CN108389710A - A kind of preparation method of high-performance neodymium-iron-boron magnet - Google Patents

A kind of preparation method of high-performance neodymium-iron-boron magnet Download PDF

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CN108389710A
CN108389710A CN201810010335.XA CN201810010335A CN108389710A CN 108389710 A CN108389710 A CN 108389710A CN 201810010335 A CN201810010335 A CN 201810010335A CN 108389710 A CN108389710 A CN 108389710A
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terbium
dysprosium
alloys
sintering
obtains
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贺琦军
林建强
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NINGBO ZHAOBAO MAGNET Co Ltd
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NINGBO ZHAOBAO MAGNET Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/66Electroplating: Baths therefor from melts
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/001Magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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 pressed, sintered or bonded together
    • H01F1/0577Alloys 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 pressed, sintered or bonded together sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266Moulding; Pressing

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  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses a kind of preparation methods of high-performance neodymium-iron-boron magnet, include the following steps:1) nearly just dividing than 2:14:1 Nd Fe B alloys raw material carries out vacuum melting and obtains Nd Fe B alloys ingot casting;2) 1) gained ingot casting is subjected to powder processed, obtains Nd Fe B alloys powder;3) 2) gained Nd Fe B alloys powder is subjected to magnetic field orientating die mould, then carries out isostatic cool pressing, obtains green compact;4) 3) gained green compact is pre-sintered, obtains the sintering briquette that consistency is 80%~90%;5) compound of dysprosium or terbium and 1 methyl, 3 ethylimidazolium chloride quinoline (MEIC) are made into fused salt, as plating solution, using the sintering briquette obtained by step 4) as cathode, dysprosium or terbium metal are as anode, it is electroplated so that adhere to the metal atomic layer of one layer of dysprosium or terbium on sintering briquette;Sintering briquette after will be electroplated in step 5) re-sinters and tempering heat treatment, obtains and finally oozes Dy/Tb magnets.It is few that gained magnet oozes dysprosium/terbium dosage, oozes Dy, oozes that Tb is efficient, and the production time is short.

Description

A kind of preparation method of high-performance neodymium-iron-boron magnet
Technical field
The present invention relates to rare-earth permanent-magnet material technical fields, more specifically, it relates to a kind of high-performance neodymium-iron-boron magnet Preparation method.
Background technology
True benevolence in assistant river of nineteen eighty-three Japan et al. uses on the basis of to RE-Fe-X ternary alloy three-partalloys study extensively Powder metallurgical technique prepares magnetic energy product and is up to 290kJ/m3Neodymium iron boron (Nd-Fe-B) sintered magnet, it is dilute to have started the third generation Native permanent-magnet material.Sintered Nd-Fe-B is widely used in military industry equipment, electro-acoustic element, motor, generator, hard disc of computer and drives Dynamic device (HDD), voice coil motor (VCM), human body NMR imaging instrument (MRI), short-wave communication tedhnology, controller, instrument, magnetic point From equipment, magnetic card disk and other need to use permanent-magnetic field device and equipment in.
Sintered NdFeB magnet is with Nd2Fe14B compounds are main phase, are around coated with the structure of Nd-rich phase.It is main Technical indicator include remanent magnetism Br, maximum magnetic energy product (BH) max, coercivity H j, Curie temperature Tc.By 20 years of researches Development has devised rational alloying component and ripe preparation process, the remanent magnetism Br of magnet is made to have reached the 96% of theoretical value More than, magnetic energy product can reach 474kJ/m3, approached theoretical magnetic energy product 512kJ/m393%.Although coercivity obtains The promotion of certain depth, but for its theoretical value 5600kA/m, still there is prodigious gap, it can reach at present Level is probably the 1/10~1/3 of its coercivity theoretical value.Neodymium iron boron magnetic body is thus greatly limited in high work temperature It is applied under degree environment.
In order to solve this problem, scientific worker has been engaged in a large amount of research, studies have shown that being oozed in neodymium iron boron magnetic body The coercivity of magnet can be improved by entering Dy or Tb, and existing technological means includes mainly that heavy rare earth alloy or Nd replace Dy/Tb oxygen Compound/fluoride, but these technologies all there is a problem of it is more or less, as the former is due to the anti-magnetic of heavy rare earth atom and iron atom Property coupling, the indexs such as the remanent magnetism of magnet and maximum magnetic energy product can substantially reduce, the Nd and Dy or Tb at the latter's main phase grain edge Oxide or fluoride directly replace, replacing velocity is very slow, to make to ooze Dy, ooze Tb efficiency very low, the production time It is long.And the dysprosium used in the above method/terbium dosage is big, it is of high cost.
Invention content
The object of the present invention is to provide a kind of dysprosium/terbium dosage is few, ooze Dy, ooze the Tb efficient production times it is short prepare high property The preparation method of energy neodymium iron boron magnetic body.
To achieve the above object, it is realized by following technological means:
A kind of preparation method of high-performance neodymium-iron-boron magnet, includes the following steps:
1) nearly just dividing than 2:14:1 Nd Fe B alloys raw material carries out vacuum melting and obtains Nd Fe B alloys ingot casting;
2) 1) gained ingot casting is subjected to powder processed, obtains Nd Fe B alloys powder;
3) 2) gained Nd Fe B alloys powder is subjected to magnetic field orientating die mould, then carries out isostatic cool pressing, obtains green compact;
4) 3) gained green compact is pre-sintered, obtains the sintering briquette that consistency is 80%~90%;
5) compound of dysprosium or terbium and 1- methyl -3- ethylimidazolium chlorides quinolines (MEIC) are made into fused salt, as plating solution, Using the sintering briquette obtained by step 4) as cathode, dysprosium or terbium metal are electroplated as anode so that on sintering briquette adhere to one layer of dysprosium or The metal atomic layer of terbium;
6) sintering briquette after will be electroplated in step 5) re-sinters and tempering heat treatment, obtains and finally oozes Dy/Tb magnetic Body.
Advanced optimize for:In step 1), the smelting technology is to use rapid hardening belt-rejecting technology that thickness is made as 0.2- The Nd Fe B alloys thin slice of 0.5mm, or Nd Fe B alloys ingot casting is made using casting ingot process.
Advanced optimize for:In step 2), the flouring technology is that alloy cast ingot is first carried out coarse crushing, is added The antioxidant of 0.02wt%-0.70wt%, it is 3~5 μm of Nd Fe B alloys powder that then air-flow, which is milled into average grain diameter,.
Advanced optimize for:Magnetic field intensity >=1.8T described in step 3), isostatic cool pressing pressure are 150-250MPa.
Advanced optimize for:It is the 900-1000 DEG C of sintering 3-5h in vacuum sintering furnace to be pre-sintered described in step 4).
Advanced optimize for:Prepare in step 5) fused salt the specific steps are:Weigh the chemical combination of quantitative anhydrous dysprosium or terbium Object and MEIC, MEIC is put into beaker, is slowly added to the compound of anhydrous dysprosium or terbium, is stirred continuously, and keeps two kinds of solids gradual It melts, is starched using the mixture of dry ice and methanol as bath in preparation process.
Advanced optimize for:The compound of the anhydrous dysprosium or terbium is dysprosium chloride, terbium chloride or dysprosium nitrate or terbium nitrate In one kind.
Advanced optimize for:Re-sintered in step 6) is that 1020-1080 DEG C of sintering 3-5h, tempering are in vacuum sintering furnace Primary tempering, or be first once tempered, carry out double tempering again, the primary tempering is carried out at 650-920 DEG C, is kept the temperature 2.5-5h, double tempering carry out at 450-650 DEG C, keep the temperature 2.5-5h.
Beneficial effects of the present invention are:The present invention is using one layer of dysprosium of plating first on not complete fully dense neodymium iron boron sintering briquette Or the metal atomic layer of terbium, metal atomic layer activity is high, and there are many gaps, metallic atom to be easy on fine and close sintering briquette It spreads, and enters inside gap thereto, during follow-up re-sinter with tempering heat treatment, the dysprosium or terbium that diffuse into advance Metallic atom is just easy to spread to magnet grain boundary, into crystal boundary, is re-sintered and tempering heat treatment by rationally controlling Temperature-time may make dysprosium or terbium to be enriched in grain boundaries, and is distributed in crystal grain inside gradient, so that oozing the surplus of Dy/Tb magnets Magnet coercivity is improved while magnetic and magnetic energy product do not significantly reduce, to obtain high performance Sintered NdFeB magnet.
The advantages of the present invention over the prior art are that:1) atomic layer level thickness obtained by plating atomic layer is uniform, and metal is former Son is fast to inner diffusing rate, that is, oozes that Dy, to ooze Tb efficient;2) metallic atom is active in the atomic layer being electroplated, and inwardly diffusion is rapid, So that Dy/Tb raw materials needed for final are few, significant effect;3) gained magnet coercivity greatly improves, and remanent magnetism and magnetic energy product reduce not Obviously.
Specific implementation mode
Invention is described in further detail below by specific embodiment, following embodiment is descriptive, is not to limit Protection scope of the present invention of property.
Embodiment 1
Design is based on 2:14:The Nd Fe B alloys ingredient Nd11.76Fe82.36B5.88 (atomic percentage) of 1 phase, according to The raw metal that purity is 99.9wt% is put into and gets rid of band in rapid hardening furnace the neodymium that thickness is 0.25mm is made by the ingredient composition of design Ferroboron thin slice;Then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 70ml/min, reacted 4 hours, hydrogen is broken to obtain 60 Mesh powder particle;Then the antioxidant of 0.05wt% is added, is transferred to the neodymium iron boron conjunction ground in airflow milling and be made 5 μm in 2 hours Bronze end, by gained powder in the magnetic fields 1.8T oriented moulding and through 200MPa isostatic presseds, obtain green compact;Green compact is put into vacuum to burn It is sintered 3 hours for 940 DEG C in freezing of a furnace, the sintering briquette that consistency is 82% is made;It starches, will burn using the mixture of dry ice and methanol as bath Cup is put into bath paddle, weighs quantitative anhydrous terbium chloride and 1- methyl -3- ethylimidazolium chlorides quinolines (MEIC), MEIC is put into In beaker, it is slowly added to anhydrous terbium chloride, is stirred continuously, so that two kinds of solids is gradually melted, be made into bath salt, using sintering briquette as the moon Pole, as plating solution, terbium metal is electroplated the fused salt that terbium chloride and MEIC are made into as anode so that adheres to one on sintering briquette Then the sintering briquette for being coated with metal atomic layer is put into vacuum sintering furnace 1020 DEG C and is sintered 3 hours, so by the metal atomic layer of layer terbium Keep the temperature 2.5 hours at 650 DEG C afterwards, air quenching to room temperature, be then warming up to again 450 DEG C keep the temperature 2.5 hours, air quenching to room temperature to get Required magnet A1.
Embodiment 2
Design is based on 2:14:The Nd Fe B alloys ingredient Nd8.82Pr2.94Fe80.00Co1.36Zr1.00B5.88 of 1 phase The raw metal that purity is 99.9wt% is put into rapid hardening furnace according to the ingredient composition of design and gets rid of band system by (atomic percentage) At the Nd Fe B alloys thin slice that thickness is 0.3mm;Then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 72ml/min, instead It answers 4 hours, hydrogen is broken to obtain 70 mesh powder particles;Then the antioxidant of 0.10wt% is added, is transferred in airflow milling and grinds 3 hours 4.5 μm of Nd Fe B alloys powder is made, by gained powder in the magnetic fields 1.8T oriented moulding and through 200MPa isostatic presseds, must press Base;Green compact is put into vacuum sintering furnace and is sintered 3.2 hours for 960 DEG C, the sintering briquette that consistency is 85% is made;With dry ice and methanol Mixture as bath starch, by beaker be put into bath paddle in, weigh quantitative anhydrous dysprosium chloride and 1- methyl -3- ethylimidazolium chlorides Quinoline (MEIC), MEIC is put into beaker, is slowly added to anhydrous dysprosium chloride, is stirred continuously, and so that two kinds of solids is gradually melted, is matched At bath salt, using sintering briquette as cathode, the fused salt that dysprosium chloride and MEIC are made into carries out electricity as plating solution, dysprosium metal as anode Plating so that the then sintering briquette for being coated with metal atomic layer is put into vacuum sintering furnace by the metal atomic layer for adhering to one layer of dysprosium on sintering briquette In 1050 DEG C be sintered 3 hours, then keep the temperature 3 hours at 650 DEG C, air quenching to room temperature, be then warming up to again 480 DEG C heat preservation 3 hours, Air quenching is to room temperature to get required magnet A2.
Embodiment 3
Design is based on 2:14:The Nd Fe B alloys ingredient Nd8.82Pr2.94Fe81.3Al1.00B5.88 (atoms hundred of 1 phase Score), according to the ingredient composition of design, the raw metal that purity is 99.9wt% is put into rapid hardening furnace to get rid of band thickness is made it is The Nd Fe B alloys thin slice of 0.3mm;Then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 74ml/min, reacted 4 hours, Hydrogen is broken to obtain 80 mesh powder particles;Then the antioxidant of 0.20wt% is added, is transferred in airflow milling and grinds 4 hours obtained 4.0 μ The Nd Fe B alloys powder of m, by gained powder in the magnetic fields 1.8T oriented moulding and through 200MPa isostatic presseds, obtain green compact;It will pressure Base is put into vacuum sintering furnace and is sintered 3.5 hours for 980 DEG C, and the sintering briquette that consistency is 87% is made;With the mixing of dry ice and methanol Object is starched as bath, and beaker is put into bath paddle, quantitative anhydrous nitric acid dysprosium and 1- methyl -3- ethylimidazolium chloride quinolines are weighed (MEIC), MEIC is put into beaker, is slowly added to anhydrous nitric acid dysprosium, is stirred continuously, so that two kinds of solids is gradually melted, be made into bath Salt, using sintering briquette as cathode, as plating solution, dysprosium metal is electroplated as anode, is made the fused salt that dysprosium nitrate and MEIC are made into The metal atomic layer for adhering to one layer of dysprosium on sintering briquette is obtained, then the sintering briquette for being coated with dysprosium metal atomic layer is put into vacuum sintering furnace 1080 DEG C are sintered 3 hours, then keep the temperature 4 hours at 690 DEG C, air quenching to room temperature, are then warming up to 500 DEG C again and keep the temperature 4 hours, gas It quenches to room temperature to get required magnet A3.
Embodiment 4
Design is based on 2:14:The Nd Fe B alloys ingredient Nd8.82Ce2.94Fe81.3Al1.00Zn0.06B5.88 of 1 phase The raw metal that purity is 99.9wt% is put into rapid hardening furnace according to the ingredient composition of design and gets rid of band system by (atomic percentage) At the Nd Fe B alloys thin slice that thickness is 0.3mm;Then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 76ml/min, instead It answers 5 hours, hydrogen is broken to obtain 80 mesh powder particles;Then the antioxidant of 0.20wt% is added, is transferred in airflow milling and grinds 5 hours 3.5 μm of Nd Fe B alloys powder is made, by gained powder in the magnetic fields 1.8T oriented moulding and through 200MPa isostatic presseds, must press Base;Green compact is put into vacuum sintering furnace and is sintered 3.6 hours for 1000 DEG C, the sintering briquette that consistency is 88% is made;With dry ice and first The mixture of alcohol is starched as bath, and beaker is put into bath paddle, quantitative anhydrous nitric acid terbium and 1- methyl -3- ethylmercury chloride miaows are weighed Oxazoline (MEIC), MEIC is put into beaker, is slowly added to anhydrous nitric acid terbium, is stirred continuously, and two kinds of solids is made gradually to melt, It is made into bath salt, using sintering briquette as cathode, the fused salt that terbium nitrate and MEIC are made into is carried out as plating solution, terbium metal as anode Plating so that adhere to the metal atomic layer of one layer of dysprosium on sintering briquette, the sintering briquette for being coated with terbium metal atomic layer, which is then put into vacuum, burns It is sintered 3 hours for 1030 DEG C in freezing of a furnace, then keeps the temperature 3 hours at 700 DEG C, then air quenching to room temperature is warming up to 550 DEG C of heat preservations 3 again Hour, air quenching to room temperature is to get required magnet A4.
Embodiment 5
Design is based on 2:14:The Nd Fe B alloys ingredient Nd8.82Pr2.94Fe80.00Ga1.36In1.00B5.88 of 1 phase The raw metal that purity is 99.9wt% is put into rapid hardening furnace according to the ingredient composition of design and gets rid of band system by (atomic percentage) At the Nd Fe B alloys thin slice that thickness is 0.3mm;Then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 80ml/min, instead It answers 4 hours, hydrogen is broken to obtain 100 mesh powder particles;Then the antioxidant of 0.30wt% is added, it is small to be transferred to mill 8 in airflow milling When 2.5 μm of Nd Fe B alloys powder is made, by gained powder in the magnetic fields 1.8T oriented moulding and through 200MPa isostatic presseds, obtain Green compact;Green compact is put into vacuum sintering furnace and is sintered 3.2 hours for 920 DEG C, the sintering briquette that consistency is 87% is made;With dry ice and first The mixture of alcohol is starched as bath, and beaker is put into bath paddle, quantitative anhydrous nitric acid terbium and 1- methyl -3- ethylmercury chloride miaows are weighed Oxazoline (MEIC), MEIC is put into beaker, is slowly added to anhydrous nitric acid terbium, is stirred continuously, and two kinds of solids is made gradually to melt, It is made into bath salt, using sintering briquette as cathode, the fused salt that terbium nitrate and MEIC are made into is carried out as plating solution, terbium metal as anode Plating so that adhere to the metal atomic layer of one layer of dysprosium on sintering briquette, the sintering briquette for being coated with terbium metal atomic layer, which is then put into vacuum, burns It is sintered 3 hours for 1050 DEG C in freezing of a furnace, then keeps the temperature 3 hours at 850 DEG C, then air quenching to room temperature is warming up to 600 DEG C of heat preservations 3 again Hour, air quenching to room temperature is to get required magnet A5.
The magnet of gained in embodiment 1 to 5 is tested for the property, the results are shown in Table 1.
The performance of 1 magnet A1 to A5 of table
Intrinsic coercivity kOe Remanent magnetism kGs Magnetic energy product MGOe
A1 18.42 13.37 44.5
A2 20.39 13.17 43.5
A3 17.95 13.27 43.5
A4 19.39 13.77 46.3
A5 18.93 13.17 42.9
From table 1 it follows that the coercivity of gained magnet is improved, while remanent magnetism and magnetic energy product do not significantly reduce, The magnet of high magnetic characteristics is obtained.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (8)

1. a kind of preparation method of high-performance neodymium-iron-boron magnet, which is characterized in that include the following steps:
1) nearly just dividing than 2:14:1 Nd Fe B alloys raw material carries out vacuum melting and obtains Nd Fe B alloys ingot casting;
2) 1) gained ingot casting is subjected to powder processed, obtains Nd Fe B alloys powder;
3) 2) gained Nd Fe B alloys powder is subjected to magnetic field orientating die mould, then carries out isostatic cool pressing, obtains green compact;
4) 3) gained green compact is pre-sintered, obtains the sintering briquette that consistency is 80%~90%;
5) compound of dysprosium or terbium and 1- methyl -3- ethylimidazolium chlorides quinolines (MEIC) are made into fused salt, as plating solution, with step It is rapid 4) obtained by sintering briquette as cathode, dysprosium or terbium metal as anode, be electroplated so that adhere to one layer of dysprosium or terbium on sintering briquette Metal atomic layer;
6) sintering briquette after will be electroplated in step 5) re-sinters and tempering heat treatment, obtains and finally oozes Dy/Tb magnets.
2. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that in step 1), The smelting technology is to use rapid hardening belt-rejecting technology that thickness is made as the Nd Fe B alloys thin slice of 0.2-0.5mm, or use ingot casting Nd Fe B alloys ingot casting is made in technique.
3. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that in step 2), The flouring technology is that alloy cast ingot is first carried out coarse crushing, the antioxidant of 0.02wt%-0.70wt% is added, then air-flow It is milled into the Nd Fe B alloys powder that average grain diameter is 3~5 μm.
4. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that institute in step 3) Magnetic field intensity >=1.8T is stated, isostatic cool pressing pressure is 150-250MPa.
5. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that institute in step 4) It is the 900-1000 DEG C of sintering 3-5h in vacuum sintering furnace to state pre-sintering.
6. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that match in step 5) Fused salt processed the specific steps are:The compound and MEIC for weighing quantitative anhydrous dysprosium or terbium, MEIC is put into beaker, is slowly added The compound for entering anhydrous dysprosium or terbium, is stirred continuously, and so that two kinds of solids is gradually melted, with the mixing of dry ice and methanol in preparation process Object is starched as bath.
7. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 6, which is characterized in that described is anhydrous The compound of dysprosium or terbium is one kind in dysprosium chloride, terbium chloride or dysprosium nitrate or terbium nitrate.
8. a kind of preparation method of high-performance neodymium-iron-boron magnet according to claim 1, which is characterized in that in step 6) again Sintering is the 1020-1080 DEG C of sintering 3-5h in vacuum sintering furnace, and tempering is once to be tempered, or be first once tempered, again Carry out double tempering, it is described it is primary tempering carried out at 650-920 DEG C, keep the temperature 2.5-5h, double tempering at 450-650 DEG C into Row keeps the temperature 2.5-5h.
CN201810010335.XA 2018-01-05 2018-01-05 A kind of preparation method of high-performance neodymium-iron-boron magnet Pending CN108389710A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113223847A (en) * 2021-04-28 2021-08-06 慈溪市兴发磁业科技有限公司 Preparation method of neodymium iron boron magnetic material and magnetic material prepared by adopting method

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1737205A (en) * 2005-07-19 2006-02-22 郑州大学 Surface treatment method for magnesium alloy
CN102103916A (en) * 2009-12-17 2011-06-22 北京有色金属研究总院 Preparation method of neodymium iron boron magnet
CN104332264A (en) * 2014-10-13 2015-02-04 宁波尼兰德磁业有限公司 Method for enhancing properties of sintered neodymium-iron-boron magnets
CN104388992A (en) * 2014-12-19 2015-03-04 中物院成都科学技术发展中心 Method for co-deposition of Al-Zn alloy coating in ionic liquid system
CN104388952A (en) * 2014-12-04 2015-03-04 北京科技大学 Method for accelerating permeation of Dy/Tb adhesive layer on surface of sintered neodymium-iron-boron magnet
CN105200475A (en) * 2015-10-29 2015-12-30 中物院成都科学技术发展中心 Bolt electroplating pretreatment method
CN105489334A (en) * 2016-01-14 2016-04-13 北京科技大学 Method for obtaining high-magnetism sintered NdFeB through grain boundary diffusion
CN106128672A (en) * 2016-06-20 2016-11-16 钢铁研究总院 A kind of diffusion-sintering serialization RE Fe B magnet and preparation method thereof
CN106169346A (en) * 2016-08-31 2016-11-30 浙江凯文磁业有限公司 A kind of neodymium iron boron plating Dy thin-film technique

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1737205A (en) * 2005-07-19 2006-02-22 郑州大学 Surface treatment method for magnesium alloy
CN102103916A (en) * 2009-12-17 2011-06-22 北京有色金属研究总院 Preparation method of neodymium iron boron magnet
CN104332264A (en) * 2014-10-13 2015-02-04 宁波尼兰德磁业有限公司 Method for enhancing properties of sintered neodymium-iron-boron magnets
CN104388952A (en) * 2014-12-04 2015-03-04 北京科技大学 Method for accelerating permeation of Dy/Tb adhesive layer on surface of sintered neodymium-iron-boron magnet
CN104388992A (en) * 2014-12-19 2015-03-04 中物院成都科学技术发展中心 Method for co-deposition of Al-Zn alloy coating in ionic liquid system
CN105200475A (en) * 2015-10-29 2015-12-30 中物院成都科学技术发展中心 Bolt electroplating pretreatment method
CN105489334A (en) * 2016-01-14 2016-04-13 北京科技大学 Method for obtaining high-magnetism sintered NdFeB through grain boundary diffusion
CN106128672A (en) * 2016-06-20 2016-11-16 钢铁研究总院 A kind of diffusion-sintering serialization RE Fe B magnet and preparation method thereof
CN106169346A (en) * 2016-08-31 2016-11-30 浙江凯文磁业有限公司 A kind of neodymium iron boron plating Dy thin-film technique

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113223847A (en) * 2021-04-28 2021-08-06 慈溪市兴发磁业科技有限公司 Preparation method of neodymium iron boron magnetic material and magnetic material prepared by adopting method

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Application publication date: 20180810