EP1698706B1 - Method for annealing grain oriented magnetic steel sheet - Google Patents

Method for annealing grain oriented magnetic steel sheet Download PDF

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Publication number
EP1698706B1
EP1698706B1 EP04801652.1A EP04801652A EP1698706B1 EP 1698706 B1 EP1698706 B1 EP 1698706B1 EP 04801652 A EP04801652 A EP 04801652A EP 1698706 B1 EP1698706 B1 EP 1698706B1
Authority
EP
European Patent Office
Prior art keywords
compound
annealing
steel sheet
annealing separator
basic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP04801652.1A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1698706A4 (en
EP1698706A1 (en
Inventor
Takeshi Omura
Kazumichi SASHI
Yasuyuki Hayakawa
Masaki Kawano
Shinichi YOSHIKAWA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Steel Corp
Original Assignee
JFE Steel Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JFE Steel Corp filed Critical JFE Steel Corp
Priority to EP12006829.1A priority Critical patent/EP2559775B1/en
Publication of EP1698706A1 publication Critical patent/EP1698706A1/en
Publication of EP1698706A4 publication Critical patent/EP1698706A4/en
Application granted granted Critical
Publication of EP1698706B1 publication Critical patent/EP1698706B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • 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
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • 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

Definitions

  • a method for changing a component of an annealing separator has been attempted, that is, a method has been attempted in which an annealing separator containing no MgO which reacts with SiO 2 present on a steel sheet surface is applied after recrystallization annealing, followed by final annealing.
  • This grain-oriented electrical steel sheet has superior magnetic properties and superior coating properties of a forsterite coating.
  • the annealing separator be composed of an Al compound and a Si compound as a primary component, the ratio of the Al compound to the Si compound calculated based on Al 2 O 3 /(Al 2 O 3 +SiO 2 ) be 40 to 95 mass percent, and the annealing separator have a viscosity of 25 mPa ⁇ s or less and be in the form of a solution or a colloidal solution.
  • the ratio of the alumina sol to the silica sol was changed in the range of 20 to 100 mass percent based on Al 2 O 3 /(Al 2 O 3 +SiO 2 ), and the viscosity of the annealing separator was changed in the range of 3.5 to 100 mPa ⁇ s.
  • the viscosity of the annealing separator was changed by using an alumina sol having a different viscosity.
  • the viscosity of the alumina sol can be controlled, for example, by the shape of sol particles and the solid component ratio thereof.
  • the experimental results are shown which were obtained when the application amount was changed.
  • the application amount was excessively small, the annealing separation effect was insufficient, and sticking between steel sheets occurred.
  • the application amount was increased, the adhesion properties of the annealing separator to a steel sheet were degraded. Accordingly, in order to ensure superior adhesion properties to a steel sheet and to obtain the annealing separation effect, the application amount of the annealing separator is preferably controlled.
  • an Al compound in the form of a solution or a colloidal solution and a stable compound at a high temperature are used, that is, as the stable compound, at least one know compound other than MgO is used which has superior high temperature stability and which does not react or is unlikely to react in batch annealing.
  • the stable compound at a high temperature may be in the form of a solution or a colloidal solution as is the Al compound. That is the annealing separator may be in the form of a solution or a colloidal solution.
  • the annealing separator described above is very effective.
  • the Al compound is limited to a compound which forms colloid in a solvent such as water. That is, when the Al compound is not in a colloidal state, the film-forming effect cannot be obtained, and as a result, the adhesion properties cannot be obtained. For example, when alumina in the form of a slurry or suspension is applied, the film is not formed.
  • the particle diameter of the colloid of the Al compound is preferably set to approximately 50 nm or less. As for the lower limit, there is not preferable particle diameter limit, and even in the vicinity of the analytical limit, a sufficient effect can be obtained.
  • non-colloidal Al compound an Al compound which is not in the form of a solution nor a colloidal solution, such as alumina particles, is stable at a high temperature, the effect of improving the application properties of the Al compound in the form of a solution or a colloidal silica is not significant.
  • a compound which is stable at a high temperature other than the non-colloidal Al compound is preferably contained.
  • the non-colloidal Al compound is not taken into calculation of the solid component ratio which will be described later.
  • solid components of the above compounds are preferably calculated based on the following respective forms:
  • the content of C is more than 0.08 mass percent, it becomes difficult to decrease the content to 50 mass ppm or less (at which no magnetic aging occurs) in a manufacturing process, and hence the content is preferably set to 0.08 mass percent of less.
  • the lower limit is not necessarily determined, from an industrial point of view, the lower-limit is approximately 5 mass ppm.
  • the above elements are inversely added in accordance with the inhibitor which is to be used. For example, it is generally performed that when AlN is used as an inhibitor, 0.015 to 0.04 mass percent of Al and 0.005 to 0.015 mass percent of N are added; when BN is used, 0.001 to 0.006 mass percent of B and 0.005 to 0.015 mass percent of N are added; when MnSe and/or MnS is used, 0.005 to 0.06 mass percent of at least one of Se and S is added.
  • the balance is preferably composed of iron and inevitable impurities.
  • a slab having a common dimension may be manufactured by a common ingot casting method or continuous casting method or a thin cast slab (so-called thin slab) having a thickness of 100 mm or less may be manufactured by a direct casting method.
  • a slab is reheated and then hot-rolled by a common method; however, without performing heating after casting, hot rolling may be directly performed.
  • hot rolling may be performed, or without performing hot rolling, subsequent steps may be performed.
  • the temperature for hot-rolled steel sheet annealing is preferably increased to 800°C or more.
  • the hot-rolled steel sheet annealing temperature is preferably set to 1,100°C or less.
  • the hot-rolled steel sheet annealing temperature is preferably set in the range of 800 to 1,100°C.
  • a preferable annealing time of the hot-rolled steel sheet annealing is 1 to 300 seconds.
  • recrystallization annealing is performed.
  • intermediate annealing is performed between cold rolling steps.
  • the intermediate annealing is preferably performed at 900 to 1,200°C for approximately 1 to 300 seconds.
  • the recrystallization annealing is mainly performed in order to form a primary recrystallization texture and is preferably performed by continuous annealing.
  • a humid atmosphere is used; however, when decarburization is not required, a dry atmosphere may be used.
  • the temperature is 750 to 1,100°C and the time is approximately 1 to 300 seconds.
  • a technique in which the amount of Si is increased by siliconizing method may be applied to a steel sheet after, for example, the recrystallization annealing.
  • the technique for increasing the amount of Si by a siliconizing method may be further employed after the final annealing. This technique is effectively used in order to further decrease the iron loss.
  • a tensile coating is finally applied whenever necessary, followed by baking.
  • the shape may be corrected by flattening annealing, and furthermore, flattening annealing which simultaneously bakes the tensile coating may also be performed.
  • first batch annealing was performed.
  • An annealing separator shown in Table 5 was applied before or after the recrystallization annealing.
  • the application of the annealing separator was performed by a roll coater, and baking treatment was then performed at ultimate temperature (sheet temperature) of the steel sheet of 250°C, followed by spontaneous cooling.
  • the baking was performed by direct flame of a propane gas.
  • the first batch annealing was performed at 850°C for 40 hours in a nitrogen atmosphere, so that the secondary recrystallization was completed.
  • the order of the step of applying the annealing separator (classification was made whether the application was performed before or after the recrystallization annealing), the application properties of the annealing separators, the adhesion properties thereof after drying, and the annealing separation effect after the first batch annealing are shown in Table 6.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
EP04801652.1A 2003-12-03 2004-12-03 Method for annealing grain oriented magnetic steel sheet Expired - Lifetime EP1698706B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP12006829.1A EP2559775B1 (en) 2003-12-03 2004-12-03 Method for manufacturing a grain-oriented electrical steel sheet

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2003404520 2003-12-03
PCT/JP2004/018431 WO2005054523A1 (ja) 2003-12-03 2004-12-03 方向性電磁鋼板の焼鈍方法および方向性電磁鋼板の製造方法

Related Child Applications (2)

Application Number Title Priority Date Filing Date
EP12006829.1A Division EP2559775B1 (en) 2003-12-03 2004-12-03 Method for manufacturing a grain-oriented electrical steel sheet
EP12006829.1A Division-Into EP2559775B1 (en) 2003-12-03 2004-12-03 Method for manufacturing a grain-oriented electrical steel sheet

Publications (3)

Publication Number Publication Date
EP1698706A1 EP1698706A1 (en) 2006-09-06
EP1698706A4 EP1698706A4 (en) 2007-05-30
EP1698706B1 true EP1698706B1 (en) 2017-08-16

Family

ID=34650139

Family Applications (2)

Application Number Title Priority Date Filing Date
EP04801652.1A Expired - Lifetime EP1698706B1 (en) 2003-12-03 2004-12-03 Method for annealing grain oriented magnetic steel sheet
EP12006829.1A Expired - Lifetime EP2559775B1 (en) 2003-12-03 2004-12-03 Method for manufacturing a grain-oriented electrical steel sheet

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP12006829.1A Expired - Lifetime EP2559775B1 (en) 2003-12-03 2004-12-03 Method for manufacturing a grain-oriented electrical steel sheet

Country Status (6)

Country Link
EP (2) EP1698706B1 (ko)
KR (1) KR100774229B1 (ko)
CN (1) CN100513597C (ko)
ES (2) ES2643750T3 (ko)
TW (1) TWI272311B (ko)
WO (1) WO2005054523A1 (ko)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6323423B2 (ja) * 2015-09-25 2018-05-16 Ｊｆｅスチール株式会社 方向性電磁鋼板およびその製造方法
KR101850133B1 (ko) * 2016-10-26 2018-04-19 주식회사 포스코 방향성 전기강판용 소둔 분리제 조성물, 방향성 전기강판 및 방향성 전기강판의 제조방법
EP3546614B1 (en) * 2016-11-28 2021-01-06 JFE Steel Corporation Grain-oriented electromagnetic steel sheet and method for producing grain-oriented electromagnetic steel sheet
KR101906962B1 (ko) * 2016-12-22 2018-10-11 주식회사 포스코 방향성 전기강판용 소둔 분리제 조성물, 방향성 전기강판 및 방향성 전기강판의 제조방법
KR102541760B1 (ko) * 2019-01-08 2023-06-13 닛폰세이테츠 가부시키가이샤 방향성 전자 강판, 방향성 전자 강판의 제조 방법 및 방향성 전자 강판의 제조에 이용되는 어닐링 분리제

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US3794520A (en) * 1967-11-06 1974-02-26 Westinghouse Electric Corp Nonreactive refractory separating coatings for electrical steels
US3785882A (en) * 1970-12-21 1974-01-15 Armco Steel Corp Cube-on-edge oriented silicon-iron having improved magnetic properties and method for making same
JPS5573823A (en) * 1978-11-28 1980-06-03 Nippon Steel Corp Annealing release material for electrical steel sheet
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JP2674917B2 (ja) 1991-12-06 1997-11-12 新日本製鐵株式会社 フォルステライト被膜のない高磁束密度方向性珪素鋼板の製造方法
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JPH06136448A (ja) 1992-10-26 1994-05-17 Nippon Steel Corp 方向性珪素鋼板の製造方法
JP2679944B2 (ja) 1993-10-26 1997-11-19 新日本製鐵株式会社 鉄損の低い鏡面方向性電磁鋼板の製造方法
JPH08134542A (ja) 1994-11-08 1996-05-28 Sumitomo Metal Ind Ltd 打抜き性に優れた方向性電磁鋼板の製造方法
JPH08188828A (ja) * 1995-01-06 1996-07-23 Nippon Steel Corp 焼鈍分離剤用懸濁液
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EP1279747B1 (en) * 2001-07-24 2013-11-27 JFE Steel Corporation A method of manufacturing grain-oriented electrical steel sheets
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Also Published As

Publication number Publication date
EP2559775B1 (en) 2018-04-18
KR100774229B1 (ko) 2007-11-07
CN1890390A (zh) 2007-01-03
EP1698706A4 (en) 2007-05-30
ES2673149T3 (es) 2018-06-20
TWI272311B (en) 2007-02-01
KR20060103517A (ko) 2006-10-02
EP2559775A1 (en) 2013-02-20
WO2005054523A1 (ja) 2005-06-16
CN100513597C (zh) 2009-07-15
EP1698706A1 (en) 2006-09-06
TW200525042A (en) 2005-08-01
ES2643750T3 (es) 2017-11-24

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