# US 9,038,429 B2 · Method for manufacturing grain-oriented silicon steel with single cold rolling

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- Number: US 9,038,429 B2
- Document ID: US9038429B2
- Status: Granted
- Kind: B2
- Application number: 13/142,955
- Filed: 2009-12-31
- Published: 2012-01-05
- Granted: 2015-05-26
- Earliest claimed: 2008-12-31
- Assignees: Baoshan Iron & Steel Co., Ltd.
- Applicants: Guobao Li; Pijun Zhang; Yongjie Yang; Kanyi Shen; Zhuochao Hu; Peiwen Wu; Weizhong Jin; Quanli Jiang
- Inventors: Guobao Li; Pijun Zhang; Yongjie Yang; Kanyi Shen; Zhuochao Hu; Peiwen Wu; Weizhong Jin; Quanli Jiang
- Web page: https://patentgrep.com/patent/US9038429B2

## CPC

- C21D 8/12: during manufacturing of articles with special electromagnetic properties
- C21D 8/1233: {Cold rolling}
- C21D 8/1255: {with diffusion of elements, e.g. decarburising, nitriding}
- C21D 8/1272: {Final recrystallisation annealing}
- C21D 8/1283: {Application of a separating or insulating coating}
- C21D 9/46: for sheet metals
- C22C 38/001: {containing N}
- C22C 38/008: {containing tin}
- C22C 38/02: containing silicon
- C22C 38/04: containing manganese
- C22C 38/06: containing aluminium
- C22C 38/16: containing copper
- H01F 1/14775: {in the form of sheets}
- B21B 1/36: by cold-rolling
- B21B 3/00: Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences {; Rolling of aluminium, copper, zinc or other non-ferrous metals}(altering special metallurgical properties of alloys, other than structure consolidation or mechanical properties resulting therefrom C21D, C22F)
- B21B 9/00: Measures for carrying out rolling operations under special conditions, e.g. in vacuum or inert atmosphere to prevent oxidation of work; Special measures for removing fumes from rolling mills
- C21D 1/28: Normalising
- 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 (surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by this subclass C23F17/00; unidirectional solidification of eutectic materials or unidirectional demixing of eutectoid materials C30B)
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- H01F: MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- B21B: ROLLING OF METAL (auxiliary operations used in connection with metal-working operations covered in B21, see B21C; bending by rolling B21D; manufacture of particular objects, e.g. screws, wheels, rings, barrels, balls, by rolling B21H; pressure welding by means of a rolling mill B23K20/04)

## Abstract

The invention provides a method for producing grain-oriented silicon steel with single cold rolling, comprising: 1) smelting, refining and continuous casting to obtain a casting blank; 2) hot rolling; 3) normalization, i.e. normalizing annealing and cooling; 4) cold-rolling, i.e. single cold rolling at a cold rolling reduction rate of 75-92%; 5) decarburizing annealing at 780-880° C. for 80-350 s in a protective atmosphere having a due point of 40-80° C., wherein the total oxygen [O] in the surface of the decarburized sheet: 171/t≦[O]≦313/t (t represents the actual thickness of the steel sheet in mm), the amount of absorbed nitrogen: 2-10 ppm; 6) high temperature annealing, wherein the dew point of the protective atmosphere: 0-50° C., the temperature holding time at the first stage: 6-30 h, the amount of absorbed nitrogen during high-temperature annealing: 10-40 ppm; 7) hot-leveling annealing. The invention may control the primary recrystallization microstructure of steel sheet effectively by controlling the normalization process of hot rolled sheet to form sufficient favorable (Al, Si)N inclusions from nitrogen absorbed by slab during decarburizing annealing and low-temperature holding of high-temperature annealing, facilitating the generation of stable, perfect secondary recrystallization microstructure of the final products. In addition, the invention avoids the impact of nitridation using ammonia on the underlying layer in prior art, and thus the formation of a good glass film underlying layer is favored.

## Claims

### Claim 1

A method for producing grain-oriented silicon steel with single cold rolling, comprising:
1) smelting:
after secondary refining and continuous casting of molten steel in a converter or an electric furnace, a casting blank having the following composition based on mass is obtained: C 0.035-0.065%, Si 2.9-4.0%, Mn 0.08-0.18%, S 0.005-0.012%, Als 0.015-0.035%, N 0.0050-0.0130%, Sn 0.001-0.15%, P 0.010-0.030%, Cu 0.05-0.60%, Cr≦0.2%, balanced by Fe and unavailable inclusions;
2) hot rolling:
the casting blank is heated to 1090-1200° C. in a heating furnace, rolling begins at a temperature below 1180° C. and ends at a temperature above 860° C., and a hot rolled steel sheet of 1.5-3.5 mm is thus obtained and then coiled at 500-650° C.;
3) normalization:
normalizing annealing is carried out at 1050-1180° C. (1-20 s)+850-950° C. (30-200 s), and cooling is carried out at 10° C./s-60° C./s;
4) cold rolling:
the steel sheet is rolled to a thickness of a final product with single cold rolling at a cold rolling reduction rate of 75-92%;
5) decarburization:
the steel sheet rolled to the thickness of the final product is decarburizing annealed at 780-880° C. for 80-350 s in a protective mixed gas atmosphere of H2 and N2 comprising 15-85% H2, a dew point of the protective mixed gas atmosphere is 40-80° C., a total oxygen [O] in a surface of the decarburized steel sheet is 171/t≦[O]≦313/t (t represents an actual thickness of the steel sheet in mm), an amount of absorbed nitrogen is 2-10 ppm, then the sheet is coated with a high-temperature annealing separator comprising MgO as a main component;
6) high-temperature annealing:
a protective annealing atmosphere below 1000° C. is comprised of a mixed gas of H2 and N2 or pure N2 and has a dew point of 0-50° C., a temperature holding time at a first stage is 6-30 h, an amount of absorbed nitrogen during high-temperature annealing is 10-40 ppm; and
7) hot leveling annealing:
a conventional hot leveling process is carried out,
wherein at ¼-⅓ and ⅔-¾ of the thickness of the normalized steel sheet, a ratio of Gaussian texture (110)[001] to cubic texture (001)[110] is controlled to be 0.2≦I(110)[001]/I(001)[110]≦8, wherein I(110)[001] and I(001)[110] are intensities of Gaussian and cubic texture respectively.

### Claim 2 (depends on 1)

The method of claim 1 for producing grain-oriented silicon steel with single cold rolling, wherein based on the foregoing basic composition, into the grain-oriented silicon steel may be further added 0.01-0.10% Mo and/or ≦0.2% Sb based on mass.

### Claim 3 (depends on 1)

The method of claim 1 for producing grain-oriented silicon steel with single cold rolling, wherein a number of crystal grains with Gaussian texture at ¼-⅓ and ⅔-¾ of the thickness of the normalized steel sheet is not less than 5% of a total number of crystal grains.

### Claim 4 (depends on 1)

The method of claim 1 for producing grain-oriented silicon steel with single cold rolling, wherein the temperature holding time at the first stage for steel coil ≧5 tons is 8-15 h.

### Claim 5

A method for producing grain-oriented silicon steel with single cold rolling, comprising:
1) smelting:
after secondary refining and continuous casting of molten steel in a converter or an electric furnace, a casting blank having the following composition based on mass is obtained: C 0.035-0.065%, Si 2.9-4.0%, Mn 0.08-0.18%, S 0.005-0.012%, Als 0.015-0.035%, N 0.0050-0.0130%, Sn 0.001-0.15%, P 0.010-0.030%, Cu 0.05-0.60%, Cr≦0.2%, balanced by Fe and unavailable inclusions;
2) hot rolling:
the casting blank is heated to 1090-1200° C. in a heating furnace, rolling begins at a temperature below 1180° C. and ends at a temperature above 860° C., and a hot rolled steel sheet of 1.5-3.5 mm is thus obtained and then coiled at 500-650° C.;
3) normalization:
normalizing annealing is carried out at 1050-1180° C. (1-20 s)+850-950° C. (30-200 s), and cooling is carried out at 10° C./s-60° C./s;
4) cold rolling:
the steel sheet is rolled to a thickness of a final product with single cold rolling at a cold rolling reduction rate of 75-92%;
5) decarburization:
the steel sheet rolled to the thickness of the final product is decarburizing annealed at 780-880° C. for 80-350 s in a protective mixed gas atmosphere of H2 and N2 comprising 15-85% H2, a dew point of the protective mixed gas atmosphere is 40-80° C., a total oxygen [O] in a surface of the decarburized steel sheet is 171/≦[O]≦313/t (t represents an actual thickness of the steel sheet in mm), an amount of absorbed nitrogen is 2-10 ppm, then the sheet is coated with a high-temperature annealing separator comprising MgO as a main component;
6) high-temperature annealing:
a protective annealing atmosphere below 1000° C. is comprised of a mixed gas of H2 and N2 or pure N2 and has a dew point of 0-50° C., a temperature holding time at a first stage is 6-30 h, an amount of absorbed nitrogen during high-temperature annealing is 10-40 ppm; and
7) hot leveling annealing:
wherein a ratio of Gaussian texture (110)[001] to cubic texture (001)[110] is controlled to be 0.5≦I(110)[001]/I(001)[110]≦2.

### Claim 6 (depends on 5)

The method of claim 5 for producing grain-oriented silicon steel with single cold rolling, wherein based on the foregoing basic composition, into the grain-oriented silicon steel may be further added 0.01-0.10% Mo and/or ≦0.2% Sb based on mass.

### Claim 7 (depends on 5)

The method of claim 5 for producing grain-oriented silicon steel with single cold rolling, wherein a number of crystal grains with Gaussian texture at ¼-⅓ and ⅔-¾ of the thickness of the normalized steel sheet is not less than 5% of a total number of crystal grains.

### Claim 8 (depends on 5)

The method of claim 5 for producing grain-oriented silicon steel with single cold rolling, wherein the temperature holding time at the first stage for steel coil ≧5 tons is 8-15 h.