US20150354051A1 - Apparatus and method for nitriding grain-oriented electrical steel sheet - Google Patents

Apparatus and method for nitriding grain-oriented electrical steel sheet Download PDF

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Publication number
US20150354051A1
US20150354051A1 US14/761,419 US201414761419A US2015354051A1 US 20150354051 A1 US20150354051 A1 US 20150354051A1 US 201414761419 A US201414761419 A US 201414761419A US 2015354051 A1 US2015354051 A1 US 2015354051A1
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Prior art keywords
nitriding
zone
steel sheet
grain
electrical steel
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Abandoned
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US14/761,419
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English (en)
Inventor
Hiroshi Matsuda
Hideyuki Takahashi
Hiroi Yamaguchi
Yasuyuki Hayakawa
Yukihiro Shingaki
Takashi Terashima
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JFE Steel Corp
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JFE Steel Corp
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Assigned to JFE STEEL CORPORATION reassignment JFE STEEL CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAYAKAWA, YASUYUKI, MATSUDA, HIROSHI, SHINGAKI, YUKIHIRO, TAKAHASHI, HIDEYUKI, TERASHIMA, TAKASHI, YAMAGUCHI, HIROI
Publication of US20150354051A1 publication Critical patent/US20150354051A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • 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
    • C23C8/36—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 using ionised gases, e.g. ionitriding
    • C23C8/38—Treatment 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 by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • 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 by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0006—Details, accessories not peculiar to any of the following furnaces
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • 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
    • 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
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • 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
    • C23C8/80—After-treatment
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32018—Glow discharge
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • H01J37/32752—Means for moving the material to be treated for moving the material across the discharge
    • H01J37/32761—Continuous moving
    • H01J37/3277—Continuous moving of continuous material

Definitions

  • the disclosure relates to an apparatus and a method that are suitable for nitriding a grain-oriented electrical steel sheet.
  • a grain oriented electrical steel sheet is a soft magnetic material used as an iron core material of transformers and generators, and is required to have excellent magnetic properties, in particular low iron loss.
  • This steel sheet has a texture in which the ⁇ 001> direction, which is an easy magnetization axis of iron, is highly accorded with the rolling direction of the steel sheet.
  • Such texture is formed through the so-called secondary recrystallization where crystal grains with (110)[001] orientation referred to as Goss orientation are preferentially grown massively, during secondary recrystallization annealing in the production process of the grain-oriented electrical steel sheet.
  • such grain-oriented electrical steel sheets have been manufactured by heating a slab containing 4.5 mass % or less of Si and inhibitor components such as MnS, MnSe and AlN to 1300° C. or higher, thereby dissolving the inhibitor components, then subjecting the slab to hot rolling to obtain a hot rolled steel sheet, and then subjecting the hot rolled steel sheet to hot band annealing as necessary, and subsequent cold rolling once, or twice or more with intermediate annealing performed therebetween until reaching final sheet thickness, then subjecting the steel sheet to primary recrystallization annealing in wet hydrogen atmosphere to perform primary recrystallization and decarburization, and then applying thereon an annealing separator mainly composed of magnesia (MgO) and performing final annealing at 1200° C.
  • MgO magnesia
  • inhibitor components e.g. see U.S. Pat. No. 1,965,559A (PTL 1), JPS4015644B (PTL 2) and JPS5113469B (PTL 3)).
  • JP3940205B (PTL 7)
  • the techniques disclosed in PTLs 5 to 7 are methods of performing nitriding by spraying nitriding gas on the steel sheet. Therefore, non-uniformity of the furnace temperature in terms of duration and position, and difference in decomposition amount of nitriding gas in pipes caused by heat could cause a difference in nitrogen increase depending on the area of the strip, and as a result, secondary recrystallization could become non-uniform and lead to deterioration of magnetic properties.
  • An apparatus for nitriding a grain-oriented electrical steel sheet for continuously nitriding a strip continuously being fed after cold rolling and before secondary recrystallization annealing in a production line of a grain-oriented electrical steel sheet comprising:
  • a nitriding zone for nitriding the strip
  • the nitriding zone contains positive electrodes for glow discharge provided opposite to the strip and negative electrodes for glow discharge provided proximate to the strip between the positive electrodes and the strip, and glow discharge is generated between the positive electrodes and the negative electrodes and the generated plasma is applied to the strip to nitride the strip.
  • the apparatus for nitriding a grain-oriented electrical steel sheet according to any of aspects 1 to 3, further comprising an upstream atmosphere adjusting zone provided between the heating zone and the nitriding zone, and a downstream atmosphere adjusting zone provided between the nitriding zone and the cooling zone.
  • a method for nitriding a grain-oriented electrical steel sheet comprising plasma nitriding the strip by glow discharge using the apparatus according to any of aspects 1 to 7 after cold rolling and before secondary recrystallization annealing during producing a grain-oriented electrical steel sheet.
  • negative electrodes are disposed near the material to be treated, and glow discharge is generated between the negative electrodes and the positive electrodes and the plasma generated by the glow discharge generation is applied to the strip to perform nitriding. Therefore, it is possible to effectively suppress generation of defects such as arcing which is caused when the strip is used as a negative electrode.
  • nitrogen gas can be used as a nitrogen source, and therefore nitrogen sources which may cause environmental problems such as ammonia required for performing gas nitriding, cyan salt required for performing salt bath nitriding or the like do not have to be used. For these reasons, our method has a significant industrial usefulness.
  • FIG. 1 schematically shows a preferable example of the nitriding apparatus of the disclosure.
  • FIG. 2 shows a preferable example of a plasma nitriding device according to the disclosure.
  • FIG. 3 schematically shows another example of the nitriding apparatus of the disclosure.
  • FIG. 1 schematically shows a preferable example of the nitriding apparatus of the disclosure.
  • a heating zone is labeled 1
  • a nitriding zone is labeled 2
  • a cooling zone is labeled 3
  • a strip continuously passing inside the nitriding apparatus with a structure comprising the aforementioned components is labeled 4 .
  • the heating zone may be provided when required and is not always necessary.
  • a strip 4 is subjected to plasma nitriding by glow discharge in the above nitriding zone 2 .
  • FIG. 2 shows a preferable example of a plasma nitriding device according to the disclosure.
  • positive electrodes for glow discharge disposed opposite to the strip 4 are labeled 5
  • pinch rolls are labeled 6
  • negative electrodes disposed near the strip 4 are labeled 7 .
  • the inner part of the nitriding zone 2 is filled with nitrogen gas and hydrogen gas as nitrogen sources.
  • a voltage is applied between the positive electrodes 5 and the negative electrodes 7 to generate glow discharge, and by irradiating the strip 4 with the plasma generated during glow discharge generation, the surface of the strip 4 is subjected to nitriding.
  • the negative electrodes must be perforated or mesh-like.
  • the strip is preferably heated to a temperature of 400° C. or higher.
  • the inside of the nitriding zone is preferably kept under a reduced pressure.
  • heating zone and the cooling zone have a lower degree of pressure reduction compared to the nitriding zone, it is preferable for them to be kept in a state with reduced pressure compared to atmospheric pressure, and by doing so, heat exchange due to convection tends to proceed, and heating and cooling efficiency can be improved.
  • the inside of the nitriding zone is preferably depressurized to around 0.5 torr to 10 torr which is a preferable glow discharge condition, and the heating zone and the cooling zone are preferably depressurized, with a lower degree of pressure reduction, to around 30 torr to 500 torr.
  • FIG. 3 shows an upstream atmosphere adjusting zone 8 - 1 and a downstream atmosphere adjusting zone 8 - 2 with a nitriding zone 2 in between.
  • each of the upstream atmosphere adjusting zone 8 - 1 and the downstream atmosphere adjusting zone 8 - 2 is preferably divided into multiple air chambers where the degrees of pressure reduction are individually adjustable.
  • the degrees of pressure reduction of the air chambers in the upstream atmosphere adjusting zone 8 - 1 are gradually increased toward the nitriding zone 2
  • the degree of pressure reduction of the air chambers in the downstream atmosphere adjusting zone 8 - 2 are gradually decreased from the nitriding zone 2 toward the cooling zone 3 .
  • the inside of the nitriding zone is divided into multiple zones in the width direction of the strip where nitriding can be performed individually inside each divided zone.
  • the heating zone can be omitted if it is disposed in a continuous line for performing other necessary treatment and the strip is already heated, or if the heating by plasma irradiation at the time of plasma nitriding is sufficient.
  • the cooling zone may be disposed after the zone for such treatment.
  • nitriding apparatus may be an independent apparatus that continuously performs only nitriding, or be attached to a processing line for performing another treatment, and in the case of a continuous line, it may be attached to the optimal place considering conditions including efficiency.
  • the strip which is the material to be treated is not particularly limited and, as long as it is a grain-oriented electrical steel strip, any conventionally known strip is applicable.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Electromagnetism (AREA)
  • Power Engineering (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Soft Magnetic Materials (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
US14/761,419 2013-02-18 2014-02-18 Apparatus and method for nitriding grain-oriented electrical steel sheet Abandoned US20150354051A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2013029356A JP5942884B2 (ja) 2013-02-18 2013-02-18 方向性電磁鋼板の窒化処理設備および窒化処理方法
JP2013-029356 2013-02-18
PCT/JP2014/000815 WO2014125839A1 (ja) 2013-02-18 2014-02-18 方向性電磁鋼板の窒化処理設備および窒化処理方法

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PCT/JP2014/000815 A-371-Of-International WO2014125839A1 (ja) 2013-02-18 2014-02-18 方向性電磁鋼板の窒化処理設備および窒化処理方法

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EP (1) EP2957653B1 (ja)
JP (1) JP5942884B2 (ja)
KR (2) KR20170095408A (ja)
CN (1) CN105074043B (ja)
RU (1) RU2614482C2 (ja)
WO (1) WO2014125839A1 (ja)

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CN104831026B (zh) * 2015-05-25 2017-12-12 马钢(集团)控股有限公司 一种电工钢可调退火加热装置及其退火加热方法
JP7174943B2 (ja) * 2017-04-26 2022-11-18 国立大学法人 大分大学 窒化処理装置
RU187937U1 (ru) * 2017-10-30 2019-03-25 Федеральное государственное автономное образовательное учреждение высшего образования "Крымский федеральный университет имени В.И. Вернадского" Устройство для ионно-плазменного упрочнения изделий из конструкционных и специальных сталей и сплавов
KR102603846B1 (ko) * 2018-03-30 2023-11-21 제이에프이 스틸 가부시키가이샤 방향성 전기 강판의 제조 설비

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EP2957653A4 (en) 2016-03-02
WO2014125839A1 (ja) 2014-08-21
EP2957653A1 (en) 2015-12-23
RU2614482C2 (ru) 2017-03-28
KR20170095408A (ko) 2017-08-22
JP2014156644A (ja) 2014-08-28
WO2014125839A8 (ja) 2015-08-06
RU2015139687A (ru) 2017-03-23
KR20150108385A (ko) 2015-09-25
CN105074043B (zh) 2017-07-28
CN105074043A (zh) 2015-11-18

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