Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
  • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
  • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
  • C23C8/10—Oxidising
  • C23C8/12—Oxidising using elemental oxygen or ozone
  • C23C8/14—Oxidising of ferrous surfaces
• • 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
  • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
  • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C19/00—Alloys based on nickel or cobalt
  • C22C19/07—Alloys based on nickel or cobalt based on cobalt
• • 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
  • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
  • C23C8/02—Pretreatment of the material to be coated
• • 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
  • H01F1/12—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 soft-magnetic materials
  • H01F1/14—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 soft-magnetic materials metals or alloys
  • H01F1/147—Alloys characterised by their composition
• • 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
  • H01F1/12—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 soft-magnetic materials
  • H01F1/14—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 soft-magnetic materials metals or alloys
  • H01F1/16—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 soft-magnetic materials metals or alloys in the form of sheets
  • H01F1/18—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 soft-magnetic materials metals or alloys in the form of sheets with insulating coating
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
  • H01F27/00—Details of transformers or inductances, in general
  • H01F27/24—Magnetic cores
  • H01F27/245—Magnetic cores made from sheets, e.g. grain-oriented

Definitions

• the present invention relates to a Fe-Co based alloy coated substrate and a laminated core member.
• Patent Document 1 discloses a laminated core in which permendur (Fe-Co based alloy) single layer materials having high saturation magnetic flux density are laminated, and proposes forming a ceramic layer of magnesium oxide, zirconium oxide, aluminum oxide or the like as an insulation coating on a surface of the single layer materials.
• Patent Document 2 describes that oxidizing annealing is performed on a plate material after a final recrystallization annealing process, an oxide layer of 0.5 ⁇ m to 10 ⁇ m is produced, and electrical insulation during lamination is ensured.
• Patent Document 1 While the insulation coating of magnesium oxide or the like described in Patent Document 1 has good insulation, a separate process for performing vapor deposition or applying solution is necessary, which becomes a cause of increased man-hours. Adhesion is also required for the Fe-Co based alloy substrate serving as a material of the laminated core, so that the insulating layer does not peel off and no current flows between the laminated single plates during manufacturing of the laminated core. Neither Patent Document 1 nor Patent Document 2 discusses maintaining all of insulation, adhesion, and magnetic properties at good levels.
• an object of the present invention is to provide a Fe-Co based alloy substrate and a laminated core member in which good magnetic properties can be achieved while insulation and adhesion are ensured.
• the present invention has been made in view of the above-described problems.
• one aspect of the present invention is a Fe-Co based alloy coated substrate having an oxide layer on at least one of a front surface and a back surface of a Fe-Co based alloy substrate.
• the Fe-Co based alloy coated substrate is characterized in the following. In a case where the oxide layer is formed only on the front surface or the back surface of the substrate, the oxide layer has a thickness of 280 nm to 500 nm. In a case where the oxide layer is formed on both the front surface and the back surface, the oxide layer on each of the front surface side and the back surface side has a thickness of 140 nm to 500 nm. In a cross-section in a thickness direction of the Fe-Co based alloy coated substrate, a maximum height difference of irregularities of the oxide layer at an interface between the oxide layer and the Fe-Co based alloy substrate is 300 nm or less.
• a lower limit of the thickness of the oxide layer on each of the front surface side and the back surface side is 250 nm.
• Another aspect of the present invention is a laminated core member in which the Fe-Co based alloy coated substrate is laminated.
• a Fe-Co based alloy coated substrate in which good magnetic properties can be achieved while insulation and adhesion are ensured, as well as a high-performance laminated core member, can be obtained.
• a Fe-Co based alloy substrate of the present invention refers to one (coil) of a strip shape, one (sheet) of a rectangular shape, or a thin plate of a part shape.
• the Fe-Co based alloy substrate of the present invention may have a plate thickness of, for example, 0.5 mm or less, preferably 0.25 mm or less.
• the Fe-Co based alloy in the present invention refers to an alloy material containing 95% by mass or more of Fe+Co and containing 25% to 60% by mass of Co.
• the lower limit of Co content is preferably 40%. Accordingly, high magnetic flux density can be exhibited.
• the Fe-Co based alloy of the present invention may contain, in addition to 1.70% to 2.10% by mass of V and 0.01% to 0.40% by mass of Mn, one or two or more elements selected from Si, Al, Zr, B, Ni, Ta, Nb, W, Ti, Mo, and Cr in a total amount of up to 2.5% by mass.
• impurity elements examples include C, S, P, and O, and the upper limit of each of these elements is preferably, for example, 0.1%.
• the Fe-Co based alloy coated substrate of the present invention has an oxide layer on at least one of a front surface and a back surface of the Fe-Co based alloy substrate having the composition described above.
• the present invention is characterized in the following: in the case where the oxide layer is formed on either the front surface or the back surface of the substrate, the oxide layer has a thickness of 280 nm to 500 nm; in the case where the oxide layer is formed on both the front surface and back surface of the substrate, the oxide layer on each of the front surface side and the back surface side has a thickness within the range of 140 nm to 500 nm.
• the oxide layer that has a larger lattice constant than the Fe-Co based alloy is formed on the substrate surface, slight tensile stress is applied to the substrate surface, and DC magnetic properties of the Fe-Co alloy having positive magnetostriction tend to be improved.
• the oxide layer has a thickness of 280 nm or less (when the oxide layer is formed on only one side of the substrate) 140 nm or less (when the oxide layer is formed on both sides (front surface and back surface) of the substrate), the thickness of the oxide layer is insufficient, and there is a possibility that current may flow between laminated single plates in the laminated core and iron loss may deteriorate.
• the oxide layer has a thickness of more than 500 nm
• the oxide layer has a thickness of more than 500 nm, due to an increase in the oxide layer that is not ferromagnetic, the magnetic flux density tends to decrease.
• the preferable lower limit of the thickness differs between the case where the oxide layer is formed on only one side (either front surface or back surface) of the substrate and the case where the oxide layer is formed on both sides is that the Fe-Co based alloy coated substrate of the present invention is assumed to be applied to a laminated core. That is, when the Fe-Co based alloy coated substrates having the oxide layer on both sides are laminated, the thickness of the oxide layer between the coated substrates is a total thickness obtained by adding the thickness of the oxide layer on the back surface of the substrate and the thickness of the oxide layer on the front surface of the substrate.
• the coated substrate having the oxide layer on both sides of the substrate may have a thinner oxide layer than the coated substrate having the oxide layer on only one side.
• the lower limit of the thickness of the oxide layer is preferably 300 nm, more preferably 310 nm.
• the lower limit of the thickness of the oxide layer is preferably 150 nm, more preferably 160 nm, even more preferably 180 nm, 200 nm, or 220 nm.
• the upper limit of the thickness of the oxide layer is preferably 400 nm, more preferably 350 nm.
• the lower limit of the thickness of the oxide layer on each of the front surface side and the back surface side is 250 nm.
• the Fe-Co based alloy substrate can be coated with a stable oxide layer, and it is possible to further enhance an effect of suppressing corrosion that may occur during storage of materials or the like.
• the lower limit of the thickness of the oxide layer is more preferably 280 nm, even more preferably 300 nm or more.
• a laminated core member obtained by laminating the Fe-Co based alloy coated substrate described above has good magnetic properties.
• the Fe-Co based alloy coated substrate of the present invention is also characterized in that a maximum height difference of irregularities at an interface between the oxide layer and the substrate is 300 nm or less in a cross-section in a thickness direction of the substrate.
• a maximum height difference of irregularities at an interface between the oxide layer and the substrate is 300 nm or less in a cross-section in a thickness direction of the substrate.
• the thickness of the oxide layer and the maximum height difference of irregularities at the interface between the oxide layer and the substrate in the present invention can be measured by using, for example, elemental mapping by a field emission transmission electron microscope (FE-TEM) and a length measurement function of an FE-TEM analysis tool.
• the adhesion in the present invention can be measured by conducting a cross-cut test specified in, for example, JIS K 5400 (1990) or JIS K 5600.
• the Fe-Co based alloy substrate of the present invention can be obtained.
• cold rolling is performed on an intermediate material, the intermediate material having the Fe-Co based alloy composition described above, having been subjected to rapid cooling treatment from an ordering temperature of around 730 °C or higher and having been disordered.
• a hot rolled material, or a strip-shaped material obtained by performing preliminary cold rolling on a hot rolled material can be used.
• the oxide layer may be, for example, mechanically or chemically removed.
• machining to obtain a part shape may be performed by press punching, wire cutting, laser processing or the like.
• oxidation heat treatment is applied to an annealed material that has been subjected to the magnetic annealing described above, so that a thickness of 200 nm to 500 nm is obtained and the maximum height difference of irregularities at the interface between the oxide layer and the substrate is 300 nm or less in the cross-section in the thickness direction.
• the thickness of the oxide layer or the maximum height difference of irregularities can be controlled mainly by adjusting the heating temperature and heating time of the oxidation heat treatment.
• an oxygen partial pressure may be adjusted. For example, by performing heat treatment at 450 °C for 0.5 to 4 hours in an atmospheric atmosphere, it is possible to obtain a Fe-Co based alloy coated substrate having the oxide layer specified in the present invention.
• a cold rolling material having a Fe-Co based alloy composition shown in Table 1 was prepared, subjected to cold rolling multiple times to obtain a cold rolled material having a thickness of 0.2 mm, followed by being subjected to magnetic annealing at 850 °C for 3 hours in a hydrogen atmosphere to obtain an annealed material (Fe-Co based alloy substrate) of Fe-Co based alloy. Thereafter, oxidation heat treatment was performed under the conditions shown in Table 2 to obtain Fe-Co based alloy coated substrates of the present inventive examples and comparative examples in which an oxide layer is formed on the front and back surfaces of the substrate. For each sample obtained, the oxide layer was observed, and adhesion, insulation, and DC magnetic properties were evaluated.
• a surface of a sample was protected with a C film.
• the sample was processed into a film-like cross-sectional test piece parallel to a width direction from the outermost surface of the test piece using focused ion beam scanning electron microscopy (FIB-SEM), and STEM observation was performed with an FE-TEM. Elemental mapping of each of O, Fe, Co, and V was also performed, and the results are shown in FIG. 1 .
• the lower side in each image is the Fe-Co based alloy substrate side.
• the thickness of the oxide layer and the maximum height difference of irregularities at the interface between the oxide layer and the substrate were measured using a length measurement function of an FE-TEM analysis tool.
• the oxide layer was also formed on the back surface of the substrate, and the thickness thereof and the maximum height difference of irregularities were approximately equivalent to those on the front surface side.
• Sample No. Oxide layer thickness [nm] Maximum height difference of irregularities [nm] Film peeling Sheet resistance [ ⁇ /sq.] 1 245 87 No 1.90 ⁇ 10 -3 2 316 88 No 5.38 ⁇ 10 -3 3 315 149 No 5.58 ⁇ 10 -3 11 36 18 No 1.93 ⁇ 10 -3 12 106 43 No 2.15 ⁇ 10 -3 13 935 405 Yes 7.74 ⁇ 10 -3
• DC magnetic properties were measured using a sample obtained by cutting a cold rolled material having a thickness of 0.2 mm into 110 mm in a rolling direction and 25 mm in a direction perpendicular to rolling, followed by subjecting the cold rolled material to magnetic annealing at 850 °C for 3 hours in a hydrogen atmosphere. Thereafter, the same sample was subjected to oxidation heat treatment under the conditions shown in Table 2, and then measured for DC magnetic properties again. The change rates of coercivity, maximum magnetic permeability, and magnetic flux density before and after the oxidation heat treatment were measured, and the results are shown in Table 4. [Table 4] Sample No.
• the thickness or form (maximum height difference of irregularities) of the oxide layer differs depending on the heating temperature and heating time of the oxidation heat treatment.
• the oxide layer has poor adhesion, there is a possibility that the insulating layer may peel off during manufacturing of the laminated core, current may flow between the laminated single plates and iron loss may deteriorate, which is thus unfavorable.
• samples No. 2, No. 3, and No. 13 showed excellent values, indicating that good insulation was exhibited.
• sample No. 1 had smaller sheet resistance than samples No. 2 and No. 3, in actual use as a laminated core, since the oxide layer is formed on both surfaces of the substrate, the thickness is defined by adding the thickness on the front surface side and the thickness on the back surface side of the substrate. Hence, the thickness of the oxide layer of sample No. 1 also becomes approximately twice (about 490 nm) in the use as a laminated core, indicating that sufficient insulation was exhibited.
• samples No. 11 and No. 12 being comparative examples, since the oxide layer was excessively thin, even if the thickness is doubled assuming lamination, the thickness of the oxide layer of sample No.
• the Fe-Co based alloy coated substrates of the present inventive examples had better insulation, adhesion, and magnetic properties than the Fe-Co based alloy coated substrates of comparative examples.
• the present inventive examples No. 2 and No. 3 having an oxide layer thickness of 250 nm or more were excellent in corrosion resistance as well.

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