EP0099619A2 - Method for producing cube-on-edge oriented silicon steel - Google Patents

Method for producing cube-on-edge oriented silicon steel Download PDF

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Publication number
EP0099619A2
EP0099619A2 EP83302013A EP83302013A EP0099619A2 EP 0099619 A2 EP0099619 A2 EP 0099619A2 EP 83302013 A EP83302013 A EP 83302013A EP 83302013 A EP83302013 A EP 83302013A EP 0099619 A2 EP0099619 A2 EP 0099619A2
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EP
European Patent Office
Prior art keywords
silicon steel
annealing
steel
texture annealing
manganese
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.)
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Application number
EP83302013A
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German (de)
French (fr)
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EP0099619A3 (en
Inventor
Robert Frederick Miller
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Allegheny Ludlum Steel Corp
Original Assignee
Allegheny Ludlum Steel Corp
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Filing date
Publication date
Application filed by Allegheny Ludlum Steel Corp filed Critical Allegheny Ludlum Steel Corp
Publication of EP0099619A2 publication Critical patent/EP0099619A2/en
Publication of EP0099619A3 publication Critical patent/EP0099619A3/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
    • C21D1/70—Temporary coatings or embedding materials applied before or during heat treatment while heating or quenching
    • 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
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • 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
    • C21D8/1294—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a localized treatment

Definitions

  • This invention relates to a method of producing cube-on-edge oriented silicon steel in the form of sheets is known for use in various electrical applications including transformer cores.
  • the alloy is characterized by secondary recrystallization in the (110) (001) position, which is termed the cube-on-edge position.
  • This material in sheet form has the direction of easy magnetization in the direction of rolling.
  • the material is required to have reduced watt loss, because the consumption of electrical energy decreases as iron loss decreases. Reduced watt loss may be promoted by achieving fine secondary grain size during texture annealing.
  • a silicon steel which has been conventionally processed by hot rolling and cold rolling with intermediate anneals is surface coated with a manganese-bearing material prior to texture annealing and is texture annealed in the conventional manner with said manganese-bearing material thereon.
  • a manganese-bearing material particularly suited for use in the invention is Mn 3 (N0 2 ). It has been found that the presence of the manganese-bearing compound during annealing inhibits secondary grain growth and thus reduces watt loss. This may be further enhanced if the steel is serrated prior to texture annealing.
  • the practice of the invention finds utility with cube-on-edge oriented silicon steels generally, it is particularly adapted to steels of this type within the following composition limits in percent by weight:
  • Epstein packs of final normalized SX-14 composition identified as Heat No. 154684, were coated with a water slurry comprising 300cc of water, 46gm. of MgO and 2gm. of H 3 B0 3 .
  • This material with the coating thereon was then texture annealed in a hydrogen atmosphere in the conventional manner.
  • the texture annealing consisted of charging the material into a furnace at a temperature of 760°C (1400°F) heating at a rate of 10°C (50°F) per hour to a temperature of 1177 0 C (2150°F), holding at temperature for 12 hours and then cooling to 649 0 C (1200°F), at which time the material was removed from the furnace.
  • Epstein packs Prior to the above slurry coating, was painted with a mixture of 30cc of 50% Mn (N0 3 ) 2 and an inert thickner, which was applied in lmm stripes perpendicular to the sheet rolling direction at intervals of lOmm; this painted coating was then air dried.
  • This Epstein pack constituted treatment in accordance with the practice of the invention; whereas, the second pack was used as a control and typified a conventional practice.
  • the average lineal dimension of the secondary grains of the conventional, control pack specimen in the sheet rolling direction was l3mm.
  • the average lineal dimension of the secondary grain of the specimen treated with Mn(N0 3 ) 2 in accordance with the practice of the invention was 7mm; these grains it was observed were often separated by the aforementioned bands of smaller primary grains where normal grain growth was stimulated by the application of the manganese-bearing compound.
  • a single Epstein strip of final normalized SX-14 composition from the same heat as in the aforementioned Example 1 was scribed with a metal scribe to produce serrations in the strip perpendicular to the rolling direction at intervals of lOmm.
  • the strip was slurry coated and texture annealed under the conditions described above with respect to the first specific example. Following this texture annealing, the average lineal dimension in the sheet rolling direction of the secondary grain in the scribed strip was 9.5mm.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Metal Rolling (AREA)

Abstract

An improvement in the manufacture of cube-on-edge oriented silicon steel; the improvement comprises coating the surface of the silicon steel with a manganese-bearing material prior to texture annealing, whereby secondary grain growth is inhibited during texture annealing to achieve reduced watt loss.

Description

  • This invention relates to a method of producing cube-on-edge oriented silicon steel in the form of sheets is known for use in various electrical applications including transformer cores..With cube-on-edge silicon steel the alloy is characterized by secondary recrystallization in the (110) (001) position, which is termed the cube-on-edge position. This material in sheet form has the direction of easy magnetization in the direction of rolling. In applications for this material, and specifically when used in the manufacture of transformer cores, the material is required to have reduced watt loss, because the consumption of electrical energy decreases as iron loss decreases. Reduced watt loss may be promoted by achieving fine secondary grain size during texture annealing.
  • It is accordingly an object of the present invention to provide a method whereby during the texture annealing of cube-on-edge silicon steel the secondary grain growth is inhibited to provide a relatively fine grained material after texture annealing with reduced watt loss.
  • Broadly, in the practice of the invention a silicon steel which has been conventionally processed by hot rolling and cold rolling with intermediate anneals is surface coated with a manganese-bearing material prior to texture annealing and is texture annealed in the conventional manner with said manganese-bearing material thereon. A manganese-bearing material particularly suited for use in the invention is Mn3(N02). It has been found that the presence of the manganese-bearing compound during annealing inhibits secondary grain growth and thus reduces watt loss. This may be further enhanced if the steel is serrated prior to texture annealing. Although the practice of the invention finds utility with cube-on-edge oriented silicon steels generally, it is particularly adapted to steels of this type within the following composition limits in percent by weight:
    Figure imgb0001
  • By the practice of coating steel with a manganese-bearing compound and texture annealing with the compound being present on the steel, said practice is believed to be effective for the purpose by diffusing manganese into the steel during annealing, which promotes primary grain coarsening by interaction with the solute sulfur, which sulfur would tend to inhibit grain growth. Hence a region is provided in which primary grain growth occurs and restricts the growth of secondary grains through this region. It would appear that the extent of grain refinement of the secondary grains after texture annealing depends on the spacing of the regions of primary grain growth on the areas of application of the manganese-containing material, provided that the width of the treated region is sufficient to act as a barrier to the secondary grains. This effect may be supplemented by creating similar barriers by subjecting the steel to serrating or the like.
  • The silicon steel composition used in the specific examples, and identified as SX-14, was of the following nominal composition in percent by weight:
    Figure imgb0002
  • Epstein packs of final normalized SX-14 composition, identified as Heat No. 154684, were coated with a water slurry comprising 300cc of water, 46gm. of MgO and 2gm. of H3B03. This material with the coating thereon was then texture annealed in a hydrogen atmosphere in the conventional manner. Specifically, the texture annealing consisted of charging the material into a furnace at a temperature of 760°C (1400°F) heating at a rate of 10°C (50°F) per hour to a temperature of 11770C (2150°F), holding at temperature for 12 hours and then cooling to 6490C (1200°F), at which time the material was removed from the furnace. One of the Epstein packs, prior to the above slurry coating, was painted with a mixture of 30cc of 50% Mn (N03)2 and an inert thickner, which was applied in lmm stripes perpendicular to the sheet rolling direction at intervals of lOmm; this painted coating was then air dried..This Epstein pack constituted treatment in accordance with the practice of the invention; whereas, the second pack was used as a control and typified a conventional practice. Following the texture annealing procedure, as described above, the average lineal dimension of the secondary grains of the conventional, control pack specimen in the sheet rolling direction was l3mm. In contrast, the average lineal dimension of the secondary grain of the specimen treated with Mn(N03)2 in accordance with the practice of the invention was 7mm; these grains it was observed were often separated by the aforementioned bands of smaller primary grains where normal grain growth was stimulated by the application of the manganese-bearing compound.
  • In a second specific example, a single Epstein strip of final normalized SX-14 composition from the same heat as in the aforementioned Example 1 was scribed with a metal scribe to produce serrations in the strip perpendicular to the rolling direction at intervals of lOmm. After the scribing operation, the strip was slurry coated and texture annealed under the conditions described above with respect to the first specific example. Following this texture annealing, the average lineal dimension in the sheet rolling direction of the secondary grain in the scribed strip was 9.5mm.

Claims (3)

1. A method of producing cube-on-edge oriented silicon steel, characterized by reduced watt loss, including the steps of hot-rolling, cold-rolling with intermediate annealing and a final texture annealing, characterized in comprising surface coating said steel with a manganese-bearing material prior to texture annealing and texture annealing said steel with said coating thereon, whereby secondary grain growth is inhibited during texture annealing.
2. A method according to claim 1, characterized in that said manganese-bearing material is Mn(NO3)2.
3. A method according to claims 1 or 2, characterized in that said steel is serrated prior to texture annealing.
EP83302013A 1982-07-19 1983-04-11 Method for producing cube-on-edge oriented silicon steel Withdrawn EP0099619A3 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US39968082A 1982-07-19 1982-07-19
US399680 1982-07-19

Publications (2)

Publication Number Publication Date
EP0099619A2 true EP0099619A2 (en) 1984-02-01
EP0099619A3 EP0099619A3 (en) 1984-07-25

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Family Applications (1)

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Country Status (6)

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EP (1) EP0099619A3 (en)
JP (1) JPS5928524A (en)
KR (1) KR890000126B1 (en)
BR (1) BR8301545A (en)
CA (1) CA1194386A (en)
PL (1) PL242750A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0225619A2 (en) * 1985-12-06 1987-06-16 Nippon Steel Corporation Grain-oriented electrical steel sheet having improved glass film properties and low watt loss and a process for producing same
EP0239688A1 (en) * 1986-04-03 1987-10-07 Nippon Steel Corporation Annealing separator used in the finishing annealing step for producing a grain-oriented electrical steel sheet

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB922521A (en) * 1959-03-05 1963-04-03 Gen Electric Improvements in coated metallic sheet material and method of making same
GB1183092A (en) * 1966-03-18 1970-03-04 Yawata Iron & Steel Co Method of Forming Electric Insulating Films on Al-Containing Silicon Steel Sheet and Surface-Coated Al-Containing Silicon Steel Sheet
GB1279334A (en) * 1969-07-07 1972-06-28 Kawasaki Steel Co Method of producing insulative coating on the surface of silicon steel sheet
FR2268868A1 (en) * 1974-04-25 1975-11-21 Nippon Steel Corp
GB2011481A (en) * 1977-12-27 1979-07-11 Allegheny Ludlum Ind Inc Silicon steel and processing therefor

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5021928A (en) * 1973-06-28 1975-03-08

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB922521A (en) * 1959-03-05 1963-04-03 Gen Electric Improvements in coated metallic sheet material and method of making same
GB1183092A (en) * 1966-03-18 1970-03-04 Yawata Iron & Steel Co Method of Forming Electric Insulating Films on Al-Containing Silicon Steel Sheet and Surface-Coated Al-Containing Silicon Steel Sheet
GB1279334A (en) * 1969-07-07 1972-06-28 Kawasaki Steel Co Method of producing insulative coating on the surface of silicon steel sheet
FR2268868A1 (en) * 1974-04-25 1975-11-21 Nippon Steel Corp
GB2011481A (en) * 1977-12-27 1979-07-11 Allegheny Ludlum Ind Inc Silicon steel and processing therefor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0225619A2 (en) * 1985-12-06 1987-06-16 Nippon Steel Corporation Grain-oriented electrical steel sheet having improved glass film properties and low watt loss and a process for producing same
EP0225619A3 (en) * 1985-12-06 1989-02-22 Nippon Steel Corporation Grain-oriented electrical steel sheet having improved glass film properties and low watt loss and a process for producing same
US4897131A (en) * 1985-12-06 1990-01-30 Nippon Steel Corporation Grain-oriented electrical steel sheet having improved glass film properties and low watt loss
US5028279A (en) * 1985-12-06 1991-07-02 Nippon Steel Corporation Grain oriented electrical steel sheet having improved glass film properties and low watt loss and process for producing same
EP0239688A1 (en) * 1986-04-03 1987-10-07 Nippon Steel Corporation Annealing separator used in the finishing annealing step for producing a grain-oriented electrical steel sheet

Also Published As

Publication number Publication date
EP0099619A3 (en) 1984-07-25
JPH0515765B2 (en) 1993-03-02
JPS5928524A (en) 1984-02-15
BR8301545A (en) 1984-04-17
KR840004174A (en) 1984-10-10
PL242750A1 (en) 1984-03-12
CA1194386A (en) 1985-10-01
KR890000126B1 (en) 1989-03-08

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Inventor name: MILLER, ROBERT FREDERICK