WO2015147053A1 - R-t-b系焼結磁石の製造方法 - Google Patents
R-t-b系焼結磁石の製造方法 Download PDFInfo
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- WO2015147053A1 WO2015147053A1 PCT/JP2015/059117 JP2015059117W WO2015147053A1 WO 2015147053 A1 WO2015147053 A1 WO 2015147053A1 JP 2015059117 W JP2015059117 W JP 2015059117W WO 2015147053 A1 WO2015147053 A1 WO 2015147053A1
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
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- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
- H01F41/0266—Moulding; Pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the present invention relates to a method for manufacturing an RTB based sintered magnet.
- RTB-based sintered magnet having an R 2 T 14 B type compound as a main phase (R is composed of a light rare earth element RL and a heavy rare earth element RH, where RL is Nd and / or Pr, RH is Dy, Tb, Gd and Ho are at least one kind, and T is a transition metal element and necessarily contains Fe), and is known as the most powerful magnet among permanent magnets.
- R is composed of a light rare earth element RL and a heavy rare earth element RH, where RL is Nd and / or Pr, RH is Dy, Tb, Gd and Ho are at least one kind, and T is a transition metal element and necessarily contains Fe
- the RTB -based sintered magnet is required to have a high coercive force H cJ (hereinafter sometimes simply referred to as “H cJ ”), particularly when used in a hybrid vehicle or electric vehicle motor.
- H cJ high coercive force
- Patent Documents 1 to 3 in an RTB-based sintered magnet, the B content is lower than the B content generally contained (less than the B amount in the stoichiometric ratio of the R 2 T 14 B type compound). low) were upon, by the addition of Ga or the like, without using much as possible heavy rare earth element such as Dy, while suppressing a decrease in B r, it is proposed to obtain a high H cJ.
- Patent Document 1 discloses that an R 2 T 17 phase is formed by lowering the amount of B than a normal RTB-based alloy and containing one or more metal elements selected from Al, Ga, and Cu. By generating a sufficient volume fraction of the transition metal rich phase (R 6 T 13 M) generated using the R 2 T 17 phase as a raw material, a RTB-based rare earth sintered with a high coercive force is obtained. It is described that a magnet is obtained.
- Patent Document 2 as well as below the critical content of boron in the conventional R-T-B based permanent magnet, Co, an alloy containing Cu and Ga is high at the same remanence B r than the conventional alloy anti It is described that it has a magnetic force HcJ .
- the amount of B is made lower than that of a normal RTB-based alloy, the amounts of B, Al, Cu, Co, Ga, C, and O are set within a predetermined range, and Nd with respect to B is further reduced. And Pr, and the atomic ratios of Ga and C each satisfy a specific relationship, it is described that high residual magnetic flux density and coercive force can be obtained.
- the rate of temperature rise may vary depending on the position in the furnace, so when heat treating a large amount of RTB-based sintered magnet material Depending on the placement position of the RTB-based sintered magnet material, the time required to reach the heat treatment temperature may differ, and accordingly, the holding time at the heat treatment temperature may differ depending on the placement position. For example, depending on the structure of the heat treatment furnace, the holding time at the heat treatment temperature may differ by about 2 hours depending on the mounting position. Usually, the holding time at the heat treatment temperature requires about 1 hour.
- a general RTB -based sintered magnet having a B amount equal to or higher than the stoichiometric ratio of the R 2 T 14 B-type compound is not affected by H cJ even if it is heat-treated for 3 hours or more. Does not fluctuate greatly.
- the B amount is lower than that of a general RTB-based sintered magnet as described in Patent Documents 1 to 3 (the chemistry of R 2 T 14 B type compounds). It was found that a sintered magnet having a composition to which Ga or the like was added was lower in the stoichiometric ratio B), and that HcJ significantly decreased when heat treatment was performed for 2 hours or longer. As described above, this phenomenon is not observed with a general RTB-based sintered magnet. As a result, when a large amount of sintered magnets having the compositions described in Patent Documents 1 to 3 are processed in a heat treatment furnace having a large capacity, HcJ of the sintered magnets may vary greatly depending on the mounting position.
- the present invention has been made in order to solve the above-mentioned problems, and is generally used as described in Patent Documents 1 to 3, which can obtain high H cJ without using heavy rare earth elements such as Dy as much as possible.
- an RTB -based sintered magnet having a composition in which the B content is lower than that of a typical RTB -based sintered magnet and Ga or the like is added the HcJ fluctuation due to the heat treatment time can be increased even during mass production.
- An object of the present invention is to provide a method for producing an RTB -based sintered magnet having high HcJ .
- Aspect 1 of the present invention Formula uRwBxGayCuzAlqM (100-uwxxyz-q) T (R is composed of light rare earth element RL and heavy rare earth element RH, RL is Nd and / or Pr, RH is Dy, Tb, Gd and Ho At least one of them, T is a transition metal element and must contain Fe, M is Nb and / or Zr, u, w, x, y, z, q and 100-uwxy -Zq represents mass%),
- Aspect 3 of the present invention is the aspect 1 or aspect 2
- the heat treatment step is a manufacturing method of an RTB-based sintered magnet in which the RTB-based sintered magnet material is heated at a temperature of 450 ° C. or higher and 470 ° C. or lower for 4 hours or longer and 8 hours or shorter.
- an RTB-based sintered material having a composition in which the amount of B is lower than that of a general RTB-based sintered magnet and Ga or the like is added.
- a bonded magnet it is possible to provide a method for producing an RTB -based sintered magnet having high HcJ by suppressing fluctuation of HcJ due to heat treatment time even in mass production.
- FIG. 6 is an explanatory diagram showing a relationship between H cJ and heat treatment time in an RTB sintered magnet of 1-3.
- Sample No. FIG. 3 is an explanatory diagram showing a relationship between H cJ and heat treatment time in an 1-1 RTB -based sintered magnet.
- FIG. 5 is an explanatory diagram showing a relationship between H cJ and heat treatment time in an RTB based sintered magnet having a general B amount.
- the present inventor has found that a general R having a B amount equal to or higher than the stoichiometric ratio of the R 2 T 14 B type compound shown in the first aspect of the present invention.
- the Cu content is adjusted to 0.3 to 1.0 mass% and at 450 ° C to 470 ° C for 4 hours or more. It has been found that an RTB -based sintered magnet having a high H cJ can be produced by suppressing the fluctuation of H cJ due to the heat treatment time even during mass production by performing the heat treatment for less than the time.
- Patent Document 1 two steps of heat treatment at 800 ° C. and 500 ° C. are performed on a sintered magnet having a composition with a Cu content of 0 to 0.31% by mass, but there is no description of the heat treatment time.
- Patent Document 2 a sintered magnet having a composition with a Cu content of 0.1 to 0.19% by mass is subjected to a heat treatment pattern as described in FIGS. 3 and 4 of Patent Document 2 at 440 ° C. to 550 ° C. Heat treatment at 0 ° C. is performed for 1 to 2 hours.
- the heat treatment time is as short as 1 to 2 hours, when a large-capacity heat treatment furnace generally used as a production facility is used, the H cJ of the sintered magnet depends on the mounting position. It can fluctuate greatly.
- Patent Document 3 performs heat treatment for 1 hour at 850 ° C. and for 2 hours at 540 ° C. with respect to the sintered magnet having a composition of 0.6 mass% Cu in the examples.
- the heat treatment temperature is not an optimum temperature according to the composition, so that not only high HcJ is not obtained, but also when a heat treatment furnace having a large capacity that is generally used as a production facility is used.
- the HcJ of the sintered magnet may vary greatly depending on the mounting position.
- RTB-based sintered magnet before the heat treatment process is referred to as an “RTB-based sintered magnet material”, and the RTB-based sintered magnet after the heat treatment process is simply referred to as “ It is called “RTB-based sintered magnet”.
- a metal or alloy of each element is prepared so that the RTB-based sintered magnet material has the composition described in detail below.
- a flaky raw material alloy is produced by a strip casting method or the like.
- an alloy powder is prepared from the flaky raw material alloy, and the RTB-based sintered magnet material is prepared by molding and sintering the alloy powder.
- the production, molding, and sintering of the alloy powder are performed as follows as an example.
- the obtained flaky raw material alloy is pulverized with hydrogen to obtain coarsely pulverized powder of, for example, 1.0 mm or less.
- the coarsely pulverized powder is finely pulverized in an inert gas by a jet mill or the like.
- the particle diameter D 50 volume center value (volume-based median diameter) obtained by measurement by an air flow dispersion type laser diffraction method) is 3 to A finely pulverized powder (alloy powder) of 5 ⁇ m is obtained.
- the alloy powder one kind of alloy powder (single alloy powder) may be used, or a so-called two alloy method may be used in which an alloy powder (mixed alloy powder) is obtained by mixing two or more kinds of alloy powder.
- the alloy powder may be prepared so as to have the composition of the present invention by using a known method.
- a known lubricant may be added as an auxiliary agent to the coarsely pulverized powder before jet mill pulverization, and to the alloy powder during and after jet mill pulverization.
- the obtained alloy powder is molded in a magnetic field to obtain a molded body. Molding is performed by inserting a dry alloy powder into a mold cavity and molding it, and injecting a slurry containing a dispersion medium and an alloy powder dispersed in the dispersion medium into the mold cavity, Any known molding method including a wet molding method of molding while discharging the slurry dispersion medium may be used. Then, the RTB-based sintered magnet material is obtained by sintering the compact.
- a well-known method can be used for sintering of a molded object.
- the atmosphere gas is preferably an inert gas such as helium or argon.
- composition of the RTB-based sintered magnet material in the present invention is: Formula uRwBxGayCuzAlqM (100-uwxyzzq) T (1) (R is composed of light rare earth element RL and heavy rare earth element RH, RL is Nd and / or Pr, RH is at least one of Dy, Tb, Gd and Ho, and T is a transition metal element and always contains Fe.
- M is Nb and / or Zr, u, w, x, y, z, q and 100-uwxyzz represent mass%)
- the RH is 5% by mass or less of the RTB-based sintered magnet, 29.5 ⁇ u ⁇ 32.0 (2) 0.86 ⁇ w ⁇ 0.93 (3) 0.2 ⁇ x ⁇ 1.0 (4) 0.3 ⁇ y ⁇ 1.0 (5) 0.05 ⁇ z ⁇ 0.5 (6) 0 ⁇ q ⁇ 0.1 (7)
- p [B] /10.811 ⁇ 14 ⁇ ([Fe] /55.847+ [Co] /58.933) (8) ([B], [Fe], and [Co] represent mass% of B, Fe, and Co, respectively) p ⁇ 0 (9) Satisfy the relationship.
- the RTB-based sintered magnet of the present invention can contain inevitable impurities.
- the effects of the present invention can be achieved even if inevitable impurities normally contained in didymium alloy (Nd—Pr), electrolytic iron, ferroboron, and the like are contained.
- Inevitable impurities are, for example, La, Ce, Cr, Mn, Si and the like.
- the amount of B is made lower than that of a general RTB-based sintered magnet, and Ga and the like are contained. Therefore, as in Patent Documents 1 to 3, the R— A T-Ga phase (and RT-Ga-Cu phase) is produced. As a result, it is possible to obtain high HcJ without using heavy rare earth elements such as Dy as much as possible.
- R is composed of a light rare earth element RL and a heavy rare earth element RH, and RL means Nd and / or Pr (that is, RL means Nd and Pr).
- the RTB-based sintered magnet may include at least one of Nd and Pr.)
- RH is at least one of Dy, Tb, Gd, and Ho (that is, RH is Dy, Tb, Gd).
- the RTB-based sintered magnet of the present invention may include at least one of Dy, Tb, Gd, and Ho.), RH is 5 of the RTB-based sintered magnet. It is below mass%.
- the present invention can obtain a high B r and high H cJ without using a heavy rare earth elements, it can reduce the amount of RH even be asked a higher H cJ, typically 2.5 It can be made into the mass% or less.
- R amount (u) can not be obtained a high B r can not sufficiently densified to insufficient liquid phase during sintering is less than 29.5 wt%, it exceeds 32.0 mass% main phase As a result, the ratio is lowered, and a high Br cannot be obtained.
- they are 30.0 mass% or more and 31.5 mass% or less.
- T is a transition metal element and necessarily contains Fe. Examples of transition metal elements other than Fe include Co.
- the substitution amount of Co is preferably 2.5% by mass or less, and if the substitution amount (content) of Co exceeds 10% by mass, Br is lowered, which is not preferable. Further, a small amount of V, Cr, Mn, Mo, Hf, Ta, W, or the like may be contained.
- B is boron, and the amount of B is 0.86 mass% or more and 0.93 mass% or less. B amount (w) can not be the main phase ratio can not be obtained a high H cJ was precipitated R 2 T 17 phase to obtain a high B r drops is less than 0.86 wt%, 0.93 If it exceeds mass%, the RT-Ga phase is reduced and high HcJ cannot be obtained. Preferably they are 0.88 mass% or more and 0.91 mass% or less.
- Ga content (x) is 0.2 mass% or more and 1.0 mass% or less. If the Ga content is less than 0.2% by mass, the amount of RT-Ga phase produced is so small that the R 2 T 17 phase cannot be lost and high H cJ cannot be obtained. There is a fear. When the content of Ga exceeds 1.0 weight%, will be unnecessary Ga is present, there is a possibility that B r decreases to decrease the main phase proportion.
- the Ga content is preferably 0.3% by mass or more and 0.7% by mass or less.
- Cu amount (y) is 0.3 mass% or more and 1.0 mass% or less.
- the amount of Cu (y) is less than 0.3% by mass, the HcJ fluctuation due to the heat treatment time cannot be suppressed, and the heat treatment furnace having a large capacity generally used as a production facility as described above. Is used, the HcJ of the RTB -based sintered magnet varies greatly depending on the mounting position.
- Cu content exceeds 1.0 mass%, will be unnecessary Cu is present, there is a possibility that B r decreases to decrease the main phase proportion.
- a preferable amount of Cu is 0.5% by mass or more and 0.7% by mass or less.
- Al amount (z) is 0.05 mass% or more and 0.5 mass% or less. By containing Al, HcJ can be improved. Al may be contained as an inevitable impurity, or may be positively added and contained. The total amount of unavoidable impurities and positively added amount is 0.05% by mass or more and 0.5% by mass or less.
- an RTB-based sintered magnet contains Nb and / or Zr to suppress abnormal grain growth during sintering.
- Nb and / or Zr may be contained in a total amount of 0.1% by mass or less (that is, at least one of Nb and Zr may be contained, and the total amount of Nb and Zr is 0.1 % By mass or less).
- the content of Nb and / or Zr is present unwanted Nb and Zr exceeds 0.1 mass% in total, there is a possibility that the main phase ratio is lowered B r drops.
- the composition of the RTB-based sintered magnet material in the present invention makes the B amount lower than that of a general RTB-based sintered magnet.
- the R 2 T 17 phase which is a soft magnetic phase, does not precipitate in addition to the R 2 T 14 B phase, which is the main phase ([B] /10.811 (B (Atomic weight of) ⁇ 14) does not fall below ([Fe] /55.847 (atomic weight of Fe) + [Co] /58.933 (atomic weight of Co)).
- composition shown in FIG. 3 is ([B] /10.811 (B atomic weight) ⁇ 14) ([Fe] /55.847 (Fe atomic weight) + [Co] /58.933 (Co The composition (p> 0) does not fall below the atomic weight).
- the R—T—Ga phase means an R content of 15 mass% to 65 mass%, a T content of 20 mass% to 80 mass%, and a Ga content of 2 mass% to 20 mass%.
- a compound having the following composition typically a compound having a La 6 Co 11 Ga 3 type crystal structure, specifically, an R 6 T 13- ⁇ Ga 1 + ⁇ compound.
- the RTB-Ga phase is obtained when the RTB-based sintered magnet contains Al, Cu, or Si.
- the obtained RTB-based sintered magnet material is heated at a temperature of 450 ° C. to 470 ° C. for 4 hours to 12 hours.
- high H cJ can be obtained, and fluctuations in H cJ due to heat treatment time can be suppressed. If the heat treatment temperature and time deviate from the scope of the present invention, high HcJ cannot be obtained, or the heat treatment time is too long and productivity is lowered. In particular, when the heat treatment time is less than 4 hours, H cJ may vary depending on the position of the heat treatment furnace, and high H cJ may not be obtained.
- the heat treatment time exceeds 8 hours, the production efficiency is lowered, and further, HcJ may be lowered. Preferably it is 4 hours or more and 8 hours or less. This is because the fluctuation range of H cJ due to the heat treatment time can be further suppressed, and high H cJ can be obtained.
- the heat treatment step is performed after the heat treatment at 600 ° C. or higher and 1020 ° C. or lower is performed on the RTB-based sintered magnet material before the heat treatment step.
- the heat treatment By performing the heat treatment, higher HcJ can be obtained.
- you may perform the said heat processing and the said heat processing process continuously after sintering. For example, after the molded body is sintered at 1100 ° C. and cooled to 460 ° C., it is subsequently kept at 460 ° C. for 6 hours to perform a heat treatment process, or after the molded body is sintered at 1100 ° C. and cooled to 800 ° C. After that, the heat treatment may be performed by holding at 800 ° C. for 2 hours, and then cooling to 460 ° C., and further continuing at 460 ° C. for 6 hours.
- the obtained sintered magnet may be subjected to machining such as grinding in order to adjust the magnet dimensions.
- the heat treatment may be performed before or after machining.
- the surface treatment may be a known surface treatment, and for example, a surface treatment such as Al vapor deposition, electric Ni plating, or resin coating can be performed.
- the resulting coarsely pulverized powder was mixed with an airflow pulverizer (jet mill device). It was dry milled in a nitrogen stream to obtain a particle size D 50 of fine pulverized powder of 4.0 ⁇ 4.6 .mu.m (the alloy powder).
- the oxygen concentration in the nitrogen gas at the time of pulverization was set to 50 ppm or less so that the finally obtained sintered magnet had an oxygen content of about 0.1 mass%.
- the particle diameter D 50 is the volume center value obtained by measurement by the air flow distributed Laser diffraction (volume basis median diameter).
- the slurry was prepared by dispersing the finely pulverized powder in oil.
- the molded object was obtained by the wet-molding method which inject
- molding apparatus lateral magnetic field shaping
- the obtained molded body was deoiled, sintered in vacuum at 1040 ° C. to 1070 ° C. for 4 hours, and then rapidly cooled to obtain an RTB-based sintered magnet material.
- the density of the RTB-based sintered magnet material was 7.5 Mg / m 3 or more.
- Table 1 shows the components of the obtained RTB-based sintered magnet material and the results of gas analysis (O (oxygen), N (nitrogen), C (carbon)). Each component in Table 1 was measured using high frequency inductively coupled plasma optical emission spectrometry (ICP-OES).
- the obtained RTB-based sintered magnet material was heated, held at 800 ° C. in vacuum for 2 hours, cooled to room temperature, and then heat-treated in vacuum under the conditions described in Tables 2 to 6. After cooling to room temperature. That is, the material No. 1-1 shows the heat treatment conditions (heat treatment temperature and heat treatment time) shown in Table 2, and the material No. 1-2 is the heat treatment condition shown in Table 3, and the material No. For 1-3 to 1-5, heat treatment was performed under the heat treatment conditions shown in Tables 4 to 6, respectively. At this time, the heat treatment under the conditions described in Tables 2 to 6 is performed in an experimental heat treatment furnace with a small capacity, and there is almost no delay in the sample temperature when the temperature is raised.
- the RTB sintered magnet after the heat treatment is machined to prepare a sample having a length of 7 mm, a width of 7 mm, and a thickness of 7 mm, and magnetized with a 3.2 MA / m pulse magnetic field, and then a BH tracer. It was measured B r and H cJ of the sample by. The measurement results are shown in Tables 2 to 6. Note that the composition of the RTB-based sintered magnet after the heat treatment is the same (substantially the same) as that of the RTB-based sintered material shown in Table 1. Analysis was confirmed by analysis (ICP-OES).
- the fluctuation range of HcJ was obtained for Table 2 (Material No. 1-1 ) to Table 6 (Material No. 1-5 ).
- the fluctuation range of H cJ is obtained as follows. First, among the heat treatment temperatures and heat treatment times in each table (each material No.), the optimum temperature and time with the highest HcJ is used as a reference. Next, in the heat treatment time of 4 hours to 12 hours at the optimum temperature, the difference between the lowest H cJ value and the reference H cJ value is obtained, and the difference is obtained as the fluctuation range of H cJ . ⁇ H cJ in the table indicates this difference.
- H cJ was the lowest value among the measurement results of experiments conducted in the range of 4 hours to 12 hours. Is used to find the difference from the standard. For example, in Table 2 (Material No. 1-1 ), the optimum temperature and time with the highest HcJ is Comparative Example 7 (1450 kA / m). Based on the temperature of Comparative Example 7 (480 ° C.), the lowest value of H cJ in the range of the heat treatment time of 4 hours to 12 hours at the temperature of Comparative Example 7 is Comparative Example 8 (heat treatment time: 4 hours, H cJ : 1360 kA / m).
- the variation width of the H cJ becomes 90kA / m.
- Table 3 (Material No. 1-2) to Table 6 (Material No. 1-5) were also obtained.
- the comparative examples and examples used to determine the fluctuation range of HcJ are underlined. Further, in the present invention, as a range in which there is no problem in production, the fluctuation range of H cJ is 60 kA / m or less, and the fluctuation width of H cJ is suppressed.
- RTB-based sintered magnets (material Nos. 1-2, 1-3, 1-4, 1-5) satisfying the composition conditions of the present invention are as shown in Tables 3 to 6. Furthermore, in the heat treatment time and heat treatment temperature of the present invention, the fluctuation range of HcJ is 17 to 57 kA / m, which is smaller than 60 kA / m. Note that, as described above, the fluctuation range of H cJ in Tables 3 to 6 is obtained on the basis of the optimum temperature at which H cJ is the highest, but also at other heat treatment temperatures and heat treatment times of the present invention. The fluctuation range of H cJ is smaller than 60 kA / m.
- the H cJ fluctuation range of Examples 4 to 6 (450 ° C.) is 20 kA / m, and the H cJ fluctuation range of Examples 10 to 13 (470 ° C.) is 52 kA / m.)
- the RTB-based sintered stone material No. 1-1 whose Cu content is outside the composition range of the present invention is H.sub.2 even at the heat treatment temperature and heat treatment time of the present invention.
- the fluctuation range of cJ is 90 kA / m, which exceeds 60 kA / m.
- the material No. whose Cu amount is outside the composition range of the present invention. 1-1 has a large fluctuation range of H cJ , and at any heat treatment temperature, H cJ rapidly decreases when the heat treatment time exceeds 2 hours.
- the composition satisfying the conditions of the present invention (Material Nos. 1-3) has a suppressed fluctuation range of HcJ , and further the temperature range of the present invention (450 C.-470 ° C.), high H cJ is obtained.
- the particle diameter D 50 is the volume center value obtained by measurement by the air flow distributed Laser diffraction (volume basis median diameter).
- the finely pulverized powder was molded and sintered in the same manner as in Experimental Example 1 to obtain an RTB-based sintered magnet material.
- the density of the RTB-based sintered magnet material was 7.5 Mg / m 3 or more.
- Components of the obtained RTB-based sintered magnet material and gas analysis (O (oxygen), N (nitrogen), C (carbon)) were performed in the same manner as in Experimental Example 1. The results are shown in Table 7.
- the obtained RTB-based sintered magnet material was heated, held at 800 ° C. in vacuum for 2 hours, cooled to room temperature, and then heat-treated in vacuum under the conditions described in Table 8 to Table 12. After cooling to room temperature. That is, the material No. No. 2-1 shows the heat treatment conditions (heat treatment temperature and heat treatment time) in Table 8, and similarly, the material No. In 2-2 to 2-5, heat treatment was performed under the heat treatment conditions shown in Table 9 to Table 12, respectively. At this time, the heat treatment under the conditions described in Tables 8 to 12 is performed in a small-capacity experimental heat treatment furnace, and there is almost no delay in the sample temperature when the temperature is raised. This corresponds to the time during which the RTB-based sintered magnet material is held at the heat treatment temperature.
- RTB-based sintered magnets (material Nos. 2-2, 2-3, 2-4, 2-5) satisfying the composition conditions of the present invention are as shown in Tables 9 to 12.
- the RTB -based sintered stone (material No. 2-1) whose Cu amount is outside the composition range of the present invention has a fluctuation range of HcJ of 68 kA / m as shown in Table 8. , Exceeding 60 kA / m.
- Tables 9 to 12 even if the composition conditions of the present invention are satisfied, if the heat treatment temperature exceeds 2 hours, the H cJ decreases when the heat treatment time exceeds 2 hours. Yes.
- the oxygen amount of the finally obtained sintered magnet was set to be about 0.1% by mass.
- the particle diameter D 50 is the volume center value obtained by measurement by the air flow distributed Laser diffraction (volume-based median diameter).
- the finely pulverized powder was molded and sintered in the same manner as in Experimental Example 1 to obtain an RTB-based sintered magnet material.
- the density of the RTB-based sintered magnet material was 7.5 Mg / m 3 or more.
- Components of the obtained RTB-based sintered magnet material and gas analysis (O (oxygen), N (nitrogen), C (carbon)) were performed in the same manner as in Experimental Example 1. The results are shown in Table 13.
- the obtained RTB-based sintered magnet material was heated, held at 800 ° C. in vacuum for 2 hours, cooled to room temperature, and then heat-treated in vacuum under the conditions described in Tables 14 to 18. After cooling to room temperature. That is, the material No. 3-1 shows the heat treatment conditions (heat treatment temperature and heat treatment time) shown in Table 14, and similarly, the material No. For 3-2 to 3-5, heat treatment was performed under the heat treatment conditions shown in Table 15 to Table 18, respectively. At this time, the heat treatment under the conditions described in Tables 14 to 18 is performed in an experimental heat treatment furnace with a small capacity, and there is almost no delay in the sample temperature when the temperature is raised. This corresponds to the time during which the RTB-based sintered magnet material is held at the heat treatment temperature.
- RTB-based sintered magnets (material Nos. 3-2, 3-3, 3-4, 3-5) satisfying the composition conditions of the present invention are as shown in Tables 15 to 18.
- the heat treatment temperature of the present invention, the heat treatment time, and the variation width of the H cJ is 8 ⁇ 49kA / m, less than 60 kA / m.
- the RTB-based sintered stone (sample No. 3-1) in which the Cu amount is outside the composition range of the present invention has a fluctuation range of HcJ of 102 kA / m as shown in Table 14. , Exceeding 60 kA / m.
- Tables 15 to 18 even if the composition conditions of the present invention were satisfied, when the heat treatment time exceeded 2 hours, the H cJ decreased when the heat treatment temperature exceeded 2 hours. Yes.
- Example 4 Using Nd metal, Pr metal, electrolytic Co, Al metal, Cu metal, Ga metal, electrolytic iron (all with a purity of 99% or more) and ferroboron alloy, ferroniobium alloy, ferrozirconium alloy, the composition after sintering is shown in Table 19.
- a coarsely pulverized powder was prepared in the same manner as in Experimental Example 1. After adding and mixing 0.04% by mass of zinc stearate as a lubricant with respect to 100% by mass of the coarsely pulverized powder, the resulting coarsely pulverized powder was mixed with nitrogen using an airflow pulverizer (jet mill device).
- the finely pulverized powder was molded and sintered in the same manner as in Experimental Example 1 to obtain an RTB-based sintered magnet material.
- the density of the RTB-based sintered magnet material was 7.5 Mg / m 3 or more.
- the obtained RTB-based sintered magnet material was heated, held at 800 ° C. in vacuum for 2 hours, cooled to room temperature, and then heat-treated in vacuum under the conditions described in Tables 20 to 24. After cooling to room temperature. That is, the material No. 4-1 shows the heat treatment conditions (heat treatment temperature and heat treatment time) in Table 20, and similarly, the material No. In 4-2 to 4-5, heat treatment was performed under the heat treatment conditions shown in Table 21 to Table 24, respectively. At this time, the heat treatment under the conditions shown in Tables 20 to 24 is performed in a small-capacity experimental heat treatment furnace, and there is almost no delay in the sample temperature when the temperature is raised. This corresponds to the time during which the RTB-based sintered magnet material is held at the heat treatment temperature.
- the RTB-based sintered magnet (material No. 4-3) satisfying the composition conditions of the present invention has an H cJ of the heat treatment temperature and heat treatment time of the present invention.
- the fluctuation range is 15 kA / m, which is smaller than 60 kA / m.
- an RTB-based sintered magnet in which the R amount, B amount or Ga amount is outside the composition range of the present invention (the material No. 4-1 has the R amount, the material No. 4-2 has the B Material No. 4-4 and Material No.
- the RTB-based sintered magnet obtained by the present invention can be suitably used for various motors for hybrid vehicles, electric vehicles, and home appliances.
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Abstract
Description
R2T14B型化合物の化学量論比以上のB量を有する一般的なR-T-B系焼結磁石は、図3に示す通り、3時間以上熱処理を行っても、HcJは大きく変動しない。しかし、発明者らが検討の結果、特許文献1~3に記載されているような一般的なR-T-B系焼結磁石よりもB量を低く(R2T14B型化合物の化学量論比のB量よりも低く)し、Ga等を添加した組成の焼結磁石は、2時間以上の熱処理を行うとHcJが大きく低下することが分かった。この現象は上述したように、一般的なR-T-B系焼結磁石では見られないものである。その結果、特許文献1~3に記載の組成の焼結磁石を容量の大きい熱処理炉で大量に処理すると、載置位置よって焼結磁石のHcJが大きく変動してしまう場合がある。
式uRwBxGayCuzAlqM(100-u-w-x-y-z-q)T(Rは軽希土類元素RLと重希土類元素RHからなり、RLはNdおよび/またはPr、RHはDy、Tb、GdおよびHoのうち少なくとも一種であり、Tは遷移金属元素でありFeを必ず含む、MはNbおよび/またはZrであり、u、w、x、y、z、qおよび100-u-w-x-y-z-qは質量%を示す)によって表され、
前記RHはR-T-B系焼結磁石の5質量%以下であり、
29.5≦u≦32.0、
0.86≦w≦0.93、
0.2≦x≦1.0、
0.3≦y≦1.0、
0.05≦z≦0.5、
0≦q≦0.1であり、かつ、
p=[B]/10.811×14-([Fe]/55.847+[Co]/58.933)([B]、[Fe]、[Co]は、それぞれB、Fe、Coの質量%を示す)のとき、
p<0の関係を満足するR-T-B系焼結磁石素材を準備する工程と、
前記R-T-B系焼結磁石素材を450℃以上470℃以下の温度で4時間以上12時間以下加熱する熱処理工程と、
を含むR-T-B系焼結磁石の製造方法である。
0.3≦x≦0.7、
0.5≦y≦0.7である、R-T-B系焼結磁石の製造方法である。
前記熱処理工程は、前記R-T-B系焼結磁石素材を450℃以上470℃以下の温度で4時間以上8時間以下加熱するR-T-B系焼結磁石の製造方法である。
さらに、特許文献3は、実施例にCu量が0.6質量%の組成の焼結磁石に対し、850℃で1時間及び540℃で2時間の熱処理をおこなっている。しかし、当該熱処理温度は組成に応じた最適な温度とは言えず、そのため、高いHcJが得られないだけでなく、生産設備として一般的に用いられるような容量の大きい熱処理炉を用いた場合、載置位置よって焼結磁石のHcJが大きく変動する可能性がある。
R-T-B系焼結磁石素材を準備する工程は、まず、R-T-B系焼結磁石素材が以下に詳述する組成となるようにそれぞれの元素の金属または合金を準備し、ストリップキャスティング法等によりフレーク状の原料合金を作製する。次に、前記フレーク状の原料合金から合金粉末を作製し、前記合金粉末を成形、焼結することによりR-T-B系焼結磁石素材を準備する。合金粉末の作製、成形、焼結は、一例として以下のようにして行う。得られたフレーク状の原料合金を水素粉砕し、例えば1.0mm以下の粗粉砕粉を得る。次に、粗粉砕粉を不活性ガス中でジェットミル等により微粉砕し、例えば粒径D50(気流分散式レーザー回折法による測定で得られる体積中心値(体積基準メジアン径))が3~5μmの微粉砕粉(合金粉末)を得る。合金粉末は、1種類の合金粉末(単合金粉末)を用いてもよいし、2種類以上の合金粉末を混合することにより合金粉末(混合合金粉末)を得る、いわゆる2合金法を用いてもよく、公知の方法などを用いて本発明の組成となるように合金粉末を作製すればよい。ジェットミル粉砕前の粗粉砕粉、ジェットミル粉砕中およびジェットミル粉砕後の合金粉末に助剤として公知の潤滑剤を添加してもよい。次に得られた合金粉末を磁界中で成形し、成形体を得る。成形は、金型のキャビティー内に乾燥した合金粉末を挿入し、成形する乾式成形法、金型のキャビティー内に分散媒と分散媒中に分散した合金粉末とを含むスラリーを注入し、スラリーの分散媒を排出しながら成形する湿式成形法を含む公知の任意の成形方法を用いてよい。そして、成形体を焼結することによりR-T-B系焼結磁石素材を得る。成形体の焼結は公知の方法を用いることができる。なお、焼結時の雰囲気による酸化を防止するために、焼結は真空雰囲気中または雰囲気ガス中で行うことが好ましい。雰囲気ガスは、ヘリウム、アルゴンなどの不活性ガスを用いることが好ましい。
なお、上記の説明ではフレーク状の原料合金を用いて合金粉末を得る方法を説明したが、フレーク状の原料合金に代えて、フレーク状以外の形状の鋳造材を含む任意の形態の原料合金を用いてよい。
式uRwBxGayCuzAlqM(100-u-w-x-y-z-q)T (1)
(Rは軽希土類元素RLと重希土類元素RHからなり、RLはNdおよび/またはPr、RHはDy、Tb、GdおよびHoのうち少なくとも一種であり、Tは遷移金属元素でありFeを必ず含む、MはNbおよび/またはZrであり、u、w、x、y、z、qおよび100-u-w-x-y-z-qは質量%を示す)によって表され、
前記RHはR-T-B系焼結磁石の5質量%以下であり、
29.5≦u≦32.0 (2)
0.86≦w≦0.93 (3)
0.2≦x≦1.0 (4)
0.3≦y≦1.0 (5)
0.05≦z≦0.5 (6)
0≦q≦0.1 (7)
であり、かつ、
p=[B]/10.811×14-([Fe]/55.847+[Co]/58.933) (8)
([B]、[Fe]、[Co]は、それぞれB、Fe、Coの質量%を示す)のとき、
p<0 (9)
の関係を満足する。
本発明のR-T-B系焼結磁石は不可避的不純物を含むことができる。例えば、ジジム合金(Nd-Pr)、電解鉄、フェロボロンなどに通常含有される不可避的不純物を含有していても本発明の効果を奏することができる。不可避的不純物は、例えば、La、Ce、Cr、Mn、Siなどである。
上記組成により、一般的なR-T-B系焼結磁石よりもB量を低くするとともに、Ga等を含有させているので、上述した特許文献1~3と同様に、粒界にR-T-Ga相(およびR-T-Ga-Cu相)が生成される。その結果、Dyなどの重希土類元素をできるだけ使用せず、高いHcJを得ることができる。
上述の式(1)において、Tの含有量が「(100-u-w-x-y-z-q)」で示されていることからも分かるように、不可避的不純物(Alを除く不可避的不純物)は、Tの含有量の中に含まれる。本発明において、式(1)~(7)を満足するかどうかの判断は、高周波誘導結合プラズマ発光分光分析法(ICP-OES)を用いて、R、B、Ga、Cu、AlおよびM(NbおよびZr)、それぞれの含有量を測定し、u、w、x、y、zおよびqを求め、式「100-u-w-x-y-z-q」によりTの含有量を求めることにより行ってよい。また、式(8)および(9)を満足しているかは、高周波誘導結合プラズマ発光分光分析法(ICP-OES)を用いて、B、FeおよびCo、それぞれの含有量を求めてよい。
得られたR-T-B系焼結磁石素材を、450℃以上470℃以下の温度で4時間以上12時間以下加熱する。本発明の範囲で熱処理を行うことで、高いHcJが得られるとともに、熱処理時間によるHcJの変動を抑制することができる。熱処理温度や時間が本発明の範囲からはずれると、高いHcJが得られなかったり、熱処理時間が長すぎて生産性が低下する。特に熱処理時間が4時間未満であると、熱処理炉の記載位置によりHcJが変動する恐れがあり、さらに、高いHcJが得られない恐れもある。また熱処理時間が8時間を超えると生産効率が低下し、さらに、HcJが低下する恐れがある。好ましくは4時間以上8時間以下である。熱処理時間によるHcJの変動幅をよりいっそう抑制し、高いHcJを得ることができるからである。
さらに、前記加熱処理および前記熱処理工程は、焼結後に連続的に行ってもよい。例えば、成形体を1100℃で焼結後、460℃まで冷却した後、つづけて、460℃で6時間保持して熱処理工程を行ったり、成形体を1100℃で焼結後、800℃まで冷却した後、つづけて、800℃で2時間保持して加熱処理を行い、その後460℃まで冷却した後、さらにつづけて、460℃で6時間保持して熱処理工程を行ってもよい。
Ndメタル、Prメタル、電解Co、Alメタル、Cuメタル、Gaメタル、電解鉄(いずれも純度99%以上)およびフェロボロン合金を用いて、焼結後の組成が表1の組成となるように配合し、それらの原料を溶解してストリップキャスト法により鋳造し、厚み0.2~0.4mmのフレーク状の原料合金を得た。得られたフレーク状の原料合金を水素加圧雰囲気で水素脆化させた後、550℃まで真空中で加熱、冷却する脱水素処理を施し、粗粉砕粉を得た。次に、得られた粗粉砕粉に、潤滑剤としてステアリン酸亜鉛を粗粉砕粉100質量%に対して0.04質量%添加、混合した後、気流式粉砕機(ジェットミル装置)を用いて、窒素気流中で乾式粉砕し、粒径D50が4.0~4.6μmの微粉砕粉(合金粉末)を得た。なお、本検討では、粉砕時の窒素ガス中の酸素濃度は50ppm以下とすることにより、最終的に得られる焼結磁石の酸素量が0.1質量%前後となるようにした。なお、粒径D50は、気流分散式レーザー回折法による測定で得られる体積中心値(体積基準メジアン径)である。
R-T-B系焼結磁石素材の密度は7.5Mg/m3 以上であった。得られたR-T-B系焼結磁石素材の成分、ガス分析(O(酸素)、N(窒素)、C(炭素))の結果を表1に示す。なお、表1における各成分は、高周波誘導結合プラズマ発光分光分析法(ICP-OES)を使用して測定した。また、O(酸素)はガス融解-赤外線吸収法、N(窒素)はガス融解-熱伝導法、C(炭素)は燃焼-赤外線吸収法によるガス分析装置を使用して測定した。また、表1において、Nd、Prの量を合計した値がR量(u)である。以下の全ての表も同様である。また、表1には「q」を記載していないが、Nb量とZr量の合計がM量(q)である(後述する表7、13および19も同じ)。
Ndメタル、Prメタル、電解Co、Alメタル、Cuメタル、Gaメタル、電解鉄(いずれも純度99%以上)およびフェロボロン合金を用いて、焼結後の組成が表7の組成となるように配合し、実験例1と同様の方法で粗粉砕粉を作製した。得られた粗粉砕粉に対し、潤滑剤としてステアリン酸亜鉛を粗粉砕粉100質量%に対して0.04質量%添加、混合した後、気流式粉砕機(ジェットミル装置)を用いて、窒素気流中で乾式粉砕し、粒径D50が4.0~4.6μmの微粉砕粉(合金粉末)を得た。このとき粉砕時の窒素ガス中の酸素濃度を制御することにより、最終的に得られる焼結磁石の酸素量が0.1質量%前後となるようにした。なお、粒径D50は、気流分散式レーザー回折法による測定で得られる体積中心値(体積基準メジアン径)である。
Ndメタル、Prメタル、電解Co、Alメタル、Cuメタル、Gaメタル、電解鉄(いずれも純度99%以上)およびフェロボロン合金を用いて、焼結後の組成が表13の組成となるように配合し、実験例1と同様の方法で粗粉砕粉を作製した。得られた粗粉砕粉に対し、潤滑剤としてステアリン酸亜鉛を粗粉砕粉100質量%に対して0.04質量%添加、混合した後、気流式粉砕機(ジェットミル装置)を用いて、窒素気流中で乾式粉砕し、粒径D50が4.1~4.7μmの微粉砕粉(合金粉末)を得た。このとき粉砕時の窒素ガス中の酸素濃度を制御することにより、最終的に得られる焼結磁石の酸素量が0.1質量%前後となるようにした。なお、粒径D50は、気流分散式レーザー回折法による測定で得られる体積中心値(体積基準メジアン径)である。
前記微粉砕粉を実験例1と同様の方法で成形、焼結し、R-T-B系焼結磁石素材を得た。R-T-B系焼結磁石素材の密度は7.5Mg/m3 以上であった。得られたR-T-B系焼結磁石素材の成分、ガス分析(O(酸素)、N(窒素)、C(炭素))を実験例1と同様の方法で行った。その結果を表13に示す。
Ndメタル、Prメタル、電解Co、Alメタル、Cuメタル、Gaメタル、電解鉄(いずれも純度99%以上)およびフェロボロン合金、フェロニオブ合金、フェロジルコニウム合金を用いて、焼結後の組成が表19の組成となるように配合し、実験例1と同様の方法で粗粉砕粉を作製した。得られた粗粉砕粉に対し、潤滑剤としてステアリン酸亜鉛を粗粉砕粉100質量%に対して0.04質量%添加、混合した後、気流式粉砕機(ジェットミル装置)を用いて、窒素気流中で乾式粉砕し、粒径D50が4.0~4.5μmの微粉砕粉(合金粉末)を得た。このとき粉砕時の窒素ガス中の酸素濃度を制御することにより、最終的に得られる焼結磁石の酸素量が0.1質量%前後となるようにした。なお、粒径D50は、気流分散式レーザー回折法による測定で得られる体積中心値(体積基準メジアン径)である。
前記微粉砕粉を実験例1と同様の方法で成形、焼結し、R-T-B系焼結磁石素材を得た。R-T-B系焼結磁石素材の密度は7.5Mg/m3 以上であった。得られたR-T-B系焼結磁石素材の成分、ガス分析(O(酸素)、N(窒素)、C(炭素))を実験例1と同様の方法で行った。その結果を表19に示す。
Claims (3)
- 式uRwBxGayCuzAlqM(100-u-w-x-y-z-q)T(Rは軽希土類元素RLと重希土類元素RHからなり、RLはNdおよび/またはPr、RHはDy、Tb、GdおよびHoのうち少なくとも一種であり、Tは遷移金属元素でありFeを必ず含む、MはNbおよび/またはZrであり、u、w、x、y、z、qおよび100-u-w-x-y-z-qは質量%を示す)によって表され、
前記RHはR-T-B系焼結磁石の5質量%以下であり、
29.5≦u≦32.0、
0.86≦w≦0.93、
0.2≦x≦1.0、
0.3≦y≦1.0、
0.05≦z≦0.5、
0≦q≦0.1であり、かつ、
p=[B]/10.811×14-[Fe]/55.847-[Co]/58.933([B]、[Fe]、[Co]は、それぞれB、Fe、Coの質量%を示す)のとき、
p<0の関係を満足するR-T-B系焼結磁石素材を準備する工程と、
前記R-T-B系焼結磁石素材を450℃以上470℃以下の温度で4時間以上12時間以下加熱する熱処理工程と、
を含むR-T-B系焼結磁石の製造方法。 - 0.3≦x≦0.7、
0.5≦y≦0.7である、
請求項1に記載のR-T-B系焼結磁石の製造方法。 - 前記熱処理工程は、前記R-T-B系焼結磁石素材を450℃以上470℃以下の温度で4時間以上8時間以下加熱する請求項1または2に記載のR-T-B系焼結磁石の製造方法。
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