CN106601404A - Method for reforming sintered neodymium-iron-boron waste blank - Google Patents

Method for reforming sintered neodymium-iron-boron waste blank Download PDF

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CN106601404A
CN106601404A CN201611239448.4A CN201611239448A CN106601404A CN 106601404 A CN106601404 A CN 106601404A CN 201611239448 A CN201611239448 A CN 201611239448A CN 106601404 A CN106601404 A CN 106601404A
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sintered ndfeb
powder
body material
iron
boron
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CN106601404B (en
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刘宇晖
樊玉川
王志坚
欧阳宇平
陈云志
王川
朱望伟
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Hunan Rare Earth New Engergy Material Co., Ltd.
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HUNAN RESEARCH INSTITUTE OF RARE EARTH METAL MATERIALS
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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
    • 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
    • H01F1/0576Alloys 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 pressed, e.g. hot working
    • 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
    • H01F41/0266Moulding; Pressing

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a method for reforming a sintered neodymium-iron-boron waste blank. The method comprises the steps as follows: the sintered neodymium-iron-boron waste blank is crushed in a protective gas atmosphere until the particle sizes do not exceed 150 meshes to obtain waste powder; the waste powder is mixed with a disperse solvent to obtain mixed powder, wherein the mass ratio of the disperse solvent to the waste powder does not exceed 0.2%; the mixed powder is pressed in a pressing mold under the condition that the oriented magnetic field intensity is not smaller than 1.7T to obtain a green body, wherein the mass of the mixed powder added to the pressing mold is 100.5%-102% of theoretical mass of neodymium-iron-boron powder required by a to-be-prepared sintered neodymium-iron-boron magnet; and isostatic pressing is carried out on the green body and then vacuum sintering treatment is carried out to obtain a sintered neodymium-iron-boron magnet. The method is simple in process and low in equipment requirement, the utilization rate of the sintered neodymium-iron-boron waste blank is high and the cost is low. According to the obtained neodymium-iron-boron magnet, an abnormal growth phenomenon of section grains is avoided and the magnetic properties of residual magnetism, intrinsic coercive force, maximum magnetic energy product and the like all can reach the use standard.

Description

The method of sintered NdFeB scrap body material reshaping
Technical field
The present invention relates to neodymium iron boron magnetic body technical field, more particularly to a kind of side of sintered NdFeB scrap body material reshaping Method.
Background technology
The preparation flow of Sintered NdFeB magnet is generally melting, broken hydrogen, powder processed, compressing, isostatic pressed at present, reburns Knot.Compressing is committed step therein, molding be by made by pressed by powder into green compact.And due to powder granularity, equipment, The impact of the factor such as operator and technological parameter, the compressing green compact for obtaining can produce cracking, concentric reducer, fall lid, chipping Or the defective work such as off-dimension.As the compressing waste material for obtaining is without isostatic pressed and sintering processes, typically by which Collection is recycled after treatment.
The recycling research of the waste material that molding is obtained experienced three developmental stage.First stage is to aoxidize waste material, Rare earth metal therein is reclaimed with Wet-process metallurgy method again, but the method technological process is long, the response rate is low, cost recovery It is high.Second stage is that waste material is sintered directly into blank, then melts down melting, and the broken powder aftershaping processed of hydrogen, sintering make neodymium-iron-boron Body;Although the method technological process is shortened, utilization rate increases, but its quality is wayward, and processing cost is still higher. Phase III is by waste material categorised collection and the powder body that is broken into below 40 mesh, using airflow milling powder, then is mixed with regular burden(ing), Molding, sintering make neodymium iron boron magnetic body.But the method airflow milling dispersing technology require it is strict, be limited only to similar waste material while Process, the bad powder body of granularity concordance adds airflow milling to be easily caused charging Hatch Opening and blocks, this to operation bring difficulty and Potential safety hazard, also have impact on the utilization rate of equipment;Also some waste material resting period length are caused to affect the property that waste material is recycled simultaneously Energy.Additionally, unavoidably becoming superfine powder using a part of powder body of airflow milling process, and then affect the utilization rate of powder body.
The content of the invention
Based on this, it is necessary to provide the neodymium iron boron magnetic body that a kind of process is simple, low for equipment requirements, utilization rate are high and obtain The method of the good sintered NdFeB scrap body material reshaping of performance.
A kind of method of sintered NdFeB scrap body material reshaping, comprises the following steps:
Sintered NdFeB scrap body material is crushed to into particle diameter less than 150 mesh in protective gas atmosphere, waste material powder body is obtained;
The waste material powder body is mixed with dispersion solvent, mixed powder, the dispersion solvent and the waste material powder body is obtained Mass ratio be less than 0.2%;
The mixed powder is placed in compacting tool set and is suppressed under conditions of alignment magnetic field is not less than 1.7T, obtained Green compact, the quality of the mixed powder being added in the compacting tool set neodymium ferrum for needed for Sintered NdFeB magnet to be prepared The 100.5%~102% of boron powder body Theoretical Mass;
The green compact are carried out into isostatic pressing, then carries out vacuum-sintering process, obtain the Sintered NdFeB magnet.
The method of above-mentioned sintered NdFeB scrap body material reshaping, process is simple are low for equipment requirements, and to sintering neodymium ferrum The utilization rate of boron scrap body material is high, low cost.The method adopts sintered NdFeB scrap body material, controls waste material powder body by preliminary crushing Particle diameter, add dispersion solvent and control the mixed powder in compacting tool set amount carry out suppressing, isostatic pressed, sintering processes, And then sintered NdFeB scrap body material reshaping is caused, and obtain neodymium iron boron magnetic body.The neodymium iron boron magnetic body for obtaining, section crystal grain are as good as Often grow up phenomenon, and which can be reached using normal neodymium iron boron in remanent magnetism, the interior coercivity, maximum magnetic energy product equimagnetic performance indications grasped Powder body prepares the performance of neodymium iron boron magnetic body.The method of the sintered NdFeB scrap body material reshaping returning to sintered NdFeB scrap body material Receive and recycle there is provided good approach, with huge practical value.
Wherein in one embodiment, it is to crush simultaneously in nitrogen atmosphere by the condition that the sintered NdFeB scrap body material is crushed Particle diameter is controlled in vibrosieve to less than 150 mesh.
Wherein in one embodiment, sintered NdFeB scrap body material is crushed to into particle diameter for 80~150 mesh.
Wherein in one embodiment, also including add antioxidant the step of:By the waste material powder body and the dispersion Solvent and antioxidant mixing, obtain mixed powder.
Wherein in one embodiment, the antioxidant is poly(ethylene oxide) allyl ether and poly(ethylene oxide) pi-allyl At least one in glycidyl ether;The antioxidant is less than 0.1% with the mass ratio of the waste material powder body.
Wherein in one embodiment, it is 0.4~0.8MPa that the mixed powder is placed in the pressure suppressed in compacting tool set.
Wherein in one embodiment, the pressure of the isostatic pressing is not less than 150MPa.
Wherein in one embodiment, the condition that the vacuum-sintering is processed is little in 1060~1090 DEG C of insulations 4~6 When.
Wherein in one embodiment, after the vacuum-sintering process step, also including Ageing Treatment step.
Wherein in one embodiment, the condition of the Ageing Treatment is that 2~4h are incubated prior to 800~900 DEG C, then at 400~500 DEG C of 2~4h of insulation.
Description of the drawings
Fig. 1 is the flow chart of the method for the sintered NdFeB scrap body material reshaping of an embodiment.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing Give the preferred embodiment of the present invention.But, the present invention can be realized in many different forms, however it is not limited to herein Described embodiment.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more saturating It is thorough comprehensive.
Fig. 1 is referred to, the method for the sintered NdFeB scrap body material reshaping of one embodiment of the invention is comprised the following steps.
Step S1:Sintered NdFeB scrap body material is crushed to into particle diameter less than 150 mesh in protective gas atmosphere, is given up Feed powder body.
Sintered NdFeB scrap body material is crushed by step S1 in protective gas atmosphere, in order to avoid sintered NdFeB scrap body material oxygen Change.Sintered NdFeB scrap body material is crushed to less than 150 mesh, it is to avoid particle diameter causes greatly very much that neodymium iron boron magnetic body is uneven to ask Topic, and realize that the Particle size requirements, without the need for special installations such as airflow millings, are capable of achieving using manual type, therefore in S1, sinter neodymium Ferrum boron scrap body material can be converted into waste material powder body, so it is high to the utilization rate of sintered NdFeB scrap body material.
Specifically, sintered NdFeB scrap body material should carry out pulverization process in time, it is to avoid resting period length causes to sinter neodymium ferrum The bonding reunion of boron scrap body material granule is difficult to disperse.Preferably, from obtain sintered NdFeB scrap body material between being crushed when Between interval less than 20h;It is furthermore preferred that the time interval is less than 8h.
Preferably, it is to crush in nitrogen atmosphere and control grain in vibrosieve by the condition that sintered NdFeB scrap body material is crushed Footpath is to less than 150 mesh.So can further promote the dispersion of waste material powder body using the vibrational energy of vibrosieve, obtain dispersibility Preferable waste material powder body.Specifically, the step of sintered NdFeB scrap body material is crushed is carried out in glove box, and is adopted in glove box Nitrogen atmosphere, the oxygen quality content controlled in glove box are less than 0.1%.
Specifically, the step of " sintered NdFeB scrap body material being crushed in protective gas atmosphere " is to " controlling in the vibrosieve Granulation footpath is to being less than 150 mesh " the step of both time interval be less than 72h, in order to avoid there is serious group in the powder body after crushing It is poly-.
Preferably, sintered NdFeB scrap body material is crushed to into particle diameter for 80~150 mesh.Obtain the waste powder of the particle size range Body, can both meet the needs of follow-up compacting, and without the need for special installations such as airflow millings, and the utilization rate of waste material powder body is high.
Step S2:Waste material powder body is mixed with dispersion solvent, the quality of mixed powder, dispersion solvent and waste material powder body is obtained Than less than 0.2%.
Step S2 is scattered in waste material powder body in dispersion solvent, obtains mixed powder, on the one hand can effectively prevent waste powder Body is reunited, on the other hand can avoid waste material powder body excessively disperse to cause its step S3 carry out compacting cannot molding, dispersion solvent The frictional force reduced in waste powder body is also acted as, the magnet degree of orientation is improved, is allowed to adapt to the needs of subsequent step moulding process.Point The quality of scattered solvent can not be too high, and otherwise mobility is too strong, can also affect subsequent forming.
Preferably, dispersion solvent is the mixture of solvent naphtha and lubricant.Specifically, solvent naphtha can for No. 93 gasoline, 97 At least one in number gasoline and No. 120 industrial napthas.Specifically, lubricant is zinc stearate.The matter of lubricant and solvent naphtha Amount is than less than 1:20.
Wherein in one embodiment, step S2 also includes the step of adding antioxidant:Will be waste material powder body molten with dispersion Agent and antioxidant mixing, obtain mixed powder.Add antioxidant to be to avoid waste material powder body from being oxidized in step S2, and add Dispersion solvent can also increase the dissolving of antioxidant.Preferably, antioxidant is less than 0.1% with the mass ratio of waste material powder body. It is furthermore preferred that antioxidant is at least in poly(ethylene oxide) allyl ether and poly(ethylene oxide) allyl glycidyl ether Kind.
The time that wherein waste material powder body is mixed with gasoline, antioxidant is different according to the quality of mixed powder;Typically , the time that waste material powder body is mixed with gasoline, antioxidant is not less than 2h for the mixed powder incorporation time of 300Kg.
Step S3:Mixed powder is placed in compacting tool set and is suppressed under conditions of alignment magnetic field is not less than 1.7T, Green compact are obtained, the quality of the mixed powder being added in the compacting tool set Nd-Fe-B powder for needed for Sintered NdFeB magnet to be prepared The 100.5%~102% of body Theoretical Mass.
In neodymium iron boron production process, according to the suitable compacting tool set of size Selection of neodymium iron boron magnetic body to be prepared, have Square, cylinder etc., commonly referred to as mould direction, differently- oriented directivity and pressing direction size, mould mould direction and are taken once selecting It is relatively fixed to direction size, variable is pressing direction.It is different with pressing pressure that compacting height throws powder amount with single mode.Single mode is thrown Powder amount theoretical value can be calculated according to the theoretical size of neodymium iron boron magnetic body to be prepared and magnet density.
Wherein, neodymium iron boron powder body Theoretical Mass needed for Sintered NdFeB magnet to be prepared is volume and the neodymium for needing to obtain The quality of the corresponding neodymium iron boron powder body of size of iron boron magnet, which can be calculated by the density of neodymium iron boron powder body and theoretical size Arrive.
Waste material powder body and the compression ratio of neodymium iron boron powder body that the present invention is obtained by research discovery sintered NdFeB scrap body material Property that there is some difference, the compression ratio of the waste material powder body that sintered NdFeB scrap body material of the present invention is obtained are bigger, therefore in compacting step The rapid appropriate mixed powder that increases is added to the amount in compacting tool set, and then causes subsequent step S4 to obtain closely knit neodymium-iron-boron Body.
Preferably, it is 0.4~0.8MPa that mixed powder is placed in the pressure suppressed in compacting tool set.
In step S3, alignment magnetic field is not less than 1.7T, to ensure the degree of orientation of step S4 neodymium iron boron magnetic body, and then obtains To the preferable neodymium iron boron magnetic body of magnetic property.Preferably, the alignment magnetic field is 1.8T~2.0T.Under the magnetic field intensity, The degree of orientation of neodymium iron boron magnetic body can be ensured.Specifically, the orientation electric current control that alignment magnetic field is applied by control in step S3 System.
Step S4:Green compact are carried out into isostatic pressing, then carries out vacuum-sintering process, obtain Sintered NdFeB magnet.
The green compact for obtaining are suppressed merely through the pressure of vertical direction, and its pressure being subject to comes solely from certain orientation, so The uniformity of green compact is not good, and the pressure suppressed is less, obtains green compact compactness inadequate;Therefore by green compact carry out isostatic pressed into Type so as to which all directions are subject to uniform pressure, to ensure its uniformity and compactness, it is ensured that the neodymium-iron-boron obtained after sintering External shape meets the requirements, and form and position tolerance reaches requirement, and and then improves the magnetic properties such as remanent magnetism, maximum magnetic energy product.
Preferably, the pressure of isostatic pressing is not less than 150MPa.
Preferably, the condition that vacuum-sintering is processed is to be incubated 4~6 hours in 1060~1090 DEG C.Preferably, vacuum-sintering The vacuum of process is less than 2Pa.
Wherein in one embodiment, after vacuum-sintering process step, also including Ageing Treatment step.Enter after sintering Row Ageing Treatment is further ensured that neodymium iron boron magnetic body obtains preferable magnetic property.
Preferably, the condition of Ageing Treatment be prior to 800~900 DEG C insulation 2~4h, then at 400~500 DEG C insulation 2~ 4h。
The method of above-mentioned sintered NdFeB scrap body material reshaping, process is simple are low for equipment requirements, and to sintering neodymium ferrum The utilization rate of boron scrap body material is high, low cost.The method adopts sintered NdFeB scrap body material, controls waste material powder body by preliminary crushing Particle diameter, add dispersion solvent and control the mixed powder in compacting tool set amount carry out suppressing, isostatic pressed, sintering processes, And then sintered NdFeB scrap body material reshaping is caused, and obtain neodymium iron boron magnetic body.The neodymium iron boron magnetic body for obtaining, section crystal grain are as good as Often grow up phenomenon, and its remanent magnetism, it is interior grasp reach in the aspect performance such as coercivity, maximum magnetic energy product and molding adopt neodymium Ferrum boron powder body prepares the performance of neodymium iron boron magnetic body.
The method of the sintered NdFeB scrap body material reshaping is provided very to the recycling of sintered NdFeB scrap body material Good approach, with huge practical value.
It is below specific embodiment.
Comparative example 1
It is by raw material neodymium iron boron (the 45SH neodymium iron boron rejection tablets of Hunan Research Institute of Rare Earth Metal Materials) after hydrogen is broken, mixed by one-level Material obtains powder body in airflow milling powder.By powder body, No. 120 industrial napthas and antioxidant three according to mass ratio 1000:0.5: 0.2 mixes 2h in batch mixer, obtains mixed powder.
Mixed powder is added in square compacting tool set.The quality of the mixed powder in addition compacting tool set is 378g, The size of compacting tool set is 60.5mm*57.5mm*28.4mm.(density of neodymium iron boron powder body is with 7.55g/cm3Calculate, No. 120 molten The quality of agent gasoline and antioxidant is negligible).Direction of adjustment electric current causes magnetic field intensity up to 1.6T for 100A, in pressure Push for 2MPa and green compact are obtained.
Green compact are carried out into isostatic pressing in 150Mpa, then vacuum is in 1080 DEG C under 2Pa in vacuum sintering furnace Sintering 5 hours, then at 900 DEG C of insulation 2h, being incubated 2h after 500 DEG C carries out Ageing Treatment, obtains neodymium iron boron magnetic body.
Embodiment 1
The unqualified lifes such as lid, cracking, dimension overproof by what is produced in pressing process in the preparation method using comparative example 1 Base is used as sintered NdFeB scrap body material raw material.The unqualified green compact are sealed with packaging bag evacuation, is carried out using manual type Break into pieces.The waste material broken into pieces is put in the glove box of nitrogen atmosphere, control glove box in oxygen quality content be down to 0.05% with When lower, open the package, the waste material broken into pieces is loaded in mixing tank and 308 kilograms is reached to waste material weight.By mixing tank and 100 mesh Vibrating scalper connects, nitrogen charging gas shielded, and oxygen quality content is controlled below 0.15%, and waste material is sieved, after 78 minutes all Sieve and finish, obtain waste material powder body.
It is 1000 in mass ratio by waste material powder body, No. 120 industrial napthas, zinc stearate and poly(ethylene oxide) allyl ethers: 1:0.05:0.2 is placed in batch mixer mixing 2h, obtains mixed powder.
It is mixed in compacting tool set by, in mixed powder input and the square compacting tool set of 1 identical of comparative example, adding every time The quality for closing powder body is 381.5g.Direction of adjustment electric current causes magnetic field intensity up to 1.7T for 102A, pushes for 0.4MPa in pressure Green compact are obtained.
Green compact are carried out into isostatic pressing and is controlled at compact dimensions, vacuum-sintering process and timeliness by isostatic tooling The step of reason, is identical with comparative example 1, obtains neodymium iron boron magnetic body.
Embodiment 2
Embodiment 2 is essentially identical with the step of embodiment 1, and the equipment of employing is identical, and difference is:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is loaded in mixing tank 188 kilograms are reached to waste material weight.Mixing tank is connected with 120 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content Below 0.15%, waste material is sieved, all sieve after 60 minutes and finish, obtain waste material powder body.According to waste material powder body, No. 93 vapour The mass ratio of oil and zinc stearate is 1000:1.5:Both are placed in batch mixer mixing 2h by 0.05, obtain mixed powder.Add every time The quality for entering the mixed powder in compacting tool set is 380g.Direction of adjustment electric current causes magnetic field intensity up to 1.8T for 105A, in pressure Power pushes for 0.6MPa and green compact is obtained.Green compact are carried out into isostatic pressing in 200Mpa, then the vacuum in vacuum sintering furnace Spend to sinter 6 hours in 1060 DEG C under 2Pa, then at 800 DEG C of insulation 3h, being incubated 4h after 450 DEG C carries out Ageing Treatment, obtains neodymium Iron boron magnet.
Embodiment 3
Embodiment 3 is essentially identical with the step of embodiment 1, and the equipment of employing is identical, and difference is:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is loaded in mixing tank 477 kilograms are reached to waste material weight.Mixing tank is connected with 80 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content Below 0.15%, waste material is sieved, all sieve after 150 minutes and finish, obtain waste material powder body.According to waste material powder body, No. 97 The mass ratio of gasoline, zinc stearate and poly(ethylene oxide) allyl glycidyl ether is 1000:1.95:0.05:Three is placed in by 1 Batch mixer mixing 2h, obtains mixed powder.The quality of the mixed powder in addition compacting tool set is 385.5g every time.Direction of adjustment Electric current causes magnetic field intensity up to 1.8T for 105A, pushes for 0.8MPa in pressure and green compact are obtained.Green compact are carried out in 180Mpa Isostatic pressing, then in vacuum sintering furnace, vacuum is to sinter 4 hours in 1090 DEG C under 2Pa, then at 850 DEG C of insulation 4h, 3h is incubated after 400 DEG C carries out Ageing Treatment, obtains neodymium iron boron magnetic body.
Embodiment 4
Embodiment 4 is essentially identical with the step of embodiment 1, and the equipment of employing is identical, and difference is:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is loaded in mixing tank 477 kilograms are reached to waste material weight.Mixing tank is connected with 150 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content Below 0.15%, waste material is sieved, all sieve after 150 minutes and finish, obtain waste material powder body.
The neodymium iron boron magnetic body that comparative example 1 and embodiment 1~4 are obtained is carried out into performance test, various performance parameters number is obtained According to as shown below.Wherein ratio of the squareness for knee point coercivity Hknee and HCJ Hcj, squareness said closer to 1 The anti-demagnetization capability performance of the bright magnet is better.
Each technical characteristic of embodiment described above arbitrarily can be combined, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and Therefore can not be construed as limiting the scope of the patent.It should be pointed out that for one of ordinary skill in the art comes Say, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the protection of the present invention Scope.Therefore, the protection domain of patent of the present invention should be defined by claims.

Claims (10)

1. a kind of method of sintered NdFeB scrap body material reshaping, it is characterised in that comprise the following steps:
Sintered NdFeB scrap body material is crushed to into particle diameter less than 150 mesh in protective gas atmosphere, waste material powder body is obtained;
The waste material powder body is mixed with dispersion solvent, mixed powder is obtained, the matter of the dispersion solvent and the waste material powder body Amount is than less than 0.2%;
The mixed powder is placed in compacting tool set and is suppressed under conditions of alignment magnetic field is not less than 1.7T, given birth to Base, the quality of the mixed powder being added in the compacting tool set neodymium iron boron for needed for Sintered NdFeB magnet to be prepared The 100.5%~102% of powder body Theoretical Mass;
The green compact are carried out into isostatic pressing, then carries out vacuum-sintering process, obtain the Sintered NdFeB magnet.
2. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1, it is characterised in that by the sintering neodymium ferrum The condition that boron scrap body material is crushed is to crush in nitrogen atmosphere and control particle diameter in vibrosieve extremely less than 150 mesh.
3. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1 or 2, it is characterised in that will sintering neodymium ferrum Boron scrap body material is crushed to particle diameter for 80~150 mesh.
4. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1, it is characterised in that also including adding antioxygen The step of agent:The waste material powder body is mixed with the dispersion solvent and the antioxidant, mixed powder is obtained.
5. the method for sintered NdFeB scrap body material reshaping as claimed in claim 4, it is characterised in that the antioxidant is At least one in poly(ethylene oxide) allyl ether and poly(ethylene oxide) allyl glycidyl ether;The antioxidant with it is described The mass ratio of waste material powder body is less than 0.1%.
6. the method for the sintered NdFeB scrap body material reshaping as described in claim 1,4 or 5, it is characterised in that the mixing It is 0.4~0.8MPa that powder body is placed in the pressure suppressed in compacting tool set.
7. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1, it is characterised in that the isostatic pressing Pressure be not less than 150MPa.
8. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1, it is characterised in that at the vacuum-sintering The condition of reason is to be incubated 4~6 hours in 1060~1090 DEG C.
9. the method for sintered NdFeB scrap body material reshaping as claimed in claim 1, it is characterised in that in the vacuum-sintering After process step, also including Ageing Treatment step.
10. the method for sintered NdFeB scrap body material reshaping as claimed in claim 9, it is characterised in that the Ageing Treatment Condition be prior to 800~900 DEG C insulation 2~4h, then at 400~500 DEG C insulation 2~4h.
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CN115215662A (en) * 2021-04-21 2022-10-21 威海华瓷新材料有限责任公司 Raw material formula and preparation method of pressureless sintering silicon carbide granulation powder and waste recovery and powder preparation process

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CN111292911A (en) * 2020-01-13 2020-06-16 桂林电子科技大学 Improved neodymium iron boron magnet material and improvement method thereof
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