WO2010013109A1 - Procédé de formation de film sio<sb>2</sb> mince sur un matériau magnétique - Google Patents

Procédé de formation de film sio<sb>2</sb> mince sur un matériau magnétique Download PDF

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Publication number
WO2010013109A1
WO2010013109A1 PCT/IB2009/006320 IB2009006320W WO2010013109A1 WO 2010013109 A1 WO2010013109 A1 WO 2010013109A1 IB 2009006320 W IB2009006320 W IB 2009006320W WO 2010013109 A1 WO2010013109 A1 WO 2010013109A1
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Prior art keywords
magnetic material
film
oxide
thin sio
forming
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PCT/IB2009/006320
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English (en)
Inventor
Yusuke Oishi
Toshiya Yamaguchi
Eisuke Hoshina
Kazuhiro Kawashima
Takeshi Hattori
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Toyota Jidosha Kabushiki Kaisha
Fine Sinter Co., Ltd
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Publication of WO2010013109A1 publication Critical patent/WO2010013109A1/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
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • H01F1/14783—Fe-Si based alloys in the form of sheets with insulating coating
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • 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
    • H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin

Definitions

  • the invention relates to a method of forming a thin SiO 2 film in which a magnetic material is subjected to an oxidation treatment to form a thin SiO 2 film thereon.
  • Japanese Patent No. 2698003 describes a method for forming a thin insulating coating film on an electromagnetic steel sheet by which the steel is subjected to an oxidation treatment, SiO 2 is formed, and adhesion of the coating film is improved.
  • JP-A-2005-146315 and Japanese Patent No. 4010296 describe a method for subjecting a magnetic powder to an oxidation treatment, oxidizing mainly a second element with a high oxidation reactivity, and forming an oxide coating film.
  • An Fe-Si system is described as a representative example in the methods of the above-described related art, and the performance of the magnetic materials is improved, for example, electric resistivity is increased, by forming silicon oxide SiO 2 in the vicinity of the surface layer of the magnetic material by subjecting the magnetic material to an oxidation treatment.
  • a method 1 of the related art that is illustrated by FIG. 6 is described in Japanese Patent No. 2698003 and includes conducting an oxidation treatment of a steel sheet as a base material and then performing insulating coating by using a coating liquid or the like.
  • a method 2 of the related art that is illustrated by FIG. 6 is a method for producing a magnetic powder and the like that is described in JP-A-2005-146315 and Japanese Patent No. 4010296, and this method involves only a process of subjecting a base material to an oxidation treatment.
  • a method 3 of the related art that is illustrated by FIG 6 is a method for producing a magnetic powder and the like that is described in Japanese Patent No. 4010296, and this method involves repeating a processing cycle including a process of subjecting a base material to an oxidation treatment and a process of performing a treatment for preventing the diffusion of oxygen component after the oxidation treatment process.
  • the object of the invention disclosed in the aforementioned Japanese Patent No. 2698003 is to produce a SiO 2 film by performing an oxidation treatment prior to coating an insulating film in order to increase the adhesion of the insulating film coated on an electromagnetic steel sheet and an effect of increasing the electric resistance by oxidation treatment (effect of increasing electric resistivity by forming SiO 2 ; referred to hereinbelow as "resistance increase effect”) is not realized.
  • the problem associated with all the inventions of related art is that a production method by which SiO 2 is formed by conducting only an oxidation treatment cannot be expected to demonstrate the resistance increase effect, and eddy current loss increases in a case where the magnetic material coated with the thin SiO 2 film, disclosed in the related art, is used as a soft magnetic material.
  • the invention provides a method for forming a thin SiO 2 film on a magnetic material by which an electric resistance value is increased to reduce eddy current loss in the magnetic material.
  • the results of a surface analysis of magnetic materials obtained in the comprehensive research conducted by the inventors demonstrated that SiO 2 can be formed by conducting an oxidation treatment in a weakly oxidizing atmosphere according to any of the above-described inventions of the related art, but a sufficient resistance increase effect is not demonstrated because uniform SiO 2 is not formed.
  • SiO 2 itself has a high electric resistivity, but where SiO 2 is formed unevenly on a magnetic material, the electric resistivity decreases significantly and when zones where SiO 2 has not been formed are present on the magnetic material surface, the desired electric resistivity cannot be obtained.
  • an Fe oxide is mainly present in the zones where SiO 2 has not been formed, SiO 2 does not form a uniform film because of the Fe oxide presence, and the electric resistivity decreases.
  • An aspect of the invention relates to a method for forming a thin SiO 2 film of a magnetic material by which a thin SiO 2 film is formed on a surface of a magnetic material including iron and silicon as main components, characterized by including: performing an Fe oxide removal process of removing Fe oxide present on the surface of the magnetic material by performing a reduction treatment with respect to the magnetic material; and performing an oxidation treatment process of forming a thin SiO 2 film on the surface of the magnetic material by performing an oxidation treatment with respect to the magnetic material from which the Fe oxide has been removed in the Fe oxide removal process.
  • the Fe oxide present on the surface of the magnetic material may be removed in the Fe oxide removal process by performing the reduction treatment with respect to the magnetic material by using either or both C and H 2 .
  • Conditions of the reduction treatment in a case where the reduction treatment is performed with respect to the magnetic material by using C in the Fe oxide removal process may include a heating temperature of 700 to 1300 0 C and a CO partial pressure (Pco) of equal to or less than 1 Pa.
  • Conditions of the reduction treatment in a case where the reduction treatment is performed with respect to the magnetic material by using H 2 in the Fe oxide removal process may include a heating temperature of 700 to 1300 0 C and a dew point of equal to or less than -40°C.
  • the oxidation treatment process may be performed within a heating temperature range of 700 to 1300 0 C in a hydrogen gas flow with a partial pressure ratio (P H 2 O /P H2 ) of a partial pressure of water vapor (P H2O ) to a partial pressure of hydrogen (PH 2 ) of 1 x 10 '5 to 1 x 10 '1 .
  • the oxidation treatment process may be performed within a heating temperature range of 700 to 1300 0 C in a carbon monoxide gas flow with a partial pressure ratio (Pco 2 /Pco) of a partial pressure of carbon dioxide (Pco2) to a partial pressure of carbon monoxide (Pco) of 1 x 10 "6 to 1 x 10 " .
  • Fe oxide may be not present on the magnetic material surface after the oxidation treatment performed in the oxidation treatment process.
  • the Fe oxide may be FeO x .
  • a more uniform thin SiO 2 film can be formed on the magnetic material surface and, therefore, a desirable high electric resistivity is obtained for the magnetic material.
  • FIG 1 is a process flow diagram of an embodiment of the invention
  • FIG 2 shows Si element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material
  • FIG 3 shows Fe element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material
  • FIGS. 4A and 4B are formation image diagrams of thin SiO 2 films;
  • FIG 4A is a formation image diagram of a thin SiO 2 film formed by the method for forming a thin SiO 2 film in accordance with the invention; and
  • FIG 4B is a formation image diagram of a thin SiO 2 film formed by the method according to the related art;
  • FIG 5 shows a resistant value after the oxidation treatment;
  • FIG 6 shows a process flow diagram of the method according to the related art.
  • FIG. 1 is a process flow diagram of an embodiment of the invention.
  • FIG 2 shows Si element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material.
  • FIG. 3 shows Fe element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material.
  • FIGS. 4A and 4B are formation image diagrams of thin SiO 2 films.
  • FIG. 4A is a formation image diagram of a thin SiO 2 film formed by the method for forming a thin SiO 2 film in accordance with the invention.
  • FIG. 4B is a formation image diagram of a thin SiO 2 film formed by the method according to the related art.
  • FIG. 5 shows a resistant value after the oxidation treatment.
  • FIG. 1 is a process flow diagram of an embodiment of the invention.
  • FIG 2 shows Si element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material.
  • FIG. 3 shows Fe element state analysis results obtained by XPS analysis for the outermost surface of the magnetic material.
  • FIG. 6 shows a process flow diagram of the method according to the related art.
  • a method for forming a thin SiO 2 film by which a thin SiO 2 film is formed on the surface of an Fe-Si magnetic powder, which is a magnetic material will be described below, b ⁇ t the invention is not limited to the magnetic powder and can be generally applied to a wide range of magnetic materials of any shape, such as a powder and a steel sheet, provided that the magnetic material includes Fe and Si as the main components.
  • a method for forming a thin SiO 2 film by which a thin SiO 2 film is formed on the surface of a base material that is a magnetic material will be explained below with reference to FIG. 1.
  • the main processing flow of the method for forming a thin SiO 2 film involves performing in the order of description an Fe oxide removal process of removing an Fe oxide present on the surface of the magnetic material by performing a reduction treatment with C (carbon) or H 2 with respect to a base material that is a treatment object, and an oxidation treatment process of forming a thin SiO 2 on the surface of the magnetic material by performing an oxidation treatment with respect to the magnetic material from which the Fe oxide has been removed by the Fe oxide removal process.
  • a magnetic material (base material) that is the treatment object to be subjected to the treatment performed in the aforementioned processes will be described.
  • the base material that is a treatment object is a magnetic material including Fe and Si as the main components and can be in the form of a steel sheet or a powder.
  • a magnetic powder of an Fe-Si system that includes Fe and Si as the main components is used, this magnetic material being an example of a soft magnetic material.
  • Magnetic powders of an Fe-Si system are widely used as soft magnetic material powders because of a comparatively high electric resistivity and a comparatively low cost.
  • the amount of Si in the magnetic powder of an Fe-Si system is determined by a balance of specific resistance value and magnetic flux density.
  • the amount of Si may be 1 to 10 wt.%, or 1 to 7 wt.%, or 2 to 5 wt.%.
  • the amount of Si is too low, the electric resistivity is small and the eddy current loss cannot be reduced.
  • the amount of Si is too high, magnetic properties are degraded.
  • the magnetic powder of an Fe-Si system may be an alloy powder including a predetermined amount of Si and Fe and unavoidable impurities. This alloy is not necessarily a two-component alloy and may include appropriate amounts of carbon (denoted hereinbelow by C), aluminum (Al), tin (Sn), nickel (Ni), and cobalt (Co).
  • the magnetic powder may be an atomized powder obtained by gas atomization or water atomization or a ground powder obtained by grinding an alloy ingot in a ball mill or the like.
  • the original base material may include C, or C may be added to the base material by a carburization treatment.
  • C carbon
  • the Fe oxide removal process will be described below.
  • the Fe oxide removal process is performed to remove this Fe oxide.
  • a reduction treatment is performed, while conducting heating with a heating means such as an electric furnace, and in this process, the Fe oxide is removed from the surface of the base material powder by heating the base material at a predetermined temperature and a predetermined dew point for a predetermined reduction treatment time in a reducing atmosphere satisfying the below-described reduction treatment conditions and reducing the Fe oxide present on the base material powder surface.
  • the below-described oxidation treatment process is performed continuously therewith.
  • the Fe oxide as referred to herein is an Fe oxide represented by FeO x , such as FeO and Fe 2 O 3 .
  • the reduction treatment performed in the Fe oxide removal process can be performed using either of C and H 2 , or the reduction treatment of the base material powder is performed by using both the C and the H 2 , thereby removing the Fe oxide present on the surface of the base material powder.
  • a dew point adjustment device that can adjust a dew point of gases is connected to the electric furnace in the intermediate section of each gas piping serving to introduce a gas for the reduction treatment and a gas for the oxidation treatment into the electric furnace.
  • a configuration may be used in which a dew point on the inlet port side and a dew point on the outlet port side of the electric furnace that are located downstream of the dew point adjustment devices be measured with dew point meters of an electrostatic capacity system.
  • a heating temperature of 700 to 1300 0 C may be selected as a condition of the reduction treatment in a case where C is used for the reduction treatment. Furthermore, with consideration for a CO reaction (C + O ⁇ CO), a partial pressure of CO (Pco) may be equal to or less than 1 Pa.
  • a heating temperature of 700 to 1300 0 C may be selected as a condition of the reduction treatment in a case where H 2 is used instead of C for the reduction treatment.
  • the dew point may be equal to or less than -40 0 C. Where the dew point is higher than -40 0 C, SiO 2 is generated before the Fe oxide is removed by the reduction treatment.
  • the reduction treatment in the case both the C and the H 2 are used for the reduction treatment may be performed under conditions such that the conditions relating to the above-described case in which C is used and the case in which H 2 is used are satisfied.
  • the reduction treatment time the sufficient treatment can be performed for about 1 to 4 h, but the reduction treatment time is not particularly limited and may be appropriately set correspondingly to various conditions such as the base material shape, amount to be treated, and specifications of the apparatus used.
  • the reducing atmosphere is not particularly limited, and for example ammonia gas may be used.
  • a thin silicon oxide film SiO 2 is formed uniformly on the base material surface by conducting heat treatment under oxidation treatment conditions (in the embodiment, the temperature condition may be 700 to 1300 0 C and the dew point conditions may be equal to or less than 50 0 C ) in an oxidizing atmosphere having a predetermined temperature and a predetermined dew point with respect to the surface of the base material (magnetic powder of an Fe-Si system) that has been subjected to the reduction treatment in the Fe oxide removal process, the oxidation treatment process being conducted, for example, by using an electric furnace similar to that used in the above-described Fe oxide removal process in an oxidizing atmosphere (for example, in a hydrogen gas flow that is an oxidizing atmosphere maintained at a predetermined oxygen concentration (oxygen partial pressure)).
  • oxidation treatment conditions in the embodiment, the temperature condition may be 700 to 1300 0 C and the dew point conditions may be equal to or less than 50 0 C
  • the oxidation treatment process being conducted, for example, by using an electric furnace similar to that
  • the thickness of the silicon oxide film formed on the base material surface can be appropriately adjusted according to the temperature conditions of heating, heating time, and Si content in the base material. Furthermore, by performing the oxidation treatment under a dew point condition of equal to or lower than 50 0 C, it is possible to oxidize preferentially only Si on the base material surface and produce a thin SiO 2 film with good efficiency. [0038] Where heating is performed in the above-described temperature condition range of the oxidation treatment, Si, which has an oxidation rate higher than that of Fe, diffuses into the surface layer of the base material powder and is oxidized. As a result, the surface of the base material powder is covered uniformly with Si oxide.
  • the oxidizing atmosphere is usually most often formed in a hydrogen gas flow or a carbon monoxide gas flow.
  • a partial pressure ratio (PmofPrn) of a partial pressure of water vapor (P H2O ) to a partial pressure of hydrogen (P H2 ) may be 1 x 10 "5 to 1 x 10 "1 .
  • a partial pressure ratio (Pco2/Pco) of a partial pressure of carbon dioxide (Pco2) to a partial pressure of carbon monoxide (Pco) rnay be 1 x 10 "6 to 1 x 10 "1 .
  • the oxidizing atmosphere can be also attained, for example, by controlling the dew point (temperature) in the hydrogen gas flow.
  • the dew point can be easily observed with a dew point thermometer or the like.
  • the dew point of water vapor in the hydrogen gas flow may be equal to or less than +50 0 C.
  • the dew point (temperature) is a temperature at which the water vapor contained in a gas reaches the saturation and condensates and, for example, is an ambient temperature at a relative humidity of 100%. Where the amount of moisture in an oxidizing atmosphere is small, the dew point temperature is low.
  • the dew point temperature thereof rises.
  • the dew point is an indicator of the amount of moisture contained in the oxidizing atmosphere, and the dew point temperature has no correlation with the temperature of the oxidizing atmosphere itself.
  • the treatment is performed under a condition of a gas pressure of 1 atm, and the dew point referred thereto means a value under 1 atm (0.1 MPa).
  • a thin SiO 2 film may be also formed on the base material surface by using a heating means other than the electric furnace.
  • a magnetic powder including Fe and Si as the main components and serving as a base material (starting material) (in the example embodiment, the magnetic powder has a composition of Fe - 6% Si - 0.5% C; units: wt.%) is placed into the above-described electric furnace, the inside of the electric furnace is evacuated, and then a reducing gas serving as a reducing atmosphere is introduced into the electric furnace (in the example embodiment, hydrogen gas is used: the reduction treatment conditions are CO partial pressure 10 "2 , dew point -70 0 C).
  • Dew point adjustment devices that can adjust the dew point of the reducing gas and the below-described oxidizing gas are connected to the intermediate section of gas piping for introducing the reducing gas and the below-described oxidizing gas into the electric furnace.
  • the dew point at the inlet port side and the dew point at the outlet port side of the electric furnace that were located downstream of the dew point adjustment devices were measured with dew point meters of an electrostatic capacity type.
  • the dew point inside the electric furnace was stabilized at a constant value.
  • the dew point inside the electric furnace was considered and handled as being almost equal to the dew point at the inlet port side (inlet port dew point) (same hereinbelow).
  • the dew point specified the reducing gas and the below-described oxidizing gas after dew point adjustment in a state under 1 aim.
  • the temperature inside the electric furnace was raised at a predetermined temperature increase rate and held for 1 h at 1100 0 C, followed by cooling.
  • the reduction treatment Fe oxide removal process
  • the oxidation treatment process was performed for a predetermined time (in the example embodiment, 1 h) under the conditions of a heating temperature of 1100 0 C and a dew point of 0 0 C in an electric furnace with an oxidizing atmosphere constituted by a hydrogen gas flow (oxidizing gas) with a partial pressure ratio (Pmo/Pm) of a partial pressure of water vapor (P H2O ) to a partial pressure of hydrogen (P H2 ) of about 0.2.
  • a thin silicon dioxide (SiO 2 ) film which is an insulating film, was formed on the surface of the magnetic powder.
  • the CO partial pressure which is one of the reduction treatment condition, was set to a value equal to or less than 1 Pa (in the example embodiment, 10 "2 ) for the sake of advancing the equilibrium of the above-described CO reaction to the CO generation side.
  • the Si elemental state on the outermost surface of the magnetic powder was analyzed by an XPS analysis (XPS: X-ray Photoelectron Spectroscopy) with respect to the magnetic powder having SiO 2 formed on the surface thereof by subjecting the base material to the above-described Fe oxide removal process and oxidation treatment process.
  • the SiO 2 peaks were compared for the magnetic powder ((I) in FIG. 2) obtained by forming SiO 2 on the base material surface by the method for forming a thin SiO 2 film in accordance with the invention, as in the example embodiment, the comparative magnetic powder ((II) in FIG 2; method disclosed in Japanese Patent No.
  • the Fe elemental state on the outermost surface was also analyzed by the XPS analysis with respect to the magnetic powder formed by implementing the above-described Fe oxide removal process and oxidation treatment process and the magnetic powder (comparative sample) that was subjected only to the oxidation treatment as in the method according to the related art.
  • FIG. 4B shows an image of a thin SiO 2 film formed by the method according to the related art (a method in which only the oxidation treatment is performed). In this case, a uniform thin SiO 2 film cannot be produced on the surface of magnetic powder because of the presence of FeO and Fe 2 O 3 , which are Fe oxides and locally present on the original surface.
  • FIG. 4A shows an image of a thin SiO 2 film formed by the method for forming a thin SiO 2 film in accordance with the invention.
  • FeO and Fe 2 O 3 which are Fe oxides
  • FeO and Fe 2 O 3 Fe oxides represented by FeO x
  • FeO x Fe oxides represented by FeO x
  • the resistance of a magnetic material can be increased by introducing the Fe oxide removal process performed in accordance with the invention in the preliminary stage of the method according to the related art.
  • a magnetic powder is described as the magnetic material, but a thin SiO 2 film can be also formed under the treatment conditions similar to those described above on a steel material.
  • a method for forming a thin SiO 2 film on a magnetic material that is a method for forming a thin SiO 2 film by which a thin SiO 2 film is formed on a surface of a magnetic material including iron and silicon as the main components, this method including an Fe oxide removal process of removing an Fe oxide present on the surface of the magnetic material by performing a reduction treatment with respect to the magnetic material; and an oxidation treatment process of forming a thin SiO 2 on the surface of the magnetic material by performing an oxidation treatment with respect to the magnetic material from which the Fe oxide has been removed by the Fe oxide removal process, it is possible to form a more uniform thin SiO 2 film on the magnetic material surface and, therefore, the desirable high electric resistivity can be obtained for the magnetic material.
  • a method for forming a thin SiO 2 film on a magnetic material can be applied in which the Fe oxide present on the surface of the magnetic material is removed in the Fe oxide removal process by performing the reduction treatment with respect to the magnetic material by using either or both C and H 2 , and a reduction treatment method can be appropriately selected with consideration for the starting material composition, starting material form, and the treatment volume.
  • the method for forming a thin SiO 2 film in accordance with the invention has been discovered by specifying FeO and Fe 2 O 3 (inhibiting factors that decrease the resistance value) that could not be specified as problems in the methods according to the related art, and a technique for forming a more uniform thin SiO 2 film has been established by which an Fe oxide removal process of reducing Fe oxide is provided as a pretreatment of an oxidation treatment when a thin SiO 2 film is formed by the oxidation treatment on the base material surface, and the reduction treatment and oxidation treatment are performed continuously with respect to the base material.
  • the invention can be introduced when required in the process of forming a thin SiO 2 film by the oxidation treatment alone that has been performed in the related art.

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Abstract

L'invention porte sur un procédé de formation d'un film SiO2 mince sur un matériau magnétique par lequel un film SiO2 mince est formé sur une surface d'un matériau magnétique comprenant du fer et du silicium en tant que composants principaux, le procédé comprenant : une opération d'élimination d'oxyde de fer consistant à éliminer un oxyde de fer présent sur la surface du matériau magnétique par réalisation d'un traitement de réduction par rapport au matériau magnétique; et une opération de traitement d'oxydation consistant à former un film SiO2 mince sur la surface du matériau magnétique par réalisation d'un traitement d'oxydation par rapport au matériau magnétique duquel l'oxyde de fer a été éliminé dans l'opération d'élimination d'oxyde de fer. Une valeur de résistance électrique du matériau magnétique peut être augmentée et des pertes par courant de Foucault peuvent être réduites.
PCT/IB2009/006320 2008-08-01 2009-07-23 Procédé de formation de film sio<sb>2</sb> mince sur un matériau magnétique WO2010013109A1 (fr)

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JP2008199966A JP2010040666A (ja) 2008-08-01 2008-08-01 磁性材料のＳｉＯ２薄膜形成方法

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US11225706B2 (en) 2017-07-13 2022-01-18 Nippon Steel Corporation Grain-oriented electrical steel sheet

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KR102466392B1 (ko) * 2021-08-05 2022-11-11 한국생산기술연구원 선택적 산화 열처리를 이용한 균일 절연막이 코팅된 연자성 합금 분말 제조 장치 및 그 방법
KR102466390B1 (ko) * 2021-08-05 2022-11-11 한국생산기술연구원 선택적 산화 열처리를 이용한 Fe계 연자성 합금 분말 제조 장치 및 그 방법

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