WO2007119271A1 - Aimant aux terres rares en couche mince et son procédé de fabrication - Google Patents

Aimant aux terres rares en couche mince et son procédé de fabrication Download PDF

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WO2007119271A1
WO2007119271A1 PCT/JP2007/000247 JP2007000247W WO2007119271A1 WO 2007119271 A1 WO2007119271 A1 WO 2007119271A1 JP 2007000247 W JP2007000247 W JP 2007000247W WO 2007119271 A1 WO2007119271 A1 WO 2007119271A1
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film
crystal
alloy
rare earth
thin film
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PCT/JP2007/000247
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English (en)
Japanese (ja)
Inventor
Kenichi Machida
Shunji Suzuki
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Namiki Seimitsu Houseki Kabushiki Kaisha
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Priority to JP2008510732A priority Critical patent/JP4988713B2/ja
Publication of WO2007119271A1 publication Critical patent/WO2007119271A1/fr

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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
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
    • H01F10/126—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing rare earth metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/26—Thin magnetic films, e.g. of one-domain structure characterised by the substrate or intermediate layers
    • H01F10/265—Magnetic multilayers non exchange-coupled

Definitions

  • the present invention relates to a thin film rare earth magnet suitable for micromachines and sensors, small medical and information equipment, and a method for manufacturing the same. More specifically, the present invention relates to a high performance thin film rare earth magnet having a large coercive force and a method for manufacturing the same.
  • Nd_Fe_B rare-earth sintered magnets have very high magnetic properties compared to conventional Ferri magnets, so they have VCM (voice coil motor), MR I (magnetic tomography equipment) Used in various fields such as various motors.
  • the magnets used for these are generally flat or cylindrical shapes with a side of several to tens of millimeters, but mobile phone vibration motors have an outer diameter of 3 mm and a wall thickness of about 1 mm. Cylindrical magnets are used, and smaller magnets are required in the micromachine and sensor fields.
  • powder molding is difficult to produce a sintered body with a thickness of 1 mm or less. Even in the method of cutting and polishing after manufacturing a large sintered body block in advance, it is extremely difficult to obtain a magnet with a thickness of 0.3 mm or less due to problems with magnet strength and production processing technology. .
  • a thin film magnet is sintered by depositing a magnet alloy component on a substrate or a shaft in a vacuum or reduced pressure space and applying heat treatment to appropriately control various conditions.
  • thinner-film magnets are applied to actual devices, smaller devices are often required to have higher-performance magnet characteristics, and the devices can be used stably for a long time in various environments.
  • coercive force 1.5 MAZm or more, preferably 2 MAZm or more, in addition to improving the maximum energy product and remanent magnetization.
  • Fig. 1 shows the temperature dependence of the remanent magnetization (B r) and coercive force (H c j) of a typical N d_F e_B magnet. From Fig. 1, it can be seen that N d_F e_B magnets have the essential problem that the magnetic properties greatly decrease with increasing temperature, and in particular, the rate of decrease in coercive force is large. Therefore, when N d _ F e _B system magnets are used for small motors, etc., the motor temperature easily rises to 60 to 80 ° C due to heat generated from the coil when energized. In order to reduce the influence of the decrease in magnetic properties due to temperature rise to reach hundreds of degrees Celsius, increasing the coercive force at room temperature is an essential issue for industrial applications. .
  • a thin film magnet formed on a substrate such as a flat plate or a shaft grows the C axis of the N d 2 F e 14 B crystal in the thickness direction, and is magnetized in this film thickness direction.
  • the thin film magnet has a thin film thickness of about several tens of meters / m to several tens of meters, and is a few tenths to one hundredth of the length of the four sides of the flat plate and the shaft diameter.
  • Non-Patent Document 2 the remanent magnetization of this thin film is as low as about 0.7 T and the film thickness is 1 m or less. There is a problem in practical use because magnetic flux cannot be obtained.
  • the inventors of the present invention first, from the surface of the N d_F e_B based sintered magnet, N d 2
  • N dF e _ B thin film magnets N d 2 F e 4 B crystal grains are made larger than the single domain grain size, and a grain boundary phase is formed.
  • a thin film magnet with H cj of 1.5 MAZm and excellent magnetism has been obtained (Patent Document 4).
  • Patent Document 5 There is a report example (Patent Document 5) of producing an exchange spring magnet in which Nd-Fe-B and Fe are laminated for a thin film-laminated magnet. As a result, the coercive force is reduced and the N d 2 F e 4 B crystal grain size is less than 1 m. Furthermore, there is a report example of a thin-film magnet in which N d_F e_ B and Ta are laminated (Non-patent Document 3). In this example, the use of Ta improves the orientation of the N d 2 F e 14 B crystal. Therefore, there is no effect of improving the coercive force, and its value is as small as 0.9 MAZm.
  • Patent Document 1 Japanese Patent Laid-Open No. 8-83713
  • Patent Document 2 Japanese Patent Laid-Open No. 11-288812
  • Patent Document 3 JP 2005-011973
  • Patent Document 4 WO 2005/091 31 5 A 1 Publication
  • Patent Document 5 Japanese Patent Laid-Open No. 11-214219
  • Non-Patent Document 1 Journal of Japan Society of Applied Magnetics, 27, 10, 1 007, 2003 Year
  • Non-Patent Document 2 Journal of Applied Physics. Vol. 98, 1 1 3905, 20 05
  • Non-Patent Document 3 IEICE Technical Committee Materials, MAG-03-03, 2003, Invention Disclosure
  • N d 2 F e 14 B compounds have high saturation magnetization and high magnetocrystalline anisotropy, high remanence and relatively large coercive force have been obtained in the form of sintered magnets and thin film magnets.
  • Thin-film magnets are generally composed of N d 2 Fe 14 B crystal grains of approximately 0.3 U m or less, which corresponds to a single domain particle diameter.
  • the raw material alloy has a magnetic anisotropy greater than Nd, such as Dy.
  • the present inventors have determined that the N d_F e_B alloy film and M or M Alloy (However, M is one or more of Pr, Dy, Tb, and Ho) After stacking the films, heat treatment is performed, so that M element partially replaces Nd and becomes solid solution ( N d, M) 2 F e 14 B crystals formed on the surface, N d 2 F ei 4 B3 ⁇ 4i ⁇ ⁇ and N d 2 “ei 4 B crystal grain boundaries (N d, M) 2 In a thin-film magnet composed of a grain boundary phase (or simply called “grain boundary phase”) composed mainly of M element formed in contact with the interface between the e 14 B strand and the B crystal, the decrease in residual magnetization is extremely small and maintained. It has succeeded in providing a thin-film magnet with a remanent magnetization of
  • the present invention is as follows. (1) M or M alloy (where M is one or more of Pr, Dy, Tb, and Ho) Three layers in which films and Nd_Fe_B alloy films are alternately stacked A thin-film rare earth magnet obtained by heat-treating the above laminated structure and interdiffusing the M or M alloy component and the Nd-Fe-B alloy component,
  • the heat element M by the surface portion of the Li N d 2 F e 4 B crystal grains process is dissolved by replacing the N d (N d, M) 2 F e 14 B crystals are formed, and N d
  • N d A thin film rare earth characterized in that a crystal grain boundary phase made of M or M alloy is formed at the interface of (N d, M) 2 F e 14 B crystal at the grain boundary of 2 F e 14 B crystal grain magnet.
  • N d 2 F e 14 B crystal phase is formed in layers in the thickness direction of the thin film, and the (N d, M) 2 F e 14 B crystal is in contact with the interface between the crystal phases.
  • N d 2 F e 14 B crystal phase is formed in layers in the thickness direction of the film, around the N d 2 F ei 4 B Yui ⁇ Yo (N d, 2 F "e 14 B crystal and an interface A thin film rare earth magnet as described in (1) above, wherein a grain boundary phase made of M or an M alloy surrounding N d 2 F "e 14 B crystal grains is formed.
  • the N d_F e_B alloy is composed of an N d 2 F e 14 B compound, the content of M element in the thin film is 1 to 30% by mass, and the total content of N d and M element
  • N d_F e_B alloy and M metal or alloys thereof by physical film-forming method in a vacuum container are alternately laminated, and then heat-treated at 700 to 1100 ° C to mutually diffuse the M or M alloy component and the N d _Fe _ B alloy component.
  • the element M is substituted with N d to form a solid solution (N d, M) 2 F e 14 B crystal on the surface of the N d 2 F e 14 B crystal grains, and N d 2 F
  • N d, M solid solution
  • a grain boundary phase composed of M or an M alloy is formed at the grain boundary of e 14 B crystal in contact with the (N d, M) 2 F e 14 B crystal interface.
  • N d _ F e-B alloy film is 0.05 m to 50 m, and the film thickness ratio of N d _ F e _B alloy and M metal or its alloy is 99 : 1-60
  • an N d_F e_B film and an M metal such as Dy or an alloy thereof are alternately stacked to form an M metal or an M alloy as N d -F e.
  • an M alloy such as Dy or an alloy thereof
  • thermal diffusion to _ B based film around part of a solid solution by substituting the N d to N d 2 F e 4 B crystal grains formed, many of the remainder the crystal grains of the element M
  • a grain boundary phase is formed between the Z and N d 2 F e 14 B crystal phases.
  • a part of N d that easily diffuses in the N d_F e_B film diffuses into the M metal or M alloy film.
  • this crystallographic structure involves 600 ⁇ 50 ° C and 700 ° C, which causes crystallization and improved orientation and diffusion of M element in a state where the thin film magnet is highly oriented perpendicular to the substrate. It is desirable to perform two-stage heat treatment in the high temperature region of ⁇ 1100 ° C, more preferably 900 ⁇ 1100 ° C, which is larger than the conventional single domain grain size (0.3 m) of N d 2 F e 14 B. N d 2 Fe 14 B crystal grains of about 5 m to 30 m, more preferably about 1 m to 5 m are formed by heat treatment to have a magnetization mechanism similar to that of a sintered magnet. It has the effect of improving magnetism, which is important for attaching thin film magnets to equipment.
  • FIG. 1 is a diagram showing the relationship between the magnetic properties and temperature of an N d-F e _B magnet.
  • FIG. 2 is a schematic diagram showing the structure of the crystal phase, crystal grains, and grain boundary phase of the thin film rare earth magnet of the present invention.
  • A Floor plan
  • B A cross section in the film thickness direction
  • FIG. 3 Drawing SEM image of the sample (6) of the present invention.
  • FIG. 4 X-ray diffraction patterns of the sample of the present invention (3) and the comparative sample (1).
  • FIG. 6 is a relationship diagram of magnetic characteristics with respect to film thickness of the samples (24) to (30) of the present invention and the samples of comparative examples (12) to (13).
  • the thin-film magnet targeted by the present invention is made of an N d_F e_B alloy, and generally consists mainly of an N d 2 Fe 14 B crystal phase containing N d, F e, and B as essential component elements.
  • Nd used for alloy production may contain other rare earth elements such as Ce and Pr as impurities or up to about 5% by mass to reduce raw material cost. It also contains inevitable impurities derived from thin film constituent materials and film formation and heat treatment processes.
  • the N d 2 F e 14 B crystal grains of the thin film magnet such as for or Curie temperature toward the upper to miniaturization, a portion of the F e components Co, N i, T i, V, C Replacement with one or more elements of r, Cu, AI, Zn, Ga, V, Mo, Nb, Ta, W is performed.
  • the amount of substitution for Fe varies depending on each element.
  • Cu and Mo are effective for uniformizing and refining the grain size with a substitution amount of about 1% by mass. The effect of improving the Curie temperature by about 100 ° C with a mass% substitution amount.
  • N d_F e_B rare earth alloys cannot avoid the incorporation of impurities such as oxygen and carbon during raw material refining, film formation, and heat treatment. It is beneficial.
  • the M element in the M or M alloy crystal phase laminated with the N d 2 F e 14 B crystal phase is guaranteed to be one or more of Pr, Dy, Tb, and Ho. Necessary for improving magnetic force. The reason is that the magnetocrystalline anisotropy of the R 2 F e 14 B compound when R is a rare earth element is greater than when R is N d when R is Pr, Dy, T b, and Ho.
  • M elements are a single M metal and M alloy, that is, alloys obtained by mixing two or more of Pr, Dy, Tb, and Ho that can be obtained by using various film forming methods, and M metal and An alloy with other elements such as Fe and Co, and containing an M element of about 10% by weight or more, preferably about 50% by weight or more, can be used in consideration of magnetic properties and corrosion resistance.
  • the basic structure of the thin film targeted in the present invention has a structure in which N d 2 Fe 14 B crystal phases and M or M alloy crystal phases are alternately laminated in the thickness direction of the thin film. It is essential that each layer has one layer on the front and back, or one layer on the front and back, and the former has at least three layers each on the front and back. Even hundreds of layers are acceptable.
  • FIG. 2 is a schematic diagram showing a typical example of a thin film configuration.
  • 2 (a) is a thin film of perspective, (b) the thickness direction of the A cross-sectional view of a thin film, (c) is a plan view of the N d 2 F e 14 B crystal phase portion of the lower surface B.
  • an Nd_F6_8 film with a thickness of 1 m to 2 m and a 1 ⁇ 1 film with a thickness of 0.1 m to 0.2 were laminated and a thin film with a total thickness of 50 was heat-treated. It is a schematic diagram in such a case.
  • the number of crystal grains is about one per layer in the thickness direction of the film, but if the thickness of the N d_F e_B film is 10 m, for example, several N d 2 F e 14 in the thickness direction In this case, the coercive force and c-axis orientation are slightly reduced. If the N d_B_F e system film and M metal or M alloy film are alternately formed, each film consists of amorphous or fine crystals of 1 fjl m or less, but after heat treatment, it is shown in Fig. 2 (b) and Fig. 2 ( c) As shown in Fig.
  • N d 2 F e 14 B crystal grain 1 is surrounded by a grain boundary phase 2 made of M metal or M alloy, and the surface portion of N d 2 F e 14 B crystal grain 1 is
  • the M component of the M metal or M alloy is (Nd, M) 2 Fe 14 B crystal 3 in which the M component is mutually substituted and partially dissolved.
  • Figure 2 (c) shows a structure in which N d 2 F e 14 B crystal grains 1 are arranged almost randomly.
  • the lower and upper diagrams in Fig. 2 (b) show the stacking of N d 2 F e 14 B crystal grains 1 respectively.
  • the structure of the thin film consists of a grain boundary phase 2 made of M metal or M alloy upward from the lower layer, N d 2 F e 14 B crystal grain 1, M metal or M alloy. It has a five-layer structure consisting of grain boundary phase 2, N d 2 Fe 14 B crystal grain 1, crystal grain boundary phase 2 made of M metal or M alloy.
  • FIG. 2 (b) shows that the M metal or M alloy film is relatively thin, and the amount ratio of N d 2 F e 14 B and (N d, M) 2 F ei 4 B to the total film thickness is
  • This shows a structure in which the grain boundary phase 2 made of M or M alloy is arranged between the layers of the N d 2 F e 14 B crystal phase, and N d 2 F e 4 B and the total film thickness
  • the upper diagram of FIG. 2 (b) shows a structure in which a grain boundary phase 2 made of M or an M alloy is arranged around the N d 2 F e 14 B crystal grain 1 and between the crystal phases.
  • the lower limit of the content of Nd and M elements is 26.7% by mass and at least 0.3% by mass, that is, about 27% by mass. % Or less, and below that, the grain boundary phase composed of M metal or M alloy becomes relatively very thin, or Of-Fe precipitates in the thin film. It becomes substantially difficult to obtain a coercive force improving effect.
  • N d_F e_B system or a small amount of N d Ritsuchi grain boundary phase by the N d amount of 27 mass% or more in the film is formed around the N d 2 F e 14 B crystal grains, or M
  • a small amount of Nd coexists in the grain boundary phase made of metal or M alloy.
  • the improvement rate of the coercive force is only a few percent, and the effect of the present invention is extremely small.
  • the coercive force is greatly improved as the M element content in the entire thin film is increased by increasing the film thickness of the M metal or M alloy film relative to the N d_F e_B film.
  • the total content of Nd element exceeds 450/0, and the residual magnetization is greatly reduced as described above, so the content of M element in the entire thin film is 1 It is necessary to make it -30 mass%.
  • the average crystal grain size needs to be in the range of 0.5 m to 30 m, and in order to obtain a large coercive force, it is more preferably 1 m to 10 m.
  • the average crystal grain size is determined from the average size of the crystal cut from multiple directions.
  • N in which the Tb element of the sample of the present invention (6) is partially dissolved.
  • the d 2 F e 14 B crystal has a crystal grain size of approximately 2 m when viewed from the SEM (scanning electron microscope) image of the thin-film fracture surface in Fig. 3.
  • the crystal grain size was 3 m to 4 m. Therefore, since it is difficult to accurately measure the irregular crystal grain size in the thin film, in this specification, it is within the range of 50 m ⁇ 50 m at any part of the crystal observed in the film cross section or in the film surface.
  • the average size of the diameters of all crystal grains is expressed as the average crystal grain size.
  • the effect of the present invention can be sufficiently exerted when the thickness of the thin film rare earth magnet of the present invention is in the range of 1 m to 300 m. Less than Nd 2 F e 14 B crystal phase is formed only in the thickness direction of the thin film, and M around the N d 2 F e 4 B crystal grain and / or between the crystal phase M Alternatively, it is difficult to form a structure in which grain boundary phases made of M alloy are arranged, and the coercive force required for application as a machine or sensor in various application devices is insufficient.
  • the thickness of the film is preferable for increasing the coercive force.
  • the thickness exceeds 300 m, the orientation of the crystal deteriorates between the lower and upper portions of the thin film, and the residual magnetization decreases, and There is a problem that the smoothness of the thin film surface is deteriorated, and that the film forming operation needs to be operated for a long time of about 1 mm or more.
  • a thickness of more than 300 m can be obtained relatively easily by cutting and polishing the sintered magnet, so that the thickness exceeding this thickness has a small advantage in producing a thin film magnet. More preferably, it is in the range of 10 m to 300 m, more preferably in the range of 20 m to 200 m.
  • a so-called physical film forming method in which an element component constituting a thin film is formed on various base materials in a vacuum container can be used. Specific methods include vapor deposition, sputtering, ion plating, laser deposition, CVD, and coating in which fine alloy powder particles are applied or sprayed. These physical film formation methods are suitable as a film formation method for Nd_Fe_B-based thin films because a high-quality crystalline film can be obtained with few impurities.
  • Nd_Fe_B By preparing each target of alloy and Dy metal and transferring or rotating the base material or target, N d_F e_B film and Dy film can be alternately formed to obtain a film having a laminated structure .
  • the thickness of the former layer is more preferably about 0.05 m to 50 m. Is about 0.3 m to 10 m , and the film thickness ratio of the former and the latter is preferably 99: 1 to 60:40, and more preferably 97: 3 for obtaining a high coercive force while maintaining high remanent magnetization. ⁇ 75: 25, more preferably 95: 5 to 85:15.
  • each film is a base material ZDy / N d_F e_B / Dy or a base material ZN d_F e_B / Dy / N d_F e_B, and the number of laminations can be arbitrarily set to several to several hundred times.
  • the base material for forming the thin film various metals, alloys, glass, silicon, ceramics and the like can be selected and used. However, in order to obtain the desired crystal structure, it is necessary to perform heat treatment at a high temperature of 600 ° C or higher, and ceramics and metals with relatively high melting points such as Fe, Mo, and Ti are selected as the metal substrate. It is desirable to do this.
  • the demagnetizing field applied to the thin film magnet is reduced, so that the use of magnetic metals and alloys such as Fe, magnetic stainless steel, and Ni is also suitable.
  • a ceramic substrate is used, the resistance to high-temperature processing is sufficient, but the adhesion to the Nd_Fe_B film may be insufficient, and as a countermeasure, a base film such as Ti or Cr is provided. In many cases, these base films are effective even when the base material is a metal or an alloy.
  • N d -Fe-B single-layer films formed by sputtering or the like are usually composed of amorphous crystals or fine crystals of about several tens of nanometers. Therefore, conventionally, to obtain 500 to 650 ° C low-temperature heat treatment by crystallization and crystal growth by promoting an average grain size of 0.5 about 3 m of N d 2 F e 14 B crystal phase.
  • the M element of the M or M alloy film enters the N d 2 F e 14 B crystal grains. Is diffused and substituted with N d to form a solid solution, and the grain boundary phase made of M or an M alloy is surrounded by and / or around the N d 2 F e 14 B crystal grains.
  • the M element diffuses into the N d 2 F e 14 B crystal grains and replaces a part of the N d element, and at the same time, the N d component dissolves with the M element of the M or M alloy film. Diffusion proceeds in the laminated film. If it is less than 100 ° C, it takes several tens of hours to diffuse the M element, which is not practical and it is difficult to obtain a desired crystal structure. When the temperature exceeds 700 ° C, diffusion of M element into N d 2 F e 4 B crystal grains, growth of N d 2 F e 14 B crystals, and generation of crystal grain boundary phases consisting of M or M alloys proceed.
  • the heat treatment temperature is preferably 700 to 110 ° C.
  • the heat treatment needs to be performed in a vacuum or non-oxidizing atmosphere to prevent oxidation of the thin film surface.
  • a heating method a method of loading a thin film sample into an electric furnace, infrared heating or laser Rapid heating and cooling method by irradiation, and thin A Joule heating method for directly energizing the membrane can be appropriately selected and employed.
  • the film formation and the heat treatment separately because it is easy to control the crystallinity and magnetic properties of the thin film, but the substrate is heated to a high temperature during the sputtering.
  • the temperature during film formation at 400 ° C or higher, preferably 700 ° C or higher by increasing the output during film formation, the desired crystal structure can be created. It is.
  • the N d_F e_B film is easily rusted, it is common to form a corrosion-resistant protective film such as Ni or Ti after film formation or after heat treatment.
  • RF sputtering equipment decompression vessel (chamber one) N d_F e_B alloy A disk target is attached to the upper part, and two Mo substrates are placed on the SUS flat plate with a built-in heater on the lower side. Arranged side by side. After evacuating the inside of the sputtering apparatus to the 5 X 1 0- 5 P a, the reactor was kept in pressure by introducing A r gas to 1 Pa
  • the Mo substrate is reverse-sputtered to remove the surface oxide film, and then the heater was heated to maintain the temperature of the SUS flat plate surface at 400 ° C, and an RF output of 20 OW and a DC output of 30 OW were applied to form a 6 m thick N d _ F e _ B single layer film. .
  • the obtained monolayer film was taken out from the chamber.
  • N d _ F e_B alloy A disk target and T b target are mounted facing each other at 180 degrees, and each target is rotated alternately. Then, successively, T b with a thickness of 0.2 m and N d-F e _B with a thickness of 1.8 tl m were repeatedly formed, and T b / N d _ F e_B / T b / N d _ F A multilayer film of e_B / T b / N d _F e_B / T b with a total thickness of 6.2 m was manufactured. The obtained laminated film was taken out from the chamber.
  • the monolayer film and the laminated film obtained by the above method were loaded into a tubular electric furnace, and each was heat-treated for 10 minutes in an Ar gas stream maintaining an oxygen concentration of 5 ppm or less. It was.
  • the heat-treated sample (2) at 800 ° C was subjected to low-temperature heat treatment at 550 ° C, 600 ° C and 650 ° C for 30 minutes each, and a predetermined heat treatment at that temperature (800 ° C, 10 ° C). (2 '). (2' ') and (2' '') were also prepared.
  • Table 1 shows the film formation, heat treatment conditions, and magnetic properties.
  • Samples (1) to (5) of the present invention were heat-treated at 700, 800, 900, 1000, and 1100 ° C, respectively.
  • the heat treatment for crystallization can be performed at 400 ° C. to 650 ° C., but 600 ° C. is preferable from the viewpoint of improving the distribution in the C-axis direction.
  • each sample was measured using a superconducting VSM (vibrating sample magnetometer) and applying a magnetic field of ⁇ 6 T perpendicular to the film surface. Thereafter, the alignment direction of performing X-ray diffraction N d 2 F e 14 B crystals of each sample, and the multilayered sample was examined solid solution state into N d 2 F e 14 B crystal grains of T b element . Furthermore, after lightly etching the surface of each sample with alcoholic nitrate, the film surface was observed with a scanning electron microscope (SEM), and the average crystal grain size was determined from the image by the measurement method described above.
  • SEM scanning electron microscope
  • Table 2 shows the relationship between the heat treatment temperature, average crystal grain size, and magnetic properties of each sample.
  • the average crystal grain size is 0.1 m
  • the coercive force is 784 k AZm
  • the residual magnetization is 1 29 T showed.
  • the comparative sample (1) and the comparative sample (2) obtained by heat-treating the N d_F e_B single layer film are both single-domain of the N d 2 F e 14 B compound with an average grain size.
  • the coercive force was as low as around 700 k AZm, close to 0.3 m corresponding to the particle size.
  • the average crystal grain size of the N d 2 Fe 14 B compound is 0.5 m to 28 m by the high-temperature heat treatment.
  • the coercive force is 1 060 k due to the partial solid solution of the Tb element in the N d 2 F e 14 B crystal grains and the formation of a grain boundary phase mainly composed of T b.
  • the value of the sample of the present invention (3) was 1 730 kA / m, which was 2.4 times that of 724 kA / m of the comparative sample (1).
  • the residual magnetizations of the samples (1) to (5) of the present invention are 1.26 to 1.32T, which is not lower than that of the comparative sample (1), the Tb element Most of them are considered to contribute mainly to the formation of the grain boundary phase without being dissolved in the N d 2 F e 14 B crystal grains.
  • the reason why the decrease in remanent magnetization is small or slightly increased is that the decrease in remanent magnetization is suppressed as a result of the improvement in the squareness of the demagnetization curve as the coercive force increases significantly. .
  • FIG. 4 shows the X-ray diffraction patterns of the comparative sample (1) and the inventive sample (3).
  • the position of the diffraction peak on the (006) plane of N d 2 F e 14 B when the C U-KQ? Line is applied to the sample surface is 44.4 degrees in the comparative sample.
  • the sample of the present invention is shifted to 44.7 degrees. this is
  • T b I N d of Li atomic radius forms a solid solution by substituting a part of the N d atoms N d 2 F e 4 B grains, diffraction lines at high angle side shrinks crystal lattice This means that the Tb element in one of the Tb films in the multilayer film has caused a diffusion reaction with the other NdF e-B film.
  • Nd and Tb element contents (% by mass) in the thin film were determined according to the comparative sample (1) for the monolayer film and the comparative sample (3), and the inventive sample (3 ) was measured by X-ray fluorescence analysis, and the results were as follows.
  • a single layer film of N d_F e _ B alloy with a thickness of 3 m was fabricated as a comparative sample 6 in the same manner as in Example 1 except that the RF output was changed to 15 OW and the DC output was changed to 25 OW. Further, in the same manner, a Tb metal having a thickness of 0.2 m and an N d_F e_B alloy having a thickness of 0.8 m were repeatedly formed as Sample 6 of the present invention, and T b / N d -F eB / T A multilayer film of b / N dF eB / T b / N dF eB / T b was fabricated.
  • the obtained monolayer film and laminated film are loaded into a tubular electric furnace, respectively, and Ar gas Heat treatment was performed for 10 minutes in the air stream.
  • the film formation and heat treatment conditions are shown in Table 3.
  • the magnetic properties of the sample obtained in the same manner as in Example 1 were measured by VSM, and the average crystal grain size was measured by SEM.
  • Table 4 shows the relationship between the average crystal grain size of each sample and the magnetic properties. From Table 4, the present invention samples (5) to (7) have higher coercive force and larger energy volume than the comparative sample (6). It has been clarified that even if any of Tb, Dy, and Pr is laminated, the magnetic properties are greatly improved.
  • N d_F e- B alloy (alloy A) target used in Example 1 the internal pressure of the device is 3 Pa, the temperature of the SUS flat plate surface is 350 ° C, and 3 “output is 100, DC output is A 25-m-thick N d_F e_B single-layer film was fabricated in the same manner as in Example 1, except that 25 OW was used, and 90% D y _ 1 0 instead of the T b target used in Example 1.
  • Alloy target with% Co composition (unit: mass%)
  • Dy_Co metal with a thickness of 0.01 m to 0.8 m and Nd-Fe_B alloy with a thickness of 2 m were sequentially deposited 10 times each, and Dy_Co and Nd A multilayer film of _F e _B was manufactured.
  • the obtained single-layer film and a laminated film was loaded into a vacuum furnace which is evacuated below each 2 X 1 0_ 4 P a, a heat treatment was carried out for 30 minutes.
  • Table 5 shows the film formation and heat treatment conditions.
  • a heat-treated single layer film was used as a comparative sample (7).
  • the Dy-Co film thickness is 0.0 1, 0, 02, 0.05, 0.1, 0.2, 0.4, 0.6, 0.8 m.
  • the comparative sample (8), the inventive samples (9) to (14), and the comparative sample (9) were used.
  • the magnetic properties of each sample were measured by VSM, and the contents of Nd and Dy were determined by fluorescent X-ray analysis.
  • Table 6 shows the N d _F e _B / D y _C o laminated sample with respect to the D y—Co film thickness.
  • Example 5 shows a graph of the relationship between the magnetic properties and the Dy—Co film thickness in comparison with the N d — F e — B single layer film sample. From Table 6, it can be seen that compared to the single layer film comparative sample (7), the laminated film samples (9) to (14) have a significantly increased coercive force due to the introduction of Dy and a decrease in residual magnetization. It became clear that it was small, and it was found that good magnetic properties could be obtained not only with Dy metal but also with Co. However, the comparative sample (8) with a very thin D y—Co film of 0.01 m did not show an effective increase in coercive force because the Dy content was less than 1% by mass. . In addition, the comparative sample (9) whose Dy_Co film thickness is too thick exceeded 30% by mass in the preferred Dy content range, and the total content with Nd also exceeded 45% by mass. And the increase in coercive force stagnated.
  • a disk-shaped alloy target with 28% N d _1.0% B—balance Fe (unit: mass%) with a diameter of 4 Omm Co, Cr, Cu, AI, V, and Nb metal pieces, each of which is a square piece with a side of 5 mm on the alloy target, are selected as appropriate. Then, a predetermined number was loaded. Also, a Ta substrate 8 mm long, 5 mm wide, and 0.3 mm thick after solvent degreasing and acid cleaning was fixed on the alumina substrate using a mounting jig.
  • the N d: Y AG laser was irradiated to the N d_F e_B target to produce a single layer film on the Ta substrate.
  • the obtained monolayer film was taken out from the chamber.
  • the Nd_Fe_B target loaded with the Tb target and Cu metal pieces was irradiated with laser alternately for a predetermined time to dissociate and release the Cu element, and a laminated film was produced on the Ta substrate.
  • the obtained laminated film was taken out from the chamber.
  • the metal pieces were sequentially changed to AI, V, Nb, Cr, and Co, and a laminated film was fabricated on the Ta substrate.
  • the addition amount was adjusted according to the number of metal pieces used. For example, the amount of added metal In the case of 2% by mass, one metal piece was used, and in the case of 5-6% by mass, 3 metal pieces were used.
  • the distance between the target and the substrate is 25 mm
  • the laser output is constant
  • T b is 0.3 m
  • N d_F e_B-X where X is Co, C r, Cu
  • the additive metal selected from AI, V, Nb, and W was 1 m, each layer was stacked to form 20 layers, and finally Tb was formed to produce a total of 21 layers.
  • Table 8 shows the magnetic characteristics when the single-layer film and the laminated film containing the additive metal are heat-treated. From Table 8, the sample of the present invention (15) to (23) of the laminated film is approximately 2 to 3 times the coercive force even when each additive metal is introduced, compared with the comparative sample (10) of the single layer film. Part of the added metal is dissolved in the N d 2 F e 14 B crystal grains, and the other is dissolved in the grain boundary phase, or a coercive force is formed by forming a compound. It is presumed that this was effectively improved.
  • the sample containing Co shows a sufficiently large value although it has a slightly smaller coercive force than other additive metals, and improves the Curie temperature as another effect.
  • the Co content is about 35% by mass as in the comparative sample (11)
  • the coercive force decreases greatly, so the content of these added metals is preferably within a range not exceeding 30% by mass.
  • the reason why the values of remanent magnetization in Table 8 are all less than 1 T is that Nd 2 Fe 14 B crystals are isotropically dispersed in the film as a result of X-ray diffraction analysis of each sample. This is probably because the Ta substrate during film formation was not heated.
  • an alumina shaft having a diameter of 0.6 mm and a length of 12 mm was used as a base material.
  • a known three-dimensional sputtering apparatus was used as the sputtering apparatus. The configuration and principle of this three-dimensional sputtering apparatus are disclosed in Japanese Patent Publication No. 2004-304038.
  • a Cu coil for high frequency generation was placed in the middle of the opposing Tb target, and an Nd_Fe-B target and a Cu coil were also placed in the right chamber.
  • An alumina shaft was attached to the tip of the motor rotating shaft extending from the left side to the right side.
  • the shuff rod is first positioned at an intermediate position between the opposing Tb targets, and a film having a thickness of 0.2 is formed under the same rotational speed and film deposition output as those of Comparative Example Sample 12.
  • Bow I then the motor mounting rod is automatically moved to the right to position the shaft N in the middle of the N d_F e_B target, and a 0.8 m thick N d _F e_B film is deposited,
  • the shaft was again transferred to the left to form a 0.2 m thick Tb film to produce a laminated film with a total thickness of 1.2 m.
  • the number of layers was increased by the same method, and each layered film with total thickness of about 5, 10, 40, 80, 160, 280, 360 m was manufactured.
  • the heat treatment of the laminated film is made according to the samples of the present invention (24) to (30) in the order of film thicknesses of 1.2, 5, 10, 40, 80, 160, 280 m.
  • the sample with m was used as a comparative sample (13).
  • the deposited cylindrical shape The magnetic properties were measured by VSM while sweeping the magnetic field in the radial direction of the sample.
  • Figure 6 shows the relationship of the magnetic properties with respect to the total film thickness of single-layer films and laminated films. From Fig. 6, regarding the film thickness of 80 m, the decrease in the remanent magnetization in the sample of the present invention (2 8) of the laminated film is different from the comparative sample (1 2) of the single layer film indicated by the black mark in the figure. Even slightly, the coercive force increased significantly.
  • all of the samples (24) to (30) of the present invention have a high coercive force while maintaining a relatively high remanent magnetization, and are sufficiently applicable for driving micro motors and the like. Magnetic properties were obtained. However, when the total film thickness is 3600 m, a decrease in crystallinity and a decrease in magnetic properties due to disorder of crystal orientation are observed. Therefore, the total thickness is preferably set to 300 m or less.
  • the present invention provides a thin film permanent magnet having a desired high coercive force and high performance based on the above-mentioned strong demand.
  • the device By being mounted on various application devices such as a micromachine, the device has a high output and a small size. It greatly contributes to the realization of heat-resistant stability in various usage environments based on high coercive force characteristics.
  • the thin film permanent magnet of the present invention can obtain a high coercive force and, at the same time, a crystal phase composed of N d 2 F e 14 B crystal grains having a relatively large crystal grain size and / or around the crystal grains.
  • the magnetic structure is improved by the composite structure of the grain boundary phase of M or M alloy existing between the crystal phases, and the use in the applied equipment becomes easy.

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Abstract

La présente invention propose un aimant aux terres rares en couche mince ayant une force coercitive magnétique accrue de façon significative tout en supprimant une baisse de la magnétisation résiduelle de l'aimant en couche mince. Cet aimant est un aimant en couche mince de 1 mm à 300 mm d'épaisseur fabriqué en traitant thermiquement une structure stratifiée ayant une structure multicouches. Dans cette structure, une couche de M ou d'alliage de M, dans laquelle M représente au moins deux de Pr, Dy, Tb et Ho, et une couche d'alliage à base de Nd-Fe-B de 0,05 μm à 50 μm d'épaisseur ont été empilées en alternance de trois couches ou plus. Lors du traitement thermique, le composant de M ou d'alliage de M et le composant d'alliage à base de Nd-Fe-B ont été mutuellement diffusés. En outre, lors du traitement thermique, un cristal (Nd, M)2Fe14B est formé sur la partie de surface des grains cristallins Nd2Fe14B. Le cristal (Nd, M)2Fe14B a été produit suite au remplacement de Nd par l'élément M et la dissolution du Nd remplacé dans une solution solide. En outre, une phase de joint de grains cristallins de M ou d'alliage de M est formée dans le joint des grains cristallins Nd2Fe14B, de sorte que l'interface de la phase de M ou d'alliage de M soit en contact avec le cristal (Nd, M)2Fe14B.
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JP2008071904A (ja) * 2006-09-13 2008-03-27 Ulvac Japan Ltd 永久磁石及び永久磁石の製造方法
JP2008172037A (ja) * 2007-01-12 2008-07-24 Daido Steel Co Ltd 希土類磁石及びその製造方法
WO2011030409A1 (fr) * 2009-09-09 2011-03-17 信越化学工業株式会社 Rotor pour machine rotative de type à aimants permanents
JP2011130522A (ja) * 2009-12-15 2011-06-30 Minebea Co Ltd 微小回転電気機械の磁気回路
WO2011103104A2 (fr) * 2010-02-17 2011-08-25 Electron Energy Corporation Aimants composites et stratifiés en terre rare présentant une résistivité électrique accrue
WO2013103132A1 (fr) * 2012-01-04 2013-07-11 トヨタ自動車株式会社 Aimant nanocomposite de terres rares
US8638017B2 (en) 2009-09-18 2014-01-28 Shin-Etsu Chemical Co., Ltd. Rotor for permanent magnet rotating machine
WO2014115375A1 (fr) * 2013-01-28 2014-07-31 Jx日鉱日石金属株式会社 Cible de pulvérisation pour aimant en terre rare et procédé de production s'y rapportant
CN105185500A (zh) * 2015-08-28 2015-12-23 包头天和磁材技术有限责任公司 永磁材料的制造方法
CN105489336A (zh) * 2016-01-22 2016-04-13 宁波松科磁材有限公司 一种钕铁硼磁体渗镝的方法
JP2016115774A (ja) * 2014-12-12 2016-06-23 トヨタ自動車株式会社 希土類磁石粉末及びその製造方法
US9786419B2 (en) 2013-10-09 2017-10-10 Ford Global Technologies, Llc Grain boundary diffusion process for rare-earth magnets
CN108962580A (zh) * 2018-06-28 2018-12-07 宁波招宝磁业有限公司 一种渗镝/铽钕铁硼磁体的制备方法
CN110148518A (zh) * 2019-06-18 2019-08-20 天津大学 自定义增强磁场的磁铁阵列及其制备方法
CN110911151A (zh) * 2019-11-29 2020-03-24 烟台首钢磁性材料股份有限公司 一种提高钕铁硼烧结永磁体矫顽力的方法
CN110993311A (zh) * 2019-12-30 2020-04-10 宁波韵升股份有限公司 一种晶界扩散制备高性能大块钕铁硼磁体的方法
CN111243809A (zh) * 2020-02-29 2020-06-05 厦门钨业股份有限公司 一种钕铁硼材料及其制备方法和应用
CN114999801A (zh) * 2022-05-26 2022-09-02 中国科学院金属研究所 一种提高NdFeB基永磁厚膜矫顽力的方法

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US11114225B2 (en) * 2016-03-07 2021-09-07 Jx Nippon Mining & Metals Corporation Rare earth thin film magnet and production method thereof

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JPS6180046A (ja) * 1984-09-28 1986-04-23 Eiken Kizai Kk ジチオスレイト−ルによる喀痰集細胞法
JP2008071904A (ja) * 2006-09-13 2008-03-27 Ulvac Japan Ltd 永久磁石及び永久磁石の製造方法
JP2008172037A (ja) * 2007-01-12 2008-07-24 Daido Steel Co Ltd 希土類磁石及びその製造方法
WO2011030409A1 (fr) * 2009-09-09 2011-03-17 信越化学工業株式会社 Rotor pour machine rotative de type à aimants permanents
US8638017B2 (en) 2009-09-18 2014-01-28 Shin-Etsu Chemical Co., Ltd. Rotor for permanent magnet rotating machine
JP2011130522A (ja) * 2009-12-15 2011-06-30 Minebea Co Ltd 微小回転電気機械の磁気回路
WO2011103104A2 (fr) * 2010-02-17 2011-08-25 Electron Energy Corporation Aimants composites et stratifiés en terre rare présentant une résistivité électrique accrue
WO2011103104A3 (fr) * 2010-02-17 2011-12-29 Electron Energy Corporation Aimants composites et stratifiés en terre rare présentant une résistivité électrique accrue
GB2490287A (en) * 2010-02-17 2012-10-24 Electron Energy Corp Rare earth laminated, composite magnets with increased electrical resistivity
WO2013103132A1 (fr) * 2012-01-04 2013-07-11 トヨタ自動車株式会社 Aimant nanocomposite de terres rares
CN104011811A (zh) * 2012-01-04 2014-08-27 丰田自动车株式会社 稀土类纳米复合磁铁
JPWO2013103132A1 (ja) * 2012-01-04 2015-05-11 トヨタ自動車株式会社 希土類ナノコンポジット磁石
US9818520B2 (en) 2012-01-04 2017-11-14 Toyota Jidosha Kabushiki Kaisha Rare-earth nanocomposite magnet
US10090090B2 (en) 2012-01-04 2018-10-02 Toyota Jidosha Kabushiki Kaisha Rare-earth nanocomposite magnet
WO2014115375A1 (fr) * 2013-01-28 2014-07-31 Jx日鉱日石金属株式会社 Cible de pulvérisation pour aimant en terre rare et procédé de production s'y rapportant
US10290407B2 (en) 2013-10-09 2019-05-14 Ford Global Technologies, Llc Grain boundary diffusion process for rare-earth magnets
US9786419B2 (en) 2013-10-09 2017-10-10 Ford Global Technologies, Llc Grain boundary diffusion process for rare-earth magnets
JP2016115774A (ja) * 2014-12-12 2016-06-23 トヨタ自動車株式会社 希土類磁石粉末及びその製造方法
CN105185500A (zh) * 2015-08-28 2015-12-23 包头天和磁材技术有限责任公司 永磁材料的制造方法
CN105489336A (zh) * 2016-01-22 2016-04-13 宁波松科磁材有限公司 一种钕铁硼磁体渗镝的方法
CN108962580A (zh) * 2018-06-28 2018-12-07 宁波招宝磁业有限公司 一种渗镝/铽钕铁硼磁体的制备方法
CN108962580B (zh) * 2018-06-28 2020-06-30 宁波招宝磁业有限公司 一种渗镝/铽钕铁硼磁体的制备方法
CN110148518A (zh) * 2019-06-18 2019-08-20 天津大学 自定义增强磁场的磁铁阵列及其制备方法
CN110911151A (zh) * 2019-11-29 2020-03-24 烟台首钢磁性材料股份有限公司 一种提高钕铁硼烧结永磁体矫顽力的方法
CN110911151B (zh) * 2019-11-29 2021-08-06 烟台首钢磁性材料股份有限公司 一种提高钕铁硼烧结永磁体矫顽力的方法
US11948734B2 (en) 2019-11-29 2024-04-02 Yantai Shougang Magnetic Materials Inc Method about increasing the coercivity of a sintered type NdFeB permanent magnet
CN110993311A (zh) * 2019-12-30 2020-04-10 宁波韵升股份有限公司 一种晶界扩散制备高性能大块钕铁硼磁体的方法
CN111243809A (zh) * 2020-02-29 2020-06-05 厦门钨业股份有限公司 一种钕铁硼材料及其制备方法和应用
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CN114999801A (zh) * 2022-05-26 2022-09-02 中国科学院金属研究所 一种提高NdFeB基永磁厚膜矫顽力的方法

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