US3392063A - Grain-oriented iron and steel and method of making same - Google Patents

Grain-oriented iron and steel and method of making same Download PDF

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US3392063A
US3392063A US467228A US46722865A US3392063A US 3392063 A US3392063 A US 3392063A US 467228 A US467228 A US 467228A US 46722865 A US46722865 A US 46722865A US 3392063 A US3392063 A US 3392063A
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sulfur
iron
low carbon
grain
orientation
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Dale M Kohler
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Armco Inc
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Armco Inc
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Priority to FR83398A priority patent/FR1525917A/fr
Priority to BE689584D priority patent/BE689584A/xx
Priority to GB50579/66A priority patent/GB1142552A/en
Priority to DE19661508366 priority patent/DE1508366A1/de
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G6/00—Condensation polymers of aldehydes or ketones only
    • 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
    • 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
    • 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

Definitions

  • the invention relates to a method of producing oriented iron-base alloys and more particularly to a method of making preferred crystallographic orientations in ingot iron and low carbon steel, and the products made thereby.
  • ingot iron and low carbon steel can be made to have at least two highly preferred crystallographic orientations which impart useful properties to a polycrystalline sheet or strip. These textures are strong in that more than half of the total grain structure will have the preferred textures.
  • ingot iron and low carbon steel ferrous materials which by ladle analysis contain up to about 0.10% carbon, 0.01 to 0.40% manganese (preferably about 0.03 to about 0.12%), up to about 0.05% sulfur, up to about 0.03% phosphorus, up to about 0.25% copper, the balance being iron except for normal amounts of those impurities incident to the manufacture of such material.
  • the ingot iron and low carbon steel may also contain a small amount of aluminum. Silicon may also be present as a deoxidizer in small amounts, or additions up to about 1.8% may be made to increase the Volume resistivity of the product when it is used for magnetic properties.
  • the amount of silicon added may be consistent with that found in hitherto known non-oriented silicon steels, and is dictated by the phase boundary between alpha iron and gamma iron.
  • the carbon and manganese contents will determine whether the material is classified as ingot iron or low carbon steel, the latter usually containing upwards of 0.05% carbon and 0.20%
  • the two highly preferred crystallographic orientations which ingot iron and low carbon steel may be made to have in accordance with the teachings of this invention are classified by Millers indices as (110) [001] and (112) [110].
  • the (110) [001] orientation is known as cube-on-edge.
  • material with this orientation made from ingot iron and low carbon steel in accordance with the teachings of this invention will have some magnetic properties substantially as good as or better than those found in 3% oriented silicon-iron presently in commercial use.
  • ⁇ it has been impossible to obtain highly oriented cube-on-edge "ice low carbon steel or ingot iron without the use of at least 2% silicon.
  • the (112) [1110] orientation is a form of cube-oncorner texture never heretofore obtained in substantial proportions in ferrous material. As will be described hereinafter material having this orientation and made in accordance with this invention will have good forming properties.
  • lt is an object of the present invention to provide a method for making highly preferred crystallographic orientations in ingot iron and low carbon steel.
  • ingot iron and low carbon steel may be made to have a (110) [001] orientation and wherein more than half of the total grain structure will be characterized by this orientation.
  • lt is an object of the present invention to provide ingot iron and low carbon steel having a (112) [110] orientation and wherein more than half of the total grain structure is characterized by this orientation.
  • FIG. l is a photomicrograph at a magnification of 50X showing the preferred uniform fine-grained structure ⁇ of the hot rolled material of the present invention.
  • FIG. 2 is a photomicrograph at a magnification of 5 0 showing the hot rolled material of the present invention with undesirably large grains at the surfaces.
  • FIG. 3 is a photomicrograph at a magnication of showing a hot rolled material in which large surface grains such as those illustrated in FIG. 2 are not refined and persist after rolling and decaburization.
  • FIG. 4 is a photomicrograph at a magnification of 100x showing a hot rolled material in which large surface grains are not refined and persist after cold rolling, decarburization and the final anneal.
  • FIG. 5 is a photomicrograph at ⁇ a magnification of 100x showing the material of the present invention after hot rolling, cold Arolling and decarburization, wherein the grains after hot rolling were in ideal condition.
  • FIG. 6 is a (100) optical pole figure showing oriented iron having a [001] texture.
  • FlG. 7 is a (100) optical pole figure showing oriented iron having a (112) [110] texture.
  • FIG. 8 is a graph comparing the DC magnetization curves for oriented ingot iron of the present invention with the curves for conventional magnetic ingot iron, nonoriented silicon steel and oriented 3% silicon-iron.
  • the invention is based on the discovery that the recrystallization texture of ingot iron and low carbon steel can be changed by promoting as a final step in the processing the growth of grains having the preferred orientations at the expense of grains of other orientations, a phenomenon referred to as secondary recrystallization.
  • the manufacturer of low carbon ferrous materials contemplates hot and cold rolling steps to attain a desired final gauge, and an anneal slightly below the A1 or lower critical temperature to soften the material by recrystallizing the grain structure. It has been found that subjecting the material during this final anneal to higher 'temperatures or longer times at temperature will tend to increase the grain size, but will have little effect on the orientation of the grains. This is true because the material undergoes a prima-ry recrystallization and an indiscriminate and non-selective grain growth rather than a secondary recrystallization with selective grain growth.
  • a high degree of preferred orientation can be achieved in accordance with the teachings of this invention by causing sulfur to be diffused into the grain boundaries of the primary ⁇ grains and thus restricting their growth. This makes possible a secondary recrystallization with the results above noted.
  • the ingot iron or low carbon steel may be produced by any of the known melting and refining processes. When low carbon steel is used, it may be either rrimming or killed steel; but, if it is killed steel, silicon killed steel is preferred.
  • the low carbon iron or steel may be cast continuously or intermittently into ingots, billets or slabs. It may be 4hot rolled to any thickness which the rolling apparatus can produce. Depending upon ⁇ the desired cold reduetions which follow the hot rolling, and the desired final gauge of the final product, the hot rolled band may vary in thickness from about 0.125 to about 0.050 inch with present equipment.
  • the hot rolling procedure may be varied with regard to the Itemperature of the stock when it is heated for rolling, when it enters the rolling mill, when it is rolled to various intermediate thicknesses, and when it is cooled to ambient temperatures. These temperatures are well established for ingot iron land low car-bon steel destined for particular end uses; and these practices can be followed for the ,material of the present invention.
  • the grain s-ize of the material after hot rolling and before cold rolling be relatively small and uniform throughout ythe thickness of the material.
  • the preferred temperature for finishing the bot rolling of low carbon steels is above about 1600 F. in order to obtain a fine grain structure.
  • Such a desired fine grain structure is illustrated in the photomicrograph of FIG. 1. Ingot iron will be finished at a lower temperature in the conventional manner. Coiling temperatures below 1300 F. are preferred for both ingot iron and low carbon steel to prevent excessive grain growth.
  • the material may be subjected to an open anneal or normalizing heat treatment. While decarburization may be effected during this step, it is preferred to remove the carbon -at a later stage, as hereinafter described.
  • the principal purpose of the heat treatment following the hot rolling is to refine and equalize the grain structure. This may be accomplished by a continuous or strand normalizing treatment comprising a short-time heating above the A3 or upper critical point (about 1625 F.). A temperature of about 1800 F. is satisfactory. It has been found that if large grains remain at the surface of the material after hot rolling (as shown in FIG.
  • FIG. 5 is a photomicrograph showing the ideal grain structure after decarburization, where the grain structure after hot rolling was similar to that shown in FIG. 1, or was refined by a normalizing treatment. For reasons of economy, it is preferable to obtain after hot rolling a grain structure of lthe type shown in FIG. 1, thereby eliminating the normalizing step.
  • the ingot iron or low carbon steel having-a lgrain condition similar to that shown in FIG. 1, is cold rolled in one or more stages to obtain the desired final gauge.
  • a single stage cold reduction is often preferred for reasons of economy, since multiple stage cold reductions require an anneal between stages.
  • the intermediate anneal should be an open anneal at a temperature between about 1100 F. and about l800 F. in a reducing atmosphere, which may be a decarburizing atmosphere, if pickling is to be avoided. If the atmosphere is oxidizing, pickling will be necessary.
  • the amount of cold reduction in each stage should be less than Reductions of between about 50% and 85% have been found satisfactory.
  • the cold reduction should be 90% or more in a single stage process. With cold reductions of two or more stages, with intermediate anneals, only the last cold rolling stage must be 90% or greater. Reductions of 90% have produced excellent results in obtaining a (112) [110] orientation in the final product. The maximum reduction is limited only by the capacity of the rolling -mill yand the ability ⁇ of the material to withstand a drastic deformation.
  • decarburization may be carried on prior to the cold rolling. However, it is preferred to decarburize after cold rolling. Decarburization is preferably accomplished by a continuous anneal for a -few minutes in a wet hydrogen-bearing atmosphere at about 1500 F. as is Well known in the art (see U.S. Patent No. 2,307,- 391). The temperature may be varied from l200 F. to about l600 F. and less expensive hydrogen-bearing gases such as dissociated ammonia may be used. The final carbon content should be less than 0.01% and for some uses less than 0.005%. Decarburization can also be performed in a box anneal. Denitriding to less than .001% nitrogen may also be effected during the decarburizing anneal or in one of the other annealing treatments.
  • the final treatment will be a box anneal at a temperature just below the upper critical or A3 temperature in a reducing, non-oxidizing atmosphere.r
  • the iron or low carbon steel must be maintained in the alpha phase but, because of the loss of carbon in the decarburizing step, the upper critical temperature or A3 temperature is then about 1650'J F.
  • a temperature of about 1550a F. will be sufficient if the time at temperature is forty-eight hours or more.
  • a preferred temperature range is about 1600 F. to about 1650 F. and with such a restricted temperature range the time at temperature may be less than twentyfour hours.
  • a high degree of preferred orientation can be achieved in the ingot iron or low carbon steel by causing sulfur to be diffused into the grain boundaries of the primary grains, thus restricting their growth and making possible a secondary recrystallization -with selectivefgraingrowth. This is accomplished by treatment of the ingot iron or low carbon steel with sulfur or sulfur compounds at final gauge and immediately prior to or during the primary grain growth portion of an anneal. There are various ways in which this can be done.
  • the invention can be practiced by the addition of ferrous sulfide or other sulfur compounds, which dissociate or decompose at the temperatures of primary grain growth, to the annealing separator employed during the final heat treatment. Elemental sulfur can also be added to the separator for the same purpose,
  • the preferred annealing separators are magnesia, alumina or calcium oxide or mixtures of these in finely divided form although other substances may be used, if desired, such as titania and other refractory metal oxides.
  • the final anneal which may include both a primary recrystallization and a secondary recrystallization is usually an anneal in dry hydrogen in a mufiie or box.
  • the anneal may be carried on with the material in the form of stacked sheets or wound coils; and if the'atmosphere of the annealing is required to act upon the ingot iron or low carbon steel, excellent results may be obtained by annealing in loose coils formed in accordance with modern techniques. Whether or not the material exists as sheets in a stack or as convolutions of a coil, it is preferred that the quantity of the sulfur-bearing material at the surfaces of the stock be maintained within certain limits as later set forth.
  • the sulfur or sulfur compound reacts with the dry hydrogen annealing atmosphere to form hydrogen sulfide; that the sulfur is transferred to the steel by means of hydrogen sulfide as a carrier; and that the hydrogen sulfide reacts with the steel to form sulfides at the grain boundaries.
  • the reaction occurs while the furnace temperature is between about 1000 F. and 1650 F.
  • the absorption of sulfur creates high sulfur concentrations at the grain boundaries of the primary structure tending to prevent the primary grain structure from undergoing such grain growth as would interfere with subsequent secondary recrystallization.
  • a finely grained matrix is maintained until secondary grains of the preferred orientation begin to consume the grains of other orientations. Thereafter as the temperature rises further, secondary grain growth will proceed by grain boundary energy and will convert the fine grain matrix into a well developed structure of preferred orientation.
  • the sulfur or sulfur-bearing compound may be made available at the surfaces of the sheet material during a decarburizing anneal prior to the final anneal.
  • a decarburizing anneal prior to the final anneal.
  • the ingot iron or low carbon steel strip is moved through an elongated furnace containing a special atmosphere for removing carbon, it is possible to mix hydrogen sulfide with the decarburizing atmosphere to form a controlled iron sulde film on the material which will inhibit the primary grain growth which continues during the subsequent final anneal.
  • the amount of elemental sulfur or sulfur in the form of a sulfur-bearing compound added to the annealing separator may be from about 1/2% to about 10% of the annealing separator by weight, when the separator is applied in a quantity of about ten pounds per ton of ingot iron or low carbon steel. It has been found that secondaries produced over this range of sulfur additions show a tendency to become larger as the sulfur addition is increased.
  • the quantity of sulfur made available to the ingot iron or low carbon steel may exceed the solubility of sulfur in the area of the grain boundaries. Some sulfur will be lost during the drying of a slurry coating and the handling of the dried coating. Therefore it is necessary to add sufficient excess to make up for this loss, and values disclosed refer in all cases to the amount of sulfur or sulfide present during the heat treatment.
  • hydrogen sulfide or other sulfurbearing gas may be added to the annealing atmosphere in lieu of including sulfur in the annealing separator. Where this is done, and assuming that the atmosphere has access to all surfaces of the ingot iron or low carbon steel, at least 750 p.p.m. of hydrogen sulfide or its equivalent should be present in the atmosphere. It is possible, however, to add larger quantities of sulfur-bearing gases, even to the extent of forming an iron sulfide film or surface layer as taught in the copending application of the same inventor, Ser. No. 378,823, filed .Tune 29, 1964, now Patent No. 3,333,992.
  • the sulfide film is formed ahead of the final anneal and the sulfides will diffuse into the primary grain boundaries during the final anneal.
  • the total sulfur content of the ingot iron or low carbon steel is not necessarily controlling.
  • the presence of finely dispersed sulfides at the grain boundaries during the final anneal is of primary importance. It follows that a low carbon steel or ingot iron having sufficient sulfides at the grain boundaries may be suitable for primary and secondary grain growth even though its total sulfur content may be relatively low, whereas a treatment which tended to remove sulfides at the grain boundaries might impair the ability of the material to acquire a high degree of preferred orientation even though it did not appreciably lower the total sulfur content of the material.
  • the practice of this invention involves the addition of some sulfur or sulfide to the ingot iron or low carbon steel after it has been rolled to final gauge, substantially irrespective of its total sulfur content, especially since the sulfur or sulfide added by the procedures herein taught occurs primarily at the grain boundaries.
  • the properties of the iron or ⁇ steel can be damaged by too much sulfur. While limited quantities can be removed at annealing temperatures below 1650 F., normally the sulfur is not substantially lowered.
  • the layer of iron sulde should be about .02 mil to about .10 mil thick.
  • vacuum annealing is not precluded in the practice of this invention.
  • nitrogen or other inert gases ⁇ may be used with or without hydrogen or in a partial vacuum.
  • Sulfur is apparently capable of direct diffusion into the metal from the annealing separator.
  • the effective sulfur content in the environment of the steel should be maintained during the primary grain growth period until the temperature of the steel reaches about 1500 to 1600 F. When this is done grain growth will be satisfactorily inhibited and the grains having the 1800 F. and pickled.
  • the material After cold rolling various amounts in a single stage as shown in Table III below, the material was decarburized at 1500 F., -coated with mag- 50 nesia containing 4% elemental sulfur, and box annealed for 24 hours at 1600 F.
  • the permeability at all gauges was excellent, indicating that the product had a high degree of cube-on-edge orientation.
  • the managanese content should preferably be less than about .2%.
  • FIG. 6 is a pole figure illustrating the orientation of the material of Example VII. It will be seen that the pattern indicates unmistakably a high degree of 110) [001] orientation.
  • FIG. 7 is a pole figure illustrating the orientation of the material of Example VI and it will lbe seen that the pattern shows a high degree of (112) [110] orientation.
  • the grain size of the materials of this invention in final form are relatively large. While the A.S.T. ⁇ M. standard chart of grain sizes contemplates a magnification of 100x, the grain sizes of the materials of this invention can be compared at unit magnification with the S.D.T.M. chart, and as so compared generally respond to No. 8 to No. and even larger. Moreover, the grains have generally a length at least about ten times the thickness of the sheet stock.
  • a method of producing ingot iron and low carbon steel sheet stock characterized by a preponderant orientation chosen from a class consisting of (110) [001] and (112) [110], fwhich comprises hot rolling a ferrous material containing up to 0.10% carbon, 0.01% to 0.40% manganese, up to 0.05% sulfur, the balance being iron except for incidental impurities, to produce an intermediate gauge hot rolled band, cold rolling the said hot rolled band to produce a cold rolled stock at final gauge, subjecting said cold rolled stock to a nal anneal during which primary grain growth occurs in the presence of .a material chosen from the class consisting of elemental sulfur, selenium, and decomposable compounds thereof, and thereafter subjecting said stock to a secondary recrystallization treatment under box annealing conditions at a higher temperature of 1500 to 1650 F.
  • Ingot iron and low carbon steel sheet stock characterized by a preponderant orientation chosen from a class consisting of (110) [001] and (112) [110] and wherein the grains have a length of at least about ten times the thickness of said sheet stock.

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US467228A 1965-06-28 1965-06-28 Grain-oriented iron and steel and method of making same Expired - Lifetime US3392063A (en)

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Application Number Priority Date Filing Date Title
US467228A US3392063A (en) 1965-06-28 1965-06-28 Grain-oriented iron and steel and method of making same
FR83398A FR1525917A (fr) 1965-06-28 1966-11-10 Procédé de fabrication d'alliages orientés à base de fer et produits ainsi obtenus
BE689584D BE689584A (enrdf_load_stackoverflow) 1965-06-28 1966-11-10
GB50579/66A GB1142552A (en) 1965-06-28 1966-11-11 Grain-oriented iron and steel and method of making same
DE19661508366 DE1508366A1 (de) 1965-06-28 1966-11-12 Verfahren zur Herstellung von Gusseisen und kohlenstoffarmem Stahl mit bevorzugten kristallographischen Orientierungen

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GB (1) GB1142552A (enrdf_load_stackoverflow)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3540948A (en) * 1967-12-18 1970-11-17 United States Steel Corp Method of producing cube-on-corner oriented electrical steel sheet
US3615278A (en) * 1963-12-14 1971-10-26 Nippon Steel Corp Enameling grade steel and method of producing the same
US4251294A (en) * 1978-08-22 1981-02-17 National Steel Corporation Method for producing fully-processed low-carbon electrical steel
US4975127A (en) * 1987-05-11 1990-12-04 Kawasaki Steel Corp. Method of producing grain oriented silicon steel sheets having magnetic properties

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2287466A (en) * 1939-12-05 1942-06-23 American Rolling Mill Co Process of producing high permeability silicon steel

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2287466A (en) * 1939-12-05 1942-06-23 American Rolling Mill Co Process of producing high permeability silicon steel

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3615278A (en) * 1963-12-14 1971-10-26 Nippon Steel Corp Enameling grade steel and method of producing the same
US3540948A (en) * 1967-12-18 1970-11-17 United States Steel Corp Method of producing cube-on-corner oriented electrical steel sheet
US4251294A (en) * 1978-08-22 1981-02-17 National Steel Corporation Method for producing fully-processed low-carbon electrical steel
US4975127A (en) * 1987-05-11 1990-12-04 Kawasaki Steel Corp. Method of producing grain oriented silicon steel sheets having magnetic properties

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GB1142552A (en) 1969-02-12
DE1508366A1 (de) 1969-10-23

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