CN106601404B - The method of sintered NdFeB scrap body material reshaping - Google Patents

The method of sintered NdFeB scrap body material reshaping Download PDF

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Publication number
CN106601404B
CN106601404B CN201611239448.4A CN201611239448A CN106601404B CN 106601404 B CN106601404 B CN 106601404B CN 201611239448 A CN201611239448 A CN 201611239448A CN 106601404 B CN106601404 B CN 106601404B
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sintered ndfeb
powder
body material
waste material
scrap body
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CN106601404A (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

Abstract

A kind of method of sintered NdFeB scrap body material reshaping, comprising the following steps: sintered NdFeB scrap body material is crushed to partial size no more than 150 mesh in protective gas atmosphere, obtains waste material powder;Waste material powder is mixed with dispersion solvent, obtains mixed powder, dispersion solvent and the mass ratio of waste material powder are no more than 0.2%;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 for being added to the mixed powder in compacting tool set is 100.5%~102% of neodymium iron boron powder Theoretical Mass needed for Sintered NdFeB magnet to be prepared;Green compact are subjected to isostatic pressing, then carry out vacuum-sintering processing, obtain Sintered NdFeB magnet.This method simple process, it is low for equipment requirements, and to the utilization rate of sintered NdFeB scrap body material height, it is at low cost.Obtained neodymium iron boron magnetic body, section crystal grain phenomenon without exception of growing up, and it can reach using standard on the magnetic properties such as coercivity, maximum magnetic energy product in remanent magnetism, interior grasp.

Description

The method of sintered NdFeB scrap body material reshaping
Technical field
The present invention relates to neodymium iron boron magnetic body technical fields, more particularly to a kind of side of sintered NdFeB scrap body material reshaping Method.
Background technique
At present the preparation flow of Sintered NdFeB magnet be generally broken melting, hydrogen, powder processed, compression moulding, etc. static pressure, reburn Knot.Compression moulding is committed step therein, and molding is by manufactured pressed by powder into green compact.And due to powder granularity, equipment, The influence of the factors such as operator and technological parameter, the green compact that compression moulding obtains can generate cracking, concentric reducer, fall lid, chipping Or the rejected products such as off-dimension.The waste material obtained due to compression moulding is without equal static pressure and sintering processes, generally by it Collection recycles after treatment.
The recycling research for forming obtained waste material experienced three developing stage.First stage is to aoxidize waste material, Rare earth metal therein is recycled with Wet-process metallurgy method again, however this method process flow is long, the rate of recovery is low, cost recovery It is high.Second stage is waste material to be sintered directly into blank, then melt down melting, is formed after the broken powder processed of hydrogen, neodymium-iron-boron is made in sintering Body;Although this method process flow is shortened, utilization rate increases, however its quality is not easy to control, and processing cost is still higher. Phase III is by waste material categorised collection and to be broken into 40 mesh powder below, is mixed using airflow milling powder, then with regular burden(ing), Neodymium iron boron magnetic body is made in molding, sintering.However this method airflow milling dispersing technology requires strictly, to be limited only to similar waste material simultaneously Processing, the bad powder of granularity consistency are added airflow milling and charging Hatch Opening are easy to cause to block, this to operation bring difficulty and Security risk also affects the utilization rate of equipment;Also lead to the long property for influencing waste material and recycling of certain waste material resting periods simultaneously Energy.In addition, handling a part of powder using airflow milling unavoidably becomes superfine powder, and then influence the utilization rate of powder.
Summary of the invention
Based on this, it is necessary to provide a kind of simple process, low for equipment requirements, utilization rate is high and obtained neodymium iron boron magnetic body The method of the good sintered NdFeB scrap body material reshaping of performance.
A kind of method of sintered NdFeB scrap body material reshaping, comprising the following steps:
Sintered NdFeB scrap body material is crushed to partial size no more than 150 mesh in protective gas atmosphere, obtains waste material powder;
The waste material powder is mixed with dispersion solvent, obtains mixed powder, the dispersion solvent and the waste material powder Mass ratio be no more 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, is obtained Green compact, the quality for being added to the mixed powder in the compacting tool set is neodymium iron needed for Sintered NdFeB magnet to be prepared The 100.5%~102% of boron powder Theoretical Mass;
The green compact are subjected to isostatic pressing, then carry out vacuum-sintering processing, obtain the Sintered NdFeB magnet.
The method of above-mentioned sintered NdFeB scrap body material reshaping, simple process is low for equipment requirements, and to sintering neodymium iron The utilization rate of boron scrap body material is high, at low cost.This method uses sintered NdFeB scrap body material, by tentatively crushing control waste material powder Partial size, add dispersion solvent and control the mixed powder in compacting tool set amount suppressed, etc. static pressure, sintering processes, So that sintered NdFeB scrap body material reshaping, and obtain neodymium iron boron magnetic body.Obtained neodymium iron boron magnetic body, section crystal grain are no different Often grow up phenomenon, and its in remanent magnetism, interior grasp coercivity, maximum magnetic energy product equimagnetic performance indicator and can reach using normal neodymium iron boron Powder prepares the performance of neodymium iron boron magnetic body.The method of the sintered NdFeB scrap body material reshaping is returned to sintered NdFeB scrap body material It receives to recycle and provides good approach, there is huge practical value.
The condition that the sintered NdFeB scrap body material is crushed in one of the embodiments, is to crush simultaneously in nitrogen atmosphere In controlling partial size on vibrating screen to being no more than 150 mesh.
It is 80~150 mesh that sintered NdFeB scrap body material, which is crushed to partial size, in one of the embodiments,.
Further include the steps that antioxidant is added in one of the embodiments: by the waste material powder and the dispersion Solvent and antioxidant mixing, obtain mixed powder.
The antioxidant is polyethylene oxide allyl ether and polyethylene oxide allyl in one of the embodiments, At least one of glycidol ether;The mass ratio of the antioxidant and the waste material powder is no more than 0.1%.
It is 0.4~0.8MPa that the mixed powder, which is placed in the pressure suppressed in compacting tool set, in one of the embodiments,.
The pressure of the isostatic pressing is not less than 150MPa in one of the embodiments,.
The condition of the vacuum-sintering processing is small in 1060~1090 DEG C of heat preservations 4~6 in one of the embodiments, When.
It further include ageing treatment step in one of the embodiments, after the vacuum-sintering processing step.
The condition of the ageing treatment is prior to 800~900 DEG C 2~4h of heat preservation in one of the embodiments, then at 400~500 DEG C of 2~4h of heat preservation.
Detailed description of the invention
Fig. 1 is the flow chart of the method for the sintered NdFeB scrap body material reshaping of an embodiment.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein Described embodiment.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more saturating It is thorough comprehensive.
Referring to Fig. 1, the method for the sintered NdFeB scrap body material reshaping of one embodiment of the invention, includes the following steps.
Step S1: sintered NdFeB scrap body material is crushed to partial size no more than 150 mesh in protective gas atmosphere, is given up Feed powder body.
Step S1 crushes sintered NdFeB scrap body material in protective gas atmosphere, in order to avoid sintered NdFeB scrap body material oxygen Change.Sintered NdFeB scrap body material is crushed to no more than 150 mesh, partial size is avoided to cause neodymium iron boron magnetic body is non-uniform to ask greatly very much Topic, and realize that the Particle size requirements without special installations such as airflow millings, can be realized, therefore neodymium is sintered in S1 using manual type Iron boron scrap body material can be converted into waste material powder, so the utilization rate to sintered NdFeB scrap body material is high.
Specifically, sintered NdFeB scrap body material should carry out pulverization process in time, resting period length is avoided to cause to be sintered neodymium iron Boron scrap body material particle bonding, which is reunited, to be difficult to disperse.Preferably, from obtain sintered NdFeB scrap body material between being crushed when Between interval be no more than 20h;It is furthermore preferred that the time interval is no more than 8h.
It preferably, is to be crushed in nitrogen atmosphere and in controlling grain on vibrating screen by condition that sintered NdFeB scrap body material crushes Diameter is to being no more than 150 mesh.The dispersion that so can further promote waste material powder using the vibrational energy of vibrating screen, obtains dispersibility Preferable waste material powder.Specifically, sintered NdFeB scrap body material carries out in glove box the step of crushing, and used in glove box Nitrogen atmosphere, the oxygen quality content controlled in glove box are no more than 0.1%.
Specifically, the step of " crushing sintered NdFeB scrap body material in protective gas atmosphere ", on vibrating screen to " in controlling Granulation diameter is to being no more than 150 mesh " the step of both time interval be no more than 72h, in order to avoid serious group occurs for smashed powder It is poly-.
Preferably, sintered NdFeB scrap body material is crushed to partial size is 80~150 mesh.Obtain the waste powder of the particle size range Body can not only meet the needs of subsequent compacting, but also without special installations such as airflow millings, and the utilization rate of waste material powder is high.
Step S2: waste material powder is mixed with dispersion solvent, obtains mixed powder, the quality of dispersion solvent and waste material powder Than being no more than 0.2%.
Step S2 disperses waste material powder in dispersion solvent, obtains mixed powder, on the one hand can effectively prevent waste powder Body is reunited, and on the other hand be can avoid waste material powder and is excessively dispersed that it is caused suppress in step S3 and can not form, dispersion solvent It also acts as and reduces the intracorporal frictional force of waste powder, improve the magnet degree of orientation, be allowed to adapt to the needs of subsequent step moulding process.Point The quality for dissipating solvent cannot be excessively high, and otherwise mobility is too strong, also will affect subsequent forming.
Preferably, dispersion solvent is the mixture of solvent naphtha and lubricant.Specifically, solvent naphtha can be No. 93 gasoline, 97 At least one of number gasoline and No. 120 industrial napthas.Specifically, lubricant is zinc stearate.The matter of lubricant and solvent naphtha Amount is than being no more than 1:20.
Step S2 further includes the steps that antioxidant is added in one of the embodiments: waste material powder and dispersion is molten Agent and antioxidant mixing, obtain mixed powder.It is to avoid waste material powder from being oxidized, and be added that antioxidant is added in step S2 Dispersion solvent can also increase the dissolution of antioxidant.Preferably, the mass ratio of antioxidant and waste material powder is no more than 0.1%. It is furthermore preferred that antioxidant is at least one in polyethylene oxide allyl ether and polyethylene oxide allyl glycidyl ether Kind.
The time that wherein waste material powder is mixed with gasoline, antioxidant is different according to the quality of mixed powder;Generally , the mixed powder incorporation time that the time that waste material powder is mixed with gasoline, antioxidant is 300Kg is not less than 2h.
Step S3: mixed powder being 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 for being added to the mixed powder in compacting tool set is Nd-Fe-B powder 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 the size selection of neodymium iron boron magnetic body to be prepared, have Once square, cylinder etc., commonly referred to as mold direction, differently- oriented directivity and pressing direction size, mold mold direction and take selected Relatively fixed to direction size, variable is pressing direction.Compacting height throws powder amount and pressing pressure difference with single mode.Single mode is thrown Powder amount theoretical value can be calculated according to the theoretical size and magnet density of neodymium iron boron magnetic body to be prepared.
Wherein, neodymium iron boron powder Theoretical Mass needed for Sintered NdFeB magnet to be prepared is volume and the neodymium that needs obtain The quality of the corresponding neodymium iron boron powder of the size of iron boron magnet can be calculated by the density and theoretical size of neodymium iron boron powder It arrives.
The compression ratio of waste material powder and neodymium iron boron powder that the present invention is obtained by research discovery sintered NdFeB scrap body material The compression ratio of property that there is some difference, the waste material powder that sintered NdFeB scrap body material of the present invention obtains is bigger, therefore walks in compacting Rapid increase mixed powder appropriate is added to the amount in compacting tool set, so that subsequent step S4 obtains closely knit neodymium-iron-boron Body.
Preferably, it is 0.4~0.8MPa that mixed powder, which is placed in the pressure suppressed in compacting tool set,.
Alignment magnetic field is not less than 1.7T in step S3, to guarantee 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 strength, It can guarantee the degree of orientation of neodymium iron boron magnetic body.Specifically, the orientation electric current control that alignment magnetic field is applied by control in step S3 System.
Step S4: green compact are subjected to isostatic pressing, then carry out vacuum-sintering processing, obtain Sintered NdFeB magnet.
Obtained green compact are suppressed merely through the pressure of vertical direction, and the pressure being subject to comes solely from certain orientation, so The uniformity of green compact is bad, and the pressure suppressed is smaller, and it is inadequate to obtain green compact compactness;Therefore by green compact carry out equal static pressure at Type makes its all directions be guaranteed the neodymium-iron-boron obtained after sintering by uniform pressure to guarantee its uniformity and compactness External shape meets the requirements, and geometric tolerance reaches requirement, and improves the magnetic properties such as remanent magnetism, maximum magnetic energy product in turn.
Preferably, the pressure of isostatic pressing is not less than 150MPa.
Preferably, the condition of vacuum-sintering processing is to keep the temperature 4~6 hours in 1060~1090 DEG C.Preferably, vacuum-sintering The vacuum degree of processing is no more than 2Pa.
It further include ageing treatment step in one of the embodiments, after vacuum-sintering processing step.After sintering into 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 2~4h of heat preservation, then at 400~500 DEG C keep the temperature 2~ 4h。
The method of above-mentioned sintered NdFeB scrap body material reshaping, simple process is low for equipment requirements, and to sintering neodymium iron The utilization rate of boron scrap body material is high, at low cost.This method uses sintered NdFeB scrap body material, by tentatively crushing control waste material powder Partial size, add dispersion solvent and control the mixed powder in compacting tool set amount suppressed, etc. static pressure, sintering processes, So that sintered NdFeB scrap body material reshaping, and obtain neodymium iron boron magnetic body.Obtained neodymium iron boron magnetic body, section crystal grain are no different Often grow up phenomenon, and its remanent magnetism, it is interior grasp coercivity, maximum magnetic energy product and in terms of performance on can reach using neodymium Iron boron powder prepares the performance of neodymium iron boron magnetic body.
The method of the sintered NdFeB scrap body material reshaping provides very to the recycling and reusing of sintered NdFeB scrap body material Good approach has huge practical value.
The following are specific embodiments.
Comparative example 1
It is mixed by level-one by raw material neodymium iron boron (the 45SH neodymium iron boron rejection tablet of Hunan Research Institute of Rare Earth Metal Materials) after hydrogen is broken Material obtains powder in airflow milling powder.By powder, 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 rectangular compacting tool set.The quality that the mixed powder in compacting tool set is added is 378g, The size of compacting tool set is 60.5mm*57.5mm*28.4mm.(density of neodymium iron boron powder is with 7.55g/cm3It calculates, No. 120 molten The quality of agent gasoline and antioxidant is negligible).Direction of adjustment electric current is that 100A makes magnetic field strength up to 1.6T, in pressure Green compact are made for 2MPa pushing.
Green compact are subjected to isostatic pressing in 150Mpa, then vacuum degree is under 2Pa in 1080 DEG C in vacuum sintering furnace Sintering 5 hours, then at 900 DEG C of heat preservation 2h, after in 500 DEG C of heat preservation 2h progress ageing treatments, obtain neodymium iron boron magnetic body.
Embodiment 1
Using what is generated in pressing process in the preparation method of comparative example 1 will the unqualified life such as lid, cracking, dimension overproof Base is as sintered NdFeB scrap body material raw material.The unqualified green compact are vacuumized into sealing with packaging bag, are carried out using manual type It breaks into pieces.The waste material broken into pieces is put into the glove box of nitrogen atmosphere, control glove box in oxygen quality content be down to 0.05% with It when lower, opens the package, the waste material broken into pieces is fitted into mixing tank to waste material weight and reaches 308 kilograms.By mixing tank and 100 mesh Vibrating scalper connection, nitrogen charging gas shielded, the control of oxygen quality content is 0.15% hereinafter, waste material is sieved, after 78 minutes all Sieving finishes, and obtains waste material powder.
In mass ratio it is 1000 by waste material powder, No. 120 industrial napthas, zinc stearate and polyethylene oxide allyl ether: 1:0.05:0.2 is placed in batch mixer mixing 2h, obtains mixed powder.
Mixed powder is put into rectangular compacting tool set identical with comparative example 1, is added every time mixed in compacting tool set The quality for closing powder is 381.5g.Direction of adjustment electric current is that 102A makes magnetic field strength up to 1.7T, is 0.4MPa pushing in pressure Green compact are made.
Green compact are subjected to isostatic pressing and are controlled at compact dimensions, vacuum-sintering processing and timeliness by isostatic tooling The step of reason, is identical as comparative example 1, obtains neodymium iron boron magnetic body.
Embodiment 2
The step of embodiment 2 is with embodiment 1 is essentially identical, and the equipment of use is identical, the difference is that:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is fitted into mixing tank Reach 188 kilograms to waste material weight.Mixing tank is connect with 120 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content 0.15% hereinafter, waste material is sieved, all sieving is finished after sixty minutes, obtains waste material powder.According to waste material powder, No. 93 vapour The two is placed in batch mixer mixing 2h for 1000:1.5:0.05 by the mass ratio of oil and zinc stearate, obtains mixed powder.Add every time The quality for entering the mixed powder in compacting tool set is 380g.Direction of adjustment electric current is that 105A makes magnetic field strength up to 1.8T, is being pressed Power is that green compact are made in 0.6MPa pushing.Green compact are subjected to isostatic pressing in 200Mpa, then the vacuum in vacuum sintering furnace Degree is to be sintered 6 hours under 2Pa in 1060 DEG C, then at 800 DEG C of heat preservation 3h, after in 450 DEG C of heat preservation 4h progress ageing treatments, obtain neodymium Iron boron magnet.
Embodiment 3
The step of embodiment 3 is with embodiment 1 is essentially identical, and the equipment of use is identical, the difference is that:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is fitted into mixing tank Reach 477 kilograms to waste material weight.Mixing tank is connect with 80 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content 0.15% hereinafter, waste material is sieved, all sieving is finished after 150 minutes, obtains waste material powder.According to waste material powder, No. 97 The mass ratio of gasoline, zinc stearate and polyethylene oxide allyl glycidyl ether is that three is placed in by 1000:1.95:0.05:1 Batch mixer mixing 2h, obtains mixed powder.The quality for the mixed powder being added in compacting tool set every time is 385.5g.Direction of adjustment Electric current is that 105A makes magnetic field strength up to 1.8T, is that green compact are made in 0.8MPa pushing in pressure.Green compact are carried out in 180Mpa Isostatic pressing, then vacuum degree is to be sintered 4 hours under 2Pa in 1090 DEG C in vacuum sintering furnace, then at 850 DEG C of heat preservation 4h, Ageing treatment is carried out in 400 DEG C of heat preservation 3h afterwards, obtains neodymium iron boron magnetic body.
Embodiment 4
The step of embodiment 4 is with embodiment 1 is essentially identical, and the equipment of use is identical, the difference is that:
Oxygen quality content in glove box is down to 0.10%, opens the package, and the waste material broken into pieces is fitted into mixing tank Reach 477 kilograms to waste material weight.Mixing tank is connect with 150 mesh vibrating scalpers, nitrogen charging gas shielded, the control of oxygen quality content 0.15% hereinafter, waste material is sieved, all sieving is finished after 150 minutes, obtains waste material powder.
The neodymium iron boron magnetic body that comparative example 1 and Examples 1 to 4 obtain is tested for the property, various performance parameters number is obtained According to as shown below.Wherein squareness is the ratio between knee point coercivity Hknee and intrinsic coercivity Hcj, and squareness is said closer to 1 The anti-demagnetization capability performance of the bright magnet is better.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies 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, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (9)

1. a kind of method of sintered NdFeB scrap body material reshaping, which comprises the following steps:
The condition that the sintered NdFeB scrap body material is crushed is to crush in nitrogen atmosphere and in control partial size on vibrating screen to not More than 150 mesh, waste material powder is obtained;It is described by sintered NdFeB scrap body material in nitrogen atmosphere crush the step of and be set forth in vibration The time interval for controlling partial size to both steps for being no more than 150 mesh on sieve is no more than 72h;
The waste material powder is mixed with dispersion solvent, obtains mixed powder, the matter of the dispersion solvent and the waste material powder Amount is than being no more than 0.2%;The dispersion solvent is the mixture of solvent naphtha and lubricant, and the lubricant is zinc stearate;
The mixed powder is placed in compacting tool set and is suppressed under conditions of alignment magnetic field is not less than 1.7T, is given birth to Base, the quality for being added to the mixed powder in the compacting tool set is neodymium iron boron needed for Sintered NdFeB magnet to be prepared The 100.5%~102% of powder Theoretical Mass;
The green compact are subjected to isostatic pressing, then carry out vacuum-sintering processing, obtain the Sintered NdFeB magnet.
2. the method for sintered NdFeB scrap body material reshaping as described in claim 1, which is characterized in that sintered NdFeB gives up It is 80~150 mesh that blank, which is crushed to partial size,.
3. the method for sintered NdFeB scrap body material reshaping as described in claim 1, which is characterized in that further include that antioxygen is added The step of agent: the waste material powder is mixed with the dispersion solvent and the antioxidant, obtains mixed powder.
4. the method for sintered NdFeB scrap body material reshaping as claimed in claim 3, which is characterized in that the antioxidant is At least one of polyethylene oxide allyl ether and polyethylene oxide allyl glycidyl ether;The antioxidant with it is described The mass ratio of waste material powder is no more than 0.1%.
5. the method for the sintered NdFeB scrap body material reshaping as described in Claims 1 to 4 is any, which is characterized in that described mixed Closing powder and being placed in the pressure suppressed in compacting tool set is 0.4~0.8MPa.
6. the method for sintered NdFeB scrap body material reshaping as described in claim 1, which is characterized in that the isostatic pressing Pressure be not less than 150MPa.
7. the method for sintered NdFeB scrap body material reshaping as described in claim 1, which is characterized in that at the vacuum-sintering The condition of reason is to keep the temperature 4~6 hours in 1060~1090 DEG C.
8. the method for sintered NdFeB scrap body material reshaping as described in claim 1, which is characterized in that in the vacuum-sintering It further include ageing treatment step after processing step.
9. the method for sintered NdFeB scrap body material reshaping as claimed in claim 8, which is characterized in that the ageing treatment Condition is prior to 800~900 DEG C 2~4h of heat preservation, then at 400~500 DEG C of 2~4h of heat preservation.
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