CN109935463A - A method of reducing rare-earth Nd-Fe-B oxygen content - Google Patents

A method of reducing rare-earth Nd-Fe-B oxygen content Download PDF

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CN109935463A
CN109935463A CN201910205578.3A CN201910205578A CN109935463A CN 109935463 A CN109935463 A CN 109935463A CN 201910205578 A CN201910205578 A CN 201910205578A CN 109935463 A CN109935463 A CN 109935463A
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slab
oxygen content
earth
furnace
hydrogen
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CN109935463B (en
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黎龙贵
张燕
李超
胡烈平
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Zhejiang Dongyang Dmegc Rare Earth Co ltd
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Zhejiang Dongyang Dmegc Rare Earth Co ltd
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Abstract

The present invention relates to permanent-magnet material fields, disclose a kind of method for reducing rare-earth Nd-Fe-B oxygen content, S1: weighing each raw material of neodymium iron boron and additional oxytropism is higher than the additive of iron;Resulting material is placed in vacuum rapid hardening furnace and is vacuumized;S2: preheating material, excludes steam;S3: after preheating, to material heating melting;S4: removal floats on the oxide of bath surface, casts;Slab cooling is come out of the stove;S5: slab is subjected to hydrogen breaking;S6: material is subjected to airflow milling powder;S7: after being formed, being sintered to powder, neodymium iron boron magnetic body is made.The present invention reduces the content of oxygen in neodymium iron boron by adding alloy type additive in neodymium iron boron raw material, and this method can be effectively reduced the usage amount of heavy rare earth element, provides the foundation for production low-cost high-performance rare-earth neodymium iron boron magnetic body.

Description

A method of reducing rare-earth Nd-Fe-B oxygen content
Technical field
The present invention relates to permanent-magnet material field more particularly to a kind of methods for reducing rare-earth Nd-Fe-B oxygen content.
Background technique
Sintered NdFeB magnet is the strongest permanent-magnet material of comprehensive magnetic energy in the world today, is surmounted with it in traditional permanent magnetism The excellent characteristics and cost performance of material, are widely used in the fields such as the energy, traffic, machinery, medical treatment, computer, household electrical appliances, in state It plays an important role in people's economy.
In the technical indicator of magnetic material, magnetic energy product is mostly important.The magnet of magnetic energy product representation unit volume generates outer magnetic The energy size of field.Magnetic energy product is high, it is meant that can export bigger power on motor with lesser magnet.Neodymium iron boron is a kind of Important rare earth permanent-magnetic material has the characteristics such as high energy product, high-coercive force, light weight and cost be low, is cost performance so far Highest magnet obtains reputation " magnetic king ".The appearance of neodymium iron boron develops magnetic device to efficient, miniaturization, lightness direction.
In the prior art, heavy rare earth element Dy, Tb, Ho are mainly used in order to obtain high performance sintered neodymium-iron-boron, and its The compound addition of its nonmetalloid, but heavy rare earth element Dy, Tb, Ho higher cost, more severe, heavy rare earth element has been visited Bright reserves are very limited.With present depletion rate, in the near future, people will face the rare predicament of heavy rare earth element. Therefore, exploitation does not have to or is that strategy needs less with low high performance sintered neodymium-iron-boron technologies of preparing of heavy rare earth such as Dy, Tb, Ho. However influence of the oxygen content height to magnetic property in actual production in neodymium-iron-boron body is very big.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of method for reducing rare-earth Nd-Fe-B oxygen content, this hairs Bright to reduce the content of oxygen in neodymium iron boron by adding alloy type additive in neodymium iron boron raw material, this method can be effectively reduced The usage amount of heavy rare earth element provides the foundation for production low-cost high-performance rare-earth neodymium iron boron magnetic body.
The specific technical proposal of the invention is: a kind of method for reducing rare-earth Nd-Fe-B oxygen content, comprising the following steps:
S1: weighing each raw material of neodymium iron boron and additional oxytropism is higher than the additive of iron;The additive amount of the additive is total The 0.02-0.2wt% of amount;Resulting material is placed in the crucible of vacuum rapid hardening furnace, by vacuum rapid hardening stove evacuation.
S2: preheating material, excludes the steam of material.
S3: after preheating, further heating material, and temperature is made to reach 1400-1500 DEG C.
S4: removal floats on the oxide of bath surface obtained by S4, casts, obtains slab;By slab in inert gas Atmosphere cooling is come out of the stove.
S5: slab obtained by S4 is subjected to hydrogen breaking.
S6: the material after hydrogen breaking is subjected to airflow milling powder.
S7: after powder obtained by S6 is formed, is sintered, neodymium iron boron magnetic body is made.
The present invention directly adds the element that the affinity with oxygen is better than iron in neodymium iron boron in the form of ferroalloy or metal block etc. Into ingredient, the density for generating Precipitation the object MxOy, general MxOy insoluble in molten steel with oxygen in melting is less than molten steel Density, and can on excluded when floating on casting.Neodymium iron boron prepared by the present invention its simple process reduces oxygen in slab and contains Amount, which improves magnet magnetic property and reduces the dosage of heavy rare earth, reduces material cost.
Preferably, in S1, the additive is silicomangan, ferrosilicon, manganese iron, ferro-aluminum, at least one in Si-Al-Ba-Ca Kind.
In the present invention, the oxytropism of above-mentioned additive is higher than iron, therefore can capture oxygen in each raw material after melting The oxygen of compound due to smaller than other elements specific gravity than important, can float, only need at this time after additive forms oxide Supernatant is removed, that is, can effectively reduce the oxygen content in raw material.
In addition, it should be noted that, the content of additive needs strict control in the method for the present invention, it is necessary to add in the present invention Preferable technical effect can be realized under dosage.If addition is excessive, neodymium iron boron comprehensive magnetic can be declined obviously;It adds very few Then deoxidation effect is unobvious, and it is unobvious to reduce amplitude for oxygen content in slab.
Preferably, in S1, each raw material of neodymium iron boron are as follows: RaFe100-a-b-cBbMc;Mass percent be 35% >=a >= 20%, 1.2% >=b >=0.9%, 6% >=c >=0%, one of R Nd, Pr, Dy, Tb, Gd and Ho or a variety of;M be Co, One of Ga, Al, Cu, Nb, Zr and Mn or a variety of.
Preferably, adding materials from high to low by fusing point in S1, being evacuated to≤8Pa.
The sequence of strict control adding raw materials is needed in fusing, the present invention adds materials from high to low by fusing point, reason Be: in fusion process dystectic raw material can preferential contact molten steel carry out fusing reduce high-melting-point raw material incomplete fusion it is thorough Risk, if the preferential contact molten steel of low melting point such as light rare earth PrNd will cause low-melting-point metal scaling loss and seriously affect final magnetic Performance.
Preferably, in S2, warm-up power 120-200kW.
Preferably, in S3, heating power 350-550kW, heating time 7-15min.
Preferably, casting under the copper roller revolving speed of 35-45r/min in S4, gained slab average thickness is 0.2- 0.4mm。
Preferably, the de- property gas is argon gas in S4, cooling 120-150min.
Preferably, in S5, hydrogen breaking specifically comprises the processes of: slab is put into hydrogen breaking furnace be evacuated to≤ 10Pa is filled with hydrogen into furnace and carries out hydrogen abstraction reaction, and the suction hydrogen time is 60-210min, vacuumizes and is heated to again after inhaling hydrogen 500-600 DEG C of progress dehydrogenation, dehydrogenation time 240-420min, after dehydrogenation open furnace to furnace body carry out spraying cooling to≤ It 60 DEG C, comes out of the stove to obtain neodymium iron boron fine powder.
Preferably, in S7, molding, sintering specifically comprises the processes of: by the powder Jing Guo airflow milling be placed into magnetic field >= It is formed in the press of 1.4T, green compact after molding, which are placed into sintering furnace, is evacuated to 5.0 × 10-1Pa or less is by liter temperature 5-10 DEG C/min is warming up to 350-450 DEG C, and heat preservation 40-80min carries out dumping and goes out to handle;3-5 DEG C of heating rate/min liter is pressed again Temperature keeps the temperature 120-240min to 850-950 DEG C, is finally warming up to 1060-1080 DEG C by 2-4 DEG C/min of heating rate, heat preservation 240-360min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnetic Body is warming up to 880 DEG C of -920 DEG C of heat preservation 90min-180min by 5-8 DEG C/min of heating rate, then air-cooled to 150 DEG C accomplished below It is air-cooled to 60 to be warming up to 450 DEG C of -550 DEG C of heat preservation 180min-300min by 5-8 DEG C/min of heating rate for first segment ageing treatment DEG C or less come out of the stove and complete second segment ageing treatment.
The broken vacuum of hydrogen is evacuated to≤and 10Pa is mainly for guaranteeing that the vacuum degree in furnace prevents powder oxygen during inhaling hydrogen from containing Measure it is excessively high lead to magnetic decline, inhaling hydrogen time 60-210min is to guarantee that powder is effectively crushed, and 500-600 DEG C is de- Hydrogen temperature is too low to be easy to cause dehydrogenation to be not thorough, and temperature, which is crossed to powder, can occur disproportionated reaction influence magnet performance, dehydrogenation time For 240-420min also for guaranteeing that powder dehydrogenation is thorough, cooling temperature≤60 DEG C are the excessively high shadows of powder tapping temperature in order to prevent Ring powder oxygen content.
It is sintered vacuum degree 5.0 × 10-1Pa or less is the 5-10 DEG C/min liter in order to guarantee that vacuum degree prevents green compact from aoxidizing in furnace Temperature is rapidly heated to 350-450 DEG C of heat preservation 40-80min and foreign gas in magnet and glue is discharged, by 3-5 DEG C/min of heating rate Being warming up to 850-950 DEG C of heat preservation 120-240min and slowly heating up prevents excessive temperature differentials from causing product crack while to remain in magnet Hydrogen be discharged, be finally warming up to 1060-1080 DEG C of heat preservation also for preventing from heating up by 2-4 DEG C/min of heating rate Cause product crack fastly, heat preservation be for magnet densification,;First segment timeliness and second segment timeliness can be in fast lifting magnets Report coercivity.
It is compared with the prior art, the beneficial effects of the present invention are: the present invention in neodymium iron boron raw material by adding alloy type Additive reduces the content of oxygen in neodymium iron boron, and this method can be effectively reduced the usage amount of heavy rare earth element, for produce it is low at This high-performance rare-earth neodymium iron boron magnetic body provides the foundation.The oxygen content of the final gained neodymium iron boron slab of the present invention, which is can be controlled in, to be lower than The level of 121ppm, achieves significant progress compared with prior art.
Specific embodiment
The present invention will be further described with reference to the examples below.
Total embodiment
A method of reducing rare-earth Nd-Fe-B oxygen content, comprising the following steps:
S1: weighing each raw material of neodymium iron boron and additional oxytropism is higher than the additive of iron;The additive amount of the additive is total The 0.02-0.2wt% of amount;Resulting material is placed in the crucible of vacuum rapid hardening furnace from high to low by fusing point, by vacuum rapid hardening Stove evacuation is to≤8P.
S2: material preheat at 120-200kW, the steam of material is excluded.
S3: after preheating, further heating 7-15min at 350-550kW to material, and temperature is made to reach 1400- 1500℃。
S4: removal floats on the oxide of bath surface obtained by S4, casts, obtains under the copper roller revolving speed of 35-45r/min To slab (average thickness 0.2-0.4mm);Slab is come out of the stove in the cooling 120-150min of inert gas (preferably argon gas) atmosphere.
S5: slab obtained by S4 is subjected to hydrogen breaking.
S6: the material after hydrogen breaking is subjected to airflow milling powder.
S7: after powder obtained by S6 is formed, is sintered, neodymium iron boron magnetic body is made.
Preferably, in S1, the additive is silicomangan, ferrosilicon, manganese iron, ferro-aluminum, at least one in Si-Al-Ba-Ca Kind.
Preferably, in S1, each raw material of neodymium iron boron are as follows: RaFe100-a-b-cBbMc;Mass percent be 35% >=a >= 20%, 1.2% >=b >=0.9%, 6% >=c >=0%, one of R Nd, Pr, Dy, Tb, Gd and Ho or a variety of;M be Co, One of Ga, Al, Cu, Nb, Zr and Mn or a variety of.
Preferably, in S5, hydrogen breaking specifically comprises the processes of: slab is put into hydrogen breaking furnace be evacuated to≤ 10Pa is filled with hydrogen into furnace and carries out hydrogen abstraction reaction, and the suction hydrogen time is 60-210min, vacuumizes and is heated to again after inhaling hydrogen 500-600 DEG C of progress dehydrogenation, dehydrogenation time 240-420min, after dehydrogenation open furnace to furnace body carry out spraying cooling to≤ It 60 DEG C, comes out of the stove to obtain neodymium iron boron fine powder.
Preferably, in S7, molding, sintering specifically comprises the processes of: by the powder Jing Guo airflow milling be placed into magnetic field >= It is formed in the press of 1.4T, green compact after molding, which are placed into sintering furnace, is evacuated to 5.0 × 10-1Pa or less is by liter temperature 5-10 DEG C/min is warming up to 350-450 DEG C, and heat preservation 40-80min carries out dumping and goes out to handle;3-5 DEG C of heating rate/min liter is pressed again Temperature keeps the temperature 120-240min to 850-950 DEG C, is finally warming up to 1060-1080 DEG C by 2-4 DEG C/min of heating rate, heat preservation 240-360min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnetic Body is warming up to 880 DEG C of -920 DEG C of heat preservation 90min-180min by 5-8 DEG C/min of heating rate, then air-cooled to 150 DEG C accomplished below It is air-cooled to 60 to be warming up to 450 DEG C of -550 DEG C of heat preservation 180min-300min by 5-8 DEG C/min of heating rate for first segment ageing treatment DEG C or less come out of the stove and complete second segment ageing treatment.
Embodiment 1
(Nd, Pr) according to the ratio28.8Dy0.8Gd1Co1.5Cu0.2Al1Nb0.4B more than Fe0.97(wt%) it carries out ingredient and adds in mass ratio 0.1% manganese iron is denoted as A as additive;Do not add it is additivated be denoted as B, by A, B rare-earth Nd-Fe-B material by fusing point by up to Low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, by heating power setting to 150kW Carry out preheating and guarantee that steam etc. of raw material excludes, being by power setting after preheating is 12 minutes the 520kW time, then into Row thermometric temperature is 1460 DEG C, and copper roller revolving speed is set as 40r/min and casts, and slab average thickness is 0.28mm, by slab It came out of the stove at argon atmosphere cooling 120 minutes;A, B slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, hydrogen is filled with into furnace Gas carries out hydrogen abstraction reaction, and the suctions hydrogen time is 150min, vacuumizes be heated to 550 DEG C of progress dehydrogenations again after suction hydrogen, when dehydrogenation Between be 380min, heating furnace is opened after dehydrogenation, spraying cooling is carried out to furnace body, cooling≤40 DEG C of temperature are come out of the stove to obtain neodymium iron Boron fine powder.After airflow milling, fine powder A milling particle size consistent with fine powder B milling particle size is all 3.05-3.15um.A, B powder exists The square blank of compression moulding 55 × 40 × 31 (mm), blank is placed into sintering furnace and is vacuumized in the alignment magnetic field of >=1.6T To 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;Again by heating speed 3 DEG C/min of degree is warming up to 900 DEG C, keeps the temperature 180min, is finally warming up to 1060 DEG C by 2 DEG C/min of heating rate, keeps the temperature 330min Progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet is by heating speed 6 DEG C/min of degree is warming up to 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by heating rate 6 DEG C/min is warming up to 500 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, and sintering magnetic is made Body.It takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 1
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
A 120 12.58 20.85 38.12
B 189 12.63 20.13 38.53
The oxygen content in slab A is well below the oxygen content in slab B from the results shown in Table 1, while magnetic property slab A The magnet HcJ of production is higher than the magnet of slab B production.
Embodiment 2
(Nd, Pr) according to the ratio28.8Dy1.5Co1.5Cu0.15Al0.35Nb0.3B more than Fe0.96(wt%) it carries out ingredient and adds in mass ratio 0.15% ferrosilicon is denoted as C as additive;Do not add it is additivated be denoted as D, by C, D rare-earth Nd-Fe-B material by fusing point by up to Low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, by heating power setting to 170kW Carry out preheating and guarantee that steam etc. of raw material excludes, being by power setting after preheating is 13 minutes the 500kW time, then into Row thermometric temperature is 1450 DEG C, and copper roller revolving speed is set as 38r/min and casts, and slab average thickness is 0.29mm, by slab It came out of the stove at argon atmosphere cooling 120 minutes;C, D slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, hydrogen is filled with into furnace Gas carries out hydrogen abstraction reaction, and the suctions hydrogen time is 150min, vacuumizes be heated to 550 DEG C of progress dehydrogenations again after suction hydrogen, when dehydrogenation Between be 380min, heating furnace is opened after dehydrogenation, spraying cooling is carried out to furnace body, cooling≤40 DEG C of temperature are come out of the stove to obtain neodymium iron Boron fine powder.After airflow milling, fine powder C milling particle size consistent with fine powder D milling particle size is all 3.00-3.10um.C, D powder exists The square blank of compression moulding 60 × 45 × 32 (mm), blank is placed into sintering furnace and is vacuumized in the alignment magnetic field of >=1.6T To 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;Again by heating speed 4 DEG C/min of degree is warming up to 900 DEG C, keeps the temperature 180min, is finally warming up to 1060 DEG C by 3 DEG C/min of heating rate, keeps the temperature 300min Progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet is by heating speed 7 DEG C/min of degree is warming up to 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by heating rate 6 DEG C/min is warming up to 500 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, and sintering magnetic is made Body: it takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 2
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
C 112 13.48 19.73 44.39
D 191 13.51 18.61 44.62
The oxygen content in slab C is well below the oxygen content in slab D from the results shown in Table 2, while magnetic property slab C The magnet HcJ of production is higher than the magnet of slab D production.
Embodiment 3
(Nd, Pr) according to the ratio26.5Dy4.5Co1.5Cu0.2Al0.6Nb0.3B more than Fe0.96(wt%) it carries out ingredient and adds in mass ratio 0.12% silicomangan is denoted as E as additive;Do not add it is additivated be denoted as F, by E, F rare-earth Nd-Fe-B material by fusing point by High to low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, and heating power setting is arrived 160kW carries out preheating and guarantees that steam of raw material etc. excludes, and being by power setting after preheating is 12 minutes the 530kW time, Then carrying out thermometric temperature is 1460 DEG C, and copper roller revolving speed is set as 36r/min and casts, and slab average thickness is 0.27mm, Slab was come out of the stove at argon atmosphere cooling 120 minutes;E, F slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, into furnace It being filled with hydrogen and carries out hydrogen abstraction reaction, the suction hydrogen time is 150min, it is vacuumized again after inhaling hydrogen and is heated to 550 DEG C of progress dehydrogenations, Dehydrogenation time is 380min, and heating furnace is opened after dehydrogenation and carries out spraying cooling to furnace body, cooling≤40 DEG C of temperature are come out of the stove To neodymium iron boron fine powder.After airflow milling, fine powder E milling particle size consistent with fine powder F milling particle size is all 2.95-3.15um.E,F The square blank of powder compression moulding 63 × 39 × 33 (mm) in the alignment magnetic field of >=1.6T, blank is placed into sintering furnace It is evacuated to 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;It presses again 3 DEG C/min of heating rate is warming up to 890 DEG C, keeps the temperature 180min, is finally warming up to 1065 DEG C by 2 DEG C/min of heating rate, heat preservation 330min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet is pressed 6 DEG C/min of heating rate is warming up to 895 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by liter Warm 6 DEG C/min of speed is warming up to 510 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, is made and burns Knot magnet: it takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 3
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
E 108 12.48 26.95 38.15
F 193 12.52 26.03 38.27
The oxygen content in slab E is well below the oxygen content in slab F from the results shown in Table 3, while magnetic property slab E The magnet HcJ of production is higher than the magnet of slab F production.
Embodiment 4
(Nd, Pr) according to the ratio30.3Dy5.7Co2Cu0.2Al0.1Nb0.3B more than Fe0.95(wt%) it carries out ingredient and adds in mass ratio 0.15% ferro-aluminum is denoted as G as additive;Do not add it is additivated be denoted as H, by G, H rare-earth Nd-Fe-B material by fusing point by up to Low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, by heating power setting to 150kW Carry out preheating and guarantee that steam etc. of raw material excludes, being by power setting after preheating is 12 minutes the 520kW time, then into Row thermometric temperature is 1470 DEG C, and copper roller revolving speed is set as 35r/min and casts, and slab average thickness is 0.27mm, by slab It came out of the stove at argon atmosphere cooling 120 minutes;G, H slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, hydrogen is filled with into furnace Gas carries out hydrogen abstraction reaction, and the suctions hydrogen time is 150min, vacuumizes be heated to 550 DEG C of progress dehydrogenations again after suction hydrogen, when dehydrogenation Between be 380min, heating furnace is opened after dehydrogenation, spraying cooling is carried out to furnace body, cooling≤40 DEG C of temperature are come out of the stove to obtain neodymium iron Boron fine powder.After airflow milling, fine powder G milling particle size consistent with fine powder H milling particle size is all 3.1-3.2um.G, H powder >= 55 × 40 × 32mm of compression moulding in the alignment magnetic field of 1.6T) square blank, blank is placed into sintering furnace and is evacuated to 5.0×10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;Heating rate is pressed again 3 DEG C/min is warming up to 900 DEG C, keeps the temperature 180min, is finally warming up to 1065 DEG C by 2 DEG C/min of heating rate, keep the temperature 330min into Row magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet presses heating rate 6 DEG C/min is warming up to 895 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by heating rate 6 DEG C/min is warming up to 495 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, sintered magnet is made: It takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 4
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
G 116 13.05 26.31 41.27
H 187 13.12 25.63 41.53
The oxygen content in slab G is well below the oxygen content in slab H from the results shown in Table 4, while magnetic property slab G The magnet HcJ of production is higher than the magnet of slab H production.
Embodiment 5
(Nd, Pr) according to the ratio30.5Dy1.2Co1Cu0.15Al0.1Nb0.3B more than Fe0.97(wt%) it carries out ingredient and adds in mass ratio 0.18% Si-Al-Ba-Ca is denoted as I as additive;Do not add it is additivated be denoted as J, by I, J rare-earth Nd-Fe-B material by fusing point by High to low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, and heating power setting is arrived 140kW carries out preheating and guarantees that steam of raw material etc. excludes, and being by power setting after preheating is 13 minutes the 510kW time, Then carrying out thermometric temperature is 1450 DEG C, and copper roller revolving speed is set as 38r/min and casts, and slab average thickness is 0.28mm, Slab was come out of the stove at argon atmosphere cooling 120 minutes;I, J slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, into furnace It being filled with hydrogen and carries out hydrogen abstraction reaction, the suction hydrogen time is 150min, it is vacuumized again after inhaling hydrogen and is heated to 550 DEG C of progress dehydrogenations, Dehydrogenation time is 380min, and heating furnace is opened after dehydrogenation and carries out spraying cooling to furnace body, cooling≤40 DEG C of temperature are come out of the stove To neodymium iron boron fine powder.After airflow milling, fine powder I milling particle size consistent with fine powder J milling particle size is all 3.15-3.25um.I,J Powder 58 × 42.5 × 33mm of compression moulding in the alignment magnetic field of >=1.6T) square blank, blank is placed into sintering furnace Inside it is evacuated to 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;Again 900 DEG C are warming up to by 3 DEG C/min of heating rate, keeps the temperature 180min, is finally warming up to 1060 DEG C by 2 DEG C/min of heating rate, is protected Warm 270min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below are warming up to by 6 DEG C/min of heating rate, are pressed 6 DEG C/min of heating rate is warming up to 505 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, is made Sintered magnet: it takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 5
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
I 121 14.03 17.65 49.58
J 191 14.09 16.93 49.72
The oxygen content in slab I is well below the oxygen content in slab J from the results shown in Table 5, while magnetic property slab I The magnet HcJ of production is higher than the magnet of slab J production.
Embodiment 6
(Nd, Pr) according to the ratio29.8Tb1Co1Cu0.1Zr0.1B more than Fe0.96(wt%) it carries out ingredient and adds 0.1% aluminium in mass ratio Iron and 0.08% manganese iron are denoted as K as additive;Do not add it is additivated be denoted as L, by K, L rare-earth Nd-Fe-B material by fusing point by High to low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, and heating power setting is arrived 150kW carries out preheating and guarantees that steam of raw material etc. excludes, and being by power setting after preheating is 13 minutes the 510kW time, Then carrying out thermometric temperature is 1450 DEG C, and copper roller revolving speed is set as 36r/min and casts, and slab average thickness is 0.28mm, Slab was come out of the stove at argon atmosphere cooling 120 minutes;K, L slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, into furnace It being filled with hydrogen and carries out hydrogen abstraction reaction, the suction hydrogen time is 150min, it is vacuumized again after inhaling hydrogen and is heated to 550 DEG C of progress dehydrogenations, Dehydrogenation time is 380min, and heating furnace is opened after dehydrogenation and carries out spraying cooling to furnace body, cooling≤40 DEG C of temperature are come out of the stove To neodymium iron boron fine powder.After airflow milling, fine powder K milling particle size is consistent with fine powder L milling particle size all to be all 2.9-3.1um. K, L powder 45 × 32.7 × 28mm of compression moulding in the alignment magnetic field of >=1.6T) square blank, blank is placed into sintering 5.0 × 10 are evacuated in furnace-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle; 900 DEG C are warming up to by 3 DEG C/min of heating rate again, 180min is kept the temperature, is finally warming up to 1070 DEG C by 2 DEG C/min of heating rate, Heat preservation 330min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnetic Body is warming up to 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below by 6 DEG C/min of heating rate, 505 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min are warming up to by 6 DEG C/min of heating rate and complete second segment ageing treatment, are made It obtains sintered magnet: taking slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 6
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
K 106 14.35 17.81 51.66
L 185 14.41 17.15 51.83
The oxygen content in slab K is well below the oxygen content in slab L from the results shown in Table 6, while magnetic property slab K The magnet HcJ of production is higher than the magnet of slab L production.
Comparative example 1
This comparative example 1 the difference from embodiment 1 is that, the additive amount of deoxidier is greater than the upper limit of the scope of the invention.And progressive It can comparison.
(Nd, Pr) according to the ratio30Dy1Co1Cu0.15Al0.4Zr0.1B more than Fe0.96(wt%) it carries out ingredient and adds in mass ratio 0.3% manganese iron is denoted as M as additive;Do not add it is additivated be denoted as N, by M, N rare-earth Nd-Fe-B material by fusing point by up to Low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, by heating power setting to 150kW Carry out preheating and guarantee that steam etc. of raw material excludes, being by power setting after preheating is 13 minutes the 510kW time, then into Row thermometric temperature is 1460 DEG C, and copper roller revolving speed is set as 35r/min and casts, and slab average thickness is 0.28mm, by slab It came out of the stove at argon atmosphere cooling 120 minutes;M, N slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, hydrogen is filled with into furnace Gas carries out hydrogen abstraction reaction, and the suctions hydrogen time is 150min, vacuumizes be heated to 550 DEG C of progress dehydrogenations again after suction hydrogen, when dehydrogenation Between be 380min, heating furnace is opened after dehydrogenation, spraying cooling is carried out to furnace body, cooling≤40 DEG C of temperature are come out of the stove to obtain neodymium iron Boron fine powder.After airflow milling, fine powder M milling particle size is consistent with fine powder N milling particle size all to be all 2.9-3.0um.K, L powder 67.8 × 42 × 39mm of compression moulding in the alignment magnetic field of >=1.6T) square blank, blank is placed into sintering furnace and is taken out Vacuum is to 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;Again by liter Warm 3 DEG C/min of speed is warming up to 900 DEG C, keeps the temperature 180min, is finally warming up to 1060 DEG C by 2 DEG C/min of heating rate, heat preservation 300min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet is pressed 6 DEG C/min of heating rate is warming up to 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by liter Warm 6 DEG C/min of speed is warming up to 500 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, is made and burns Knot magnet: it takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 7
The oxygen content in slab M is far below the oxygen content in slab N from the results shown in Table 7, but magnet performance Br and (BH) m declines by a big margin.
Comparative example 2
(Nd, Pr) according to the ratio28Dy2Gd1Co1.5Cu0.2Al0.8Zr0.1B more than Fe0.95(wt%) it carries out ingredient and adds in mass ratio 0.01% ferro-aluminum is denoted as O as additive;Do not add it is additivated be denoted as P, by O, P rare-earth Nd-Fe-B material by fusing point by up to Low sequence is placed into the crucible of vacuum rapid hardening furnace, and vacuum rapid hardening furnace is evacuated to≤8Pa, by heating power setting to 150kW Carry out preheating and guarantee that steam etc. of raw material excludes, being by power setting after preheating is 13 minutes the 510kW time, then into Row thermometric temperature is 1470 DEG C, and copper roller revolving speed is set as 35r/min and casts, and slab average thickness is 0.27mm, by slab It came out of the stove at argon atmosphere cooling 120 minutes;O, P slab are put into hydrogen breaking furnace and are evacuated to≤5Pa, hydrogen is filled with into furnace Gas carries out hydrogen abstraction reaction, and the suctions hydrogen time is 150min, vacuumizes be heated to 550 DEG C of progress dehydrogenations again after suction hydrogen, when dehydrogenation Between be 380min, heating furnace is opened after dehydrogenation, spraying cooling is carried out to furnace body, cooling≤40 DEG C of temperature are come out of the stove to obtain neodymium iron Boron fine powder.After airflow milling, fine powder O milling particle size is consistent with fine powder P milling particle size all to be all 2.85-2.95um.O, P powder Expect 67.8 × 42 × 39mm of compression moulding in the alignment magnetic field of >=1.6T) square blank, blank is placed into sintering furnace It is evacuated to 5.0 × 10-1Pa or less is warming up to 400 DEG C by 8 DEG C/min of temperature is risen, and heat preservation 60min carries out dumping and goes out to handle;It presses again 3 DEG C/min of heating rate is warming up to 900 DEG C, keeps the temperature 180min, is finally warming up to 1060 DEG C by 2 DEG C/min of heating rate, heat preservation 300min progress magnet finally densifies again air-cooled to 150 DEG C or less of argon filling and obtains sintered magnet;Sintered magnet is pressed 6 DEG C/min of heating rate is warming up to 900 DEG C of heat preservation 120min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by liter Warm 6 DEG C/min of speed is warming up to 500 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 240min and completes second segment ageing treatment, is made and burns Knot magnet: it takes slab to compare oxygen content, the standard specimen of magnet Φ 10 × 10 (mm) is taken to compare test magnetic property.
Table 8
Project Slab oxygen content/ppm Br/KGs HcJ/KOe (BH)m/MGsOe
M 169 12.49 23.63 37.89
N 176 12.51 23.57 37.91
The oxygen content in slab O and the oxygen content in slab P are without bigger difference, magnet performance from the results shown in Table 8 Without larger promotion.
By comparative example 1-2 it is found that the content of additive is most important in the present invention, can not arbitrarily change.And by implementing Example 1-6 in gained neodymium iron boron oxygen content it is found that the present invention can by the Control for Oxygen Content of neodymium iron boron in 121ppm hereinafter, with existing Technology is compared and achieves significant progress.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field;In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side The protection scope of case.

Claims (10)

1. a kind of method for reducing rare-earth Nd-Fe-B oxygen content, it is characterised in that the following steps are included:
S1: weighing each raw material of neodymium iron boron and additional oxytropism is higher than the additive of iron;The additive amount of the additive is total The 0.02-0.2wt% of amount;Resulting material is placed in the crucible of vacuum rapid hardening furnace, by vacuum rapid hardening stove evacuation;
S2: preheating material, excludes the steam of material;
S3: after preheating, further heating material, and temperature is made to reach 1400-1500 DEG C;
S4: removal floats on the oxide of bath surface obtained by S4, casts, obtains slab;By slab in atmosphere of inert gases Cooling is come out of the stove;
S5: slab obtained by S4 is subjected to hydrogen breaking;
S6: the material after hydrogen breaking is subjected to airflow milling powder;
S7: after powder obtained by S6 is formed, is sintered, neodymium iron boron magnetic body is made.
2. a kind of method for reducing rare-earth Nd-Fe-B slab oxygen content as described in claim 1, which is characterized in that in S1, institute Stating additive is at least one of silicomangan, ferrosilicon, manganese iron, ferro-aluminum, Si-Al-Ba-Ca.
3. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S1, the neodymium Each raw material of iron boron are as follows: RaFe100-a-b-cBbMc;Mass percent is 35% >=a >=20%, 1.2% >=b >=0.9%, 6% >=c >=0%, R For one of Nd, Pr, Dy, Tb, Gd and Ho or a variety of;M is one of Co, Ga, Al, Cu, Nb, Zr and Mn or a variety of.
4. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S1, by fusing point It adds materials from high to low, is evacuated to≤8Pa.
5. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S2, pre- hot merit Rate is 120-200kW.
6. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S3, heat function Rate is 350-550kW, heating time 7-15min.
7. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S4, in 35- It casts under the copper roller revolving speed of 45r/min, gained slab average thickness is 0.2-0.4mm.
8. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that described de- in S4 Property gas be argon gas, cooling 120-150min.
9. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S5, hydrogen breaking Specifically comprises the processes of: slab is put into hydrogen breaking furnace and is evacuated to≤10Pa, hydrogen is filled with into furnace and carries out hydrogen abstraction reaction, The suction hydrogen time is 60-210min, vacuumizes again after inhaling hydrogen and is heated to 500-600 DEG C of progress dehydrogenation, dehydrogenation time 240- 420min opens furnace and carries out spraying cooling to≤60 DEG C to furnace body, comes out of the stove to obtain neodymium iron boron fine powder after dehydrogenation.
10. a kind of method for reducing rare-earth Nd-Fe-B oxygen content as described in claim 1, which is characterized in that in S7, molding, Sintering specifically comprises the processes of: the powder Jing Guo airflow milling is placed into magnetic field >=1.4T press and is formed, it is after molding Green compact, which are placed into sintering furnace, is evacuated to 5.0 × 10-1Pa or less is warming up to 350-450 DEG C by 5-10 DEG C of temperature/min is risen, and protects Warm 40-80min carries out dumping and goes out to handle;It is warming up to 850-950 DEG C by 3-5 DEG C/min of heating rate again, keeps the temperature 120-240min, It finally is warming up to 1060-1080 DEG C by 2-4 DEG C/min of heating rate, heat preservation 240-360min progress magnet finally densifies to be filled again Air-cooled to 150 DEG C or less of argon obtain sintered magnet;Sintered magnet by 5-8 DEG C/min of heating rate be warming up to 880 DEG C- 920 DEG C of heat preservation 90min-180min, then air-cooled to 150 DEG C first segment ageing treatments accomplished below, by 5-8 DEG C/min of heating rate It is warming up to 450 DEG C of -550 DEG C of air-cooled come out of the stove to 60 DEG C or less of heat preservation 180min-300min and completes second segment ageing treatment.
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