum degree is evacuated to below 0.3Pa, is warming up to 200 DEG C or so heat preservations
Draining gas is warming up to 500 DEG C or so heat preservation row's organic matters, is warming up to 800 DEG C of heat preservation row H2, it is warming up to below main phase fusing point i.e.
1050 DEG C of temperature liquid-phase sinterings, crystal boundary richness neodymium is mutually in liquid phase state at this time, continues to keep the temperature 120min at a temperature of this, closes heating
Device, applying argon gas to 95Kpa, the machine that blows in are cooled to 80 DEG C and come out of the stove, and it is 51*47*32mm to obtain specification (differently- oriented directivity is 32 sizes)
Blank.
Finally, oriented surface one side 80% is shown in into light with surface grinding machine, is glued on iron staff, is cut into inside diameter slicer
9.59*6.69*0.88 (M) black-film with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.3mm with automatic chamfering machine, removes
Burrs on edges, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 9.95*6.69*0.88's (M) to obtain size
Finished product.
Performance detection is carried out to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, referring to table 7, table 7 is real for the present invention
Apply the magnetic property of the finished product neodymium iron boron magnetic body of the preparation of example 2.
The magnetic property of finished product neodymium iron boron magnetic body prepared by 7 embodiment of the present invention 2 of table
As shown in Table 7, using powder depositing process provided by the invention, the Br and Hcj of magnet there is no variation, but also
Have and promoted by a small margin, this shows that the treatment process of the present invention has no effect on the magnetic property and temperature stability of material.
Subtract magnetic experiment, referring to table 8, table 8 subtracts magnetic situation for the finished product neodymium iron boron magnetic body of the preparation of the embodiment of the present invention 2.
Subtract magnetic stripe part：120℃×2h；Equipment：High temperature drying case.
Finished product neodymium iron boron magnetic body prepared by 8 embodiment of the present invention 2 of table subtracts magnetic situation
| Subtract magnetic | |
| Powder depositing process | 0.6%~3% |
| Normal process | 6%~10% |
As shown in Table 8, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet subtracts magnetic feelings
Condition is decreased obviously.
Weightless test, referring to the reduced gravity situations for the finished product neodymium iron boron magnetic body that table 9, table 9 are prepared for the embodiment of the present invention 2.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar.
Equipment：HAST ageing ovens
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by 9 embodiment of the present invention 2 of table
| Weightlessness/mg/cm2 | |
| Powder depositing process | 0.2~1.6 |
| Normal process | 2.0~8.0 |
As shown in Table 9, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet weightlessness is bright
It is aobvious to reduce.
Salt air corrosion is tested, and referring to table 10, table 10 is corrosion-resistant for the finished product neodymium iron boron magnetic body of the preparation of the embodiment of the present invention 2
Performance.
Salt fog condition：
A. sodium chloride concentration:50g/l pH values:6.5~7.2；
B. spray amount:(ml/80cm2/h)=1.0~2.0；
C. pressure measuring cylinder temperature:The test temperature of the brine temp of (DEG C)=47 ± 2 (DEG C)=35 ± 2:(DEG C)=35 ± 2；
D. spray:Continuous spraying
Equipment：Salt spray test chamber
The corrosion resistance of finished product neodymium iron boron magnetic body prepared by 10 embodiment of the present invention 2 of table
| Rank | |
| Powder depositing process | 8~9 |
| Normal process | 2~7 |
As shown in Table 10, the corrosion resistance of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet is resistance to
Corrosive nature is obviously improved, and rank can reach 8~9.
Embodiment 3
With the verification that 45UH sintered neodymium iron boron materials are done, 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, 600Kg raw material are allotted, wherein iron staff derusts, rare earth material carry out oil-free, it is amphidromic and
The raw material prepared under conditions of Frequency Induction Heating are melted metal by vacuum melting (SC), finally obtained by rustless processing
Obtain the fast quenching Nd Fe B alloys with columnar crystal structure of sheet.
Then hydrogen dehydrogenation is inhaled in hydrogen broken furnace and is broken into millimetre-sized coarse granule, the further crushed particles of intermediate crusher, then led to
It crosses airflow milling and grinds the micron-sized powder of epigranular with high pressure nitrogen, powder mean particle sizes are 3.5~4.5 μm.
Then chemical nickel plating carries out airflow milling powder particle by electroless plating tank, chemical nickel-plating solution formula is as follows：
Contain nickel sulfate 26g, reducing agent sodium hypophosphite 27g, complexing agent sodium citrate 22g in every liter of solution, stabilizer is sweet
Nitrilo acetic acid 0.002g, buffer sodium lactate 21g, remaining is deionized water.
Neodymium iron boron raw material fine powder Jing Guo airflow milling is immersed in above-mentioned chemical nickel-plating solution, 85 DEG C of bath temperature, PH
It is worth for 6, directly carries out chemical nickel plating, thickness of coating is about 70nm, and process applies 19 revs/min of uniform stirring, and plating time is
25min, the neodymium iron boron raw material powder after chemical plating is cleaned by 4 deionized waters, filtering, by filtered powder constant temperature 100
DEG C drying process 6h, is cooled to room temperature, and the mo(u)ldenpress orientation that magnetizes is pressed into the green compact of density 4.0g/cm3, and cold isostatic press is into one
Step compresses green compact, and green compact are packed into vacuum sintering furnace, vacuum degree is evacuated to below 0.3Pa, is warming up to 200 DEG C or so heat preservations
Draining gas is warming up to 500 DEG C or so heat preservation row's organic matters, is warming up to 800 DEG C of heat preservation row H2, it is warming up to below main phase fusing point i.e.
1040 DEG C of temperature liquid-phase sinterings, crystal boundary richness neodymium is mutually in liquid phase state at this time, continues to keep the temperature 100min at a temperature of this, closes heating
Device, applying argon gas to 90Kpa, the machine that blows in are cooled to 80 DEG C and come out of the stove, and it is 51*47*32mm to obtain specification (differently- oriented directivity is 32 sizes)
Blank.
Finally, oriented surface one side 70% is shown in into light with surface grinding machine, is glued on iron staff, is cut into inside diameter slicer
9.59*6.69*0.88 (M) black-film with the solution oil removing removing glue for adding cleaning agent, falls the radian of 0.5mm with automatic chamfering machine, removes
Burrs on edges, by ultrasonic oil removal, pickling, passivation, automatic zincincation, it is 9.95*6.69*0.88's (M) to obtain size
Finished product.
Performance detection is carried out to finished product neodymium iron boron magnetic body prepared by the embodiment of the present invention 1, referring to table 12, table 12 is the present invention
The magnetic property of finished product neodymium iron boron magnetic body prepared by embodiment 3.
The magnetic property of finished product neodymium iron boron magnetic body prepared by 12 embodiment of the present invention 3 of table
As shown in Table 12, using powder depositing process provided by the invention, the Br and Hcj of magnet there is no variation, and
It is also promoted by a small margin, this shows that the treatment process of the present invention has no effect on the magnetic property and temperature stability of material.
Subtract magnetic experiment, referring to table 13, table 13 subtracts magnetic situation for the finished product neodymium iron boron magnetic body of the preparation of the embodiment of the present invention 3.
Subtract magnetic stripe part：120℃×2h；Equipment：High temperature drying case.
Finished product neodymium iron boron magnetic body prepared by 13 embodiment of the present invention 3 of table subtracts magnetic situation
| Subtract magnetic | |
| Powder depositing process | 0.4%~2.5% |
| Normal process | 4%~10% |
As shown in Table 13, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet subtracts magnetic
Situation is decreased obviously.
Weightless test, referring to the reduced gravity situations for the finished product neodymium iron boron magnetic body that table 14, table 14 are prepared for the embodiment of the present invention 3.
Below-G conditions：130 DEG C of temperature, humidity 100%, time 240h, pressure 2.7Bar.
Equipment：HAST ageing ovens
The reduced gravity situations of finished product neodymium iron boron magnetic body prepared by 14 embodiment of the present invention 3 of table
As shown in Table 14, the finished product neodymium iron boron magnetic body that prepared by the present invention subtracts magnetic situation compared to traditional handicraft, and magnet is weightless
It significantly reduces.
Salt air corrosion is tested, and referring to table 15, table 15 is corrosion-resistant for the finished product neodymium iron boron magnetic body of the preparation of the embodiment of the present invention 3
Performance.
Salt fog condition：
A. sodium chloride concentration:50g/l pH values:6.5~7.2；
B. spray amount:(ml/80cm2/h)=1.0~2.0；
C. pressure measuring cylinder temperature:The test temperature of the brine temp of (DEG C)=47 ± 2 (DEG C)=35 ± 2:(DEG C)=35 ± 2；
D. spray:Continuous spraying
Equipment：Salt spray test chamber
The corrosion resistance of finished product neodymium iron boron magnetic body prepared by 15 embodiment of the present invention 3 of table
| Rank | |
| Powder depositing process | 8~9 |
| Normal process | 2~8 |
As shown in Table 15, the corrosion resistance of finished product neodymium iron boron magnetic body prepared by the present invention compares traditional handicraft, and magnet is resistance to
Corrosive nature is obviously improved, and rank can reach 8~9.
A kind of neodymium iron boron magnetic body raw material powder provided by the present invention and its treatment process, neodymium iron boron magnetic body are carried out above
It is discussed in detail.Specifically a example used herein is set forth the principle of the present invention and embodiment, implements above
The explanation of example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that for the general of the art
For logical technical staff, without departing from the principle of the present invention, can also to the present invention, some improvement and modification can also be carried out, this
A little improvement and modification are also fallen into the protection domain of the claims in the present invention.
Claims (6)
1. a kind for the treatment of process of neodymium iron boron magnetic body raw material powder, which is characterized in that comprise the following steps：
Under conditions of protective gas, the neodymium iron boron raw material fine powder after airflow milling is ground after carrying out plating nickel on surface, obtains
Neodymium iron boron magnetic body raw material powder；
The neodymium iron boron magnetic body raw material powder includes neodymium iron boron raw material fine powder and the nickel layer for being coated on its surface；
The neodymium iron boron raw material fine powder is the fine powder after airflow milling is ground；
The granularity of the neodymium iron boron raw material fine powder is 3~5 μm；
The thickness of the nickel layer is 30~70nm；
The nickel plating solution of the nickel plating includes nickel sulfate, reducing agent, complexing agent, stabilizer, buffer and water.
2. treatment process according to claim 1, which is characterized in that the neodymium iron boron magnetic body raw material, by mass percentage
Composition includes：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.
3. treatment process according to claim 1, which is characterized in that the temperature of the plating nickel on surface is 75~85 DEG C, institute
The time for stating plating nickel on surface is 20~30min.
4. treatment process according to claim 1, which is characterized in that the plating nickel on surface be specially immerse nickel plating solution into
Row plating nickel on surface；
The neodymium iron boron raw material fine powder quality and the volume ratio of the nickel plating solution are (30~50) g：1L.
5. treatment process according to claim 1, which is characterized in that the reducing agent be sodium hypophosphite, the complexing agent
For sodium citrate, the stabilizer is sweet nitrilo acetic acid, and the buffer is sodium lactate；
In the nickel plating solution, the concentration of the nickel sulfate is 25~30g/L；The concentration of the reducing agent is 25~30g/L；Institute
The concentration for stating complexing agent is 20~25g/L；The concentration of the stabilizer is 0.001~0.004g/L；The concentration of the buffer
For 20~25g/L.
6. a kind of neodymium iron boron magnetic body, which is characterized in that as the neodymium iron boron prepared by Claims 1 to 5 any one treatment process
Magnet raw material powder obtains after compression moulding and sintering.
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| CN105931786A (en) * | 2016-07-14 | 2016-09-07 | 安徽万磁电子有限公司 | Dysprosium-yttrium ion implanted galvanized neodymium-iron-boron magnet and preparation method for same |
| CN106024239A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Mesoporous-material-added zinc-plated neodymium-iron-boron magnet and preparation method thereof |
| CN106024238A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof |
| CN105931787A (en) * | 2016-07-14 | 2016-09-07 | 安徽万磁电子有限公司 | Dysprosium-holmium ion implanted galvanized neodymium-iron-boron magnet and preparation method for same |
| CN106024240A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Oxidation-resistant zinc-plated neodymium-iron-boron raw material powder and preparation method thereof |
| CN105976959A (en) * | 2016-07-14 | 2016-09-28 | 安徽万磁电子有限公司 | Nickel-plating NdFeB magnet with terbium yttrium ions injected and preparation method of magnet |
| CN106024241A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Mesoporous-material-added nickel-plated neodymium-iron-boron magnet and preparation method thereof |
| CN105931785A (en) * | 2016-07-14 | 2016-09-07 | 安徽万磁电子有限公司 | Gadolinium-holmium ion-implanted nickel-plating neodymium-iron-boron magnet and preparation method thereof |
| CN106024242A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Corrosion-resistant nickel-plated neodymium-iron-boron raw material powder and preparation method thereof |
| CN106024237A (en) * | 2016-07-14 | 2016-10-12 | 安徽万磁电子有限公司 | Terbium/holmium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof |
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| CN106252012B (en) * | 2016-08-29 | 2019-01-25 | 京磁材料科技股份有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
| CN110197752B (en) * | 2019-06-13 | 2021-07-27 | 深圳市麦捷微电子科技股份有限公司 | Insulating powder process for hard-to-passivate magnetic powder and magnetic powder prepared by using insulating powder process |
| CN113539665B (en) * | 2021-07-28 | 2023-08-22 | 中国科学院宁波材料技术与工程研究所 | Method for regulating and controlling coarse grain growth of neodymium-iron-boron magnet |
| JP2023032622A (en) * | 2021-08-27 | 2023-03-09 | ミネベアミツミ株式会社 | Spindle motor and hard disk drive device |
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