US3130094A - Manufacture of silicon-iron having cubic texture - Google Patents
Manufacture of silicon-iron having cubic texture Download PDFInfo
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- US3130094A US3130094A US145540A US14554061A US3130094A US 3130094 A US3130094 A US 3130094A US 145540 A US145540 A US 145540A US 14554061 A US14554061 A US 14554061A US 3130094 A US3130094 A US 3130094A
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- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 title claims description 37
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 238000001953 recrystallisation Methods 0.000 claims description 58
- 238000000034 method Methods 0.000 claims description 36
- 230000009467 reduction Effects 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical class [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 11
- 239000011593 sulfur Substances 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 description 51
- 238000005097 cold rolling Methods 0.000 description 45
- 238000011282 treatment Methods 0.000 description 24
- 238000005096 rolling process Methods 0.000 description 15
- 230000035699 permeability Effects 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 239000007858 starting material Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
- 230000001590 oxidative effect Effects 0.000 description 6
- 238000005098 hot rolling Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 241000276498 Pollachius virens Species 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 241000837181 Andina Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 235000010269 sulphur dioxide Nutrition 0.000 description 1
- 239000004291 sulphur dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—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
- B21B3/02—Rolling special iron alloys, e.g. stainless steel
-
- 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
- C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
- C21D8/1233—Cold rolling
-
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/76—Adjusting the composition of the atmosphere
-
- 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
- C21D8/1261—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 following hot rolling
-
- 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
- C21D8/1266—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 between cold rolling steps
-
- 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
- a silicon-iron sheet stock in which the grains have preponderantly an orientation which can be described as a (100) [001] orientation by Millers indices has a number of useful advantages in the electrical arts.
- such a sheet stock may have an unusually high permeability in the straight grain or rolling direction coupled with a high permeability in the cross grain direction, so that its utility is not confined to the manufacture of magnetic core structures in which the primary direction of the magnetic flux must always be parallel to the rolling direction.
- the material is carried through a series of relatively well-defined derivative orientations to produce a material which, after a primary recrystallization, will be in a condition to pro prise a cubic texture material in a secondary recrystallization treatment.
- the procedure of the said application has the advantage of producing a very large number of grains which can grow in the desired cubic texture upon secondary recrystallization, so that an end product may be produced in which the grains are relatively small. But the procedure also has certain disadvantages.
- the starting material is the equivalent of commercial oriented silicon-iron having the cube-on edge texture. This means it will already have been subjected to a series of expensive treatments involving cold rollings and intermediate and final anneals. The cost of the steps outlined in the said copending application thus becomes additive to the cost of preparing the starting material.
- FIG. 1 is an X-ray pole stereogram of the [200] poles of a silicon-iron stock which has been cold rolled from a thickness of about .150 inch to about .050 inch.
- FIG. 2 is an optical pole figure of the orientation produced by annealing the material of FIG. 1 for 100 hours at 2200 F.
- FIG. 3 is a chart in which the permeability of material having the general orientation shown in FIG. 2 is plotted against the degree of cold reduction.
- the data in FIG. 3 were taken from two heats as indicated by the solid circles and the open circles.
- the reduction scale shows thickness in mils for the material of FIG. 2, there being another horizontal scale marked in percentages of reduction, applying as well to other thicknesses.
- FIG. 4 is an X-ray stereogram of the [200] poles of the material of FIG. 2 after it has been cold rolled in a second operation from a thickness of .050 inch to a thickness of .012 inch.
- FIG. 5 is an X-ray stereogram of the [200] poles of the material of FIG. 4 after it has been subjected to a primary recrystallization by being box annealed at a temperature of about 1400 F. for about one hour.
- FIG. 6 is an optical pole figure of a final orientation produced by subjecting the material of FIG. 5 to secondary recrystallization as hereinafter taught.
- FIG. 7 is a flow sheet diagram of the steps of a typical process embodiment of the invention as applied to siliconiron containing substantially 2.5% to 4% silicon and not more than 0.040% total oxides.
- the material which is to be subjected to the secondary recrystallization should have certain characteristics both as to orientation and as to chemistry, which will hereinafter be outlined.
- the product contain a substantial number of well dispersed crystal nuclei having a cube face less than 5 and preferably less than 2 of angularity to the surface of the sheet stock and that as to these grains, the orientation of the cube edgesshould be such that most of the edges are parallel to the rolling direction. It is preferred that at least 75% of the cube edges lie within 20 of the rolling direction.
- a product containing a reasonable number of properly. oriented'nuclei can be produced from a material having cube-on-edge orientation by a procedure involving tilting the cube faces to varying angles transversely of the direction of rolling to such an extent that there will be a number of the grains having their cube faces tilted into parallelism with the surface planes of the sheet or lying within 5 of that position.
- the orientation obtained after the first stage and intermediate anneal is not a true cube-on-edge orientation although a large number of the grains will be in that position. It may be characterized as an imperfect cubeon-edge orientation; and the less perfect it is, so long as there is a high degree of azimuthal orientation, the greater will be the number of grains having the cubic texture in the material at the start of the secondary recrystallization.
- the effect of the second cold rolling treatment and the resulting primary recrystallization will be to produce a substantial number of grains in which the cube faces are either parallel to the sheet surfaces or lie within 5 of such parallelism, and in which the cube edges are substantially aligned in the rolling direction. It will be understood that some deviation or scatter in azimuthal orientation is tolerable, and in one phase of the invention, as hereinafter set forth, some scatter in azimuthal orientation is deliberately permitted.
- the silicon-iron to be treated is preferably melted and refined in the open hearth furnace or equivalent treatment apparatus, and it is a commercial advantage of the process that it may be so melted and refined.
- a vacuum melting technique may, however, be employed if desired.
- composition of silicon-iron should be substantially as follows:
- the balance will be iron with such impurities as are normal in the manufacture of high grade silicon-iron.
- the product if it contains any aluminum, should not contain aluminum in excess of about 004%.
- the material should be as clean as possible. A total oxides content over about 040% is undesirable. Materials which form oxides that are not reducible in hydrogen having a -50 dew point at 2200 F. should be at a minimum and preferably below .004%.
- the analysis given - is that for the hot rolled material as distinguished from a ladle analysis.
- the manganese and sulfur contents are important and care should be taken to maintain them within the ranges set forth whether the material be vacuum melted or air melted.
- the silicon-iron material is preferably hot rolled from a high slab or ingot temperature because this improves the quality of the orientation.
- the precise gauge to which the material is hot rolled may be varied depending on the desired final thickness. As an example, for the production of a final product of 12 to :14 mils in thickness, the silicon-iron may be hot rolled to a thickness of about .150 inch.
- the hot rolled gauge of the material can be varied in view of the desired final gauge, and the desired percentages of reduction in the two cold rolling stages, as will hereinafter be explained.
- the hot rolled material is then given an initial anneal which may be a box anneal at about 1400 F. in air for a total time of 24 hours.
- An open anneal in air may be substituted for the box anneal; but if this is done a higher temperature should be used, namely a temperature of about 1800 F. with a soaking period of several minutes.
- a box anneal, if employed, may be carried on with the hot mill scale still on the surfaces of the stock, and it may be followed by a brief open anneal in air to facilitate picklin
- the hot rolled material will in any event be pickled to provide a clean surface.
- the stock is cold rolled in a first stage with a reduction of about 55% to 80%, an optimum reduction being about 67%.
- the hot rolled stock having the aforesaid thickness of about .150 inch may be cold rolled to a thickness of about .050 inch, but these values are not limiting.
- hot rolled material having a thickness of about .110 inch may be cold rolled in this first stage to about .033 inch, which is a reduction of about 70%.
- high temperature is meant a temperature substantially within the range of 2200 F. to 2350" F.
- the annealing is practiced for a considerable length of time, i.e., about 30 to about 90 hours at the high temperature. A number of actions occur during this anneal.
- the carbon unless previously reduced to a minimal value, will be reduced to 0.010% or less.
- Oxide inclusions in the metal will also be reduced; and after this heat treatment, the total quantity of such oxides should preferably be less than about 005%.
- the oxides in the starting material are substantially lower than about 0.04%, a somewhat lower temperature may be employed for this intermediate anneal, i.e., a temperature down to about 2000 F.
- the total quantity of oxides in the starting material will be lower if the material has been manufactured by the vacuum melting technique, and products so produced may be used in the process of this invention.
- an advantage of the invention is that it may be applied With entire success to air melted siliconiron as produced, for example, in the open hearth furnace.
- the intermediate anneal also has a function in lowering the sulfur content of the silicon-iron. At the end of the intermediate anneal the sulfur content will preferably have been lowered to .005 or less, thereby diminishing the time necessary for accomplishing secondary recrystallization in the final anneal.
- the temperature of the intermediate anneal and the time at temperature may be varied depending upon the amount of impurities in the stock. If the material is initially low in impurities as the result of melting and refining processes practiced upon it, a box anneal at a temperature of about 2000 F. for a few hours may be suificient. Normally, however, open hearth stock is relatively high in oxides, and such stock may require a temperature of about 2200" F. or higher for times up to 90 hours to reduce the impurities to the desired level.
- the orientation and texture of the metal following the recrystallization may be regarded as an imperfect form of cube-on-edge texture, in which the cube edges are reasonably aligned in the rolling direction, and in which a considerable number of the grains have their cube faces lying at an angle of 45 to the plane of the surface of the shee But it will be seen that there is a very substantial spread in the lateral tilt of the grains and in particular that an appreciable number of the grains have cube faces lying at an angle of less than about 32 to the planes of the surfaces of the sheet.
- the optical pole figure, forming FIG. 2 of the drawings hereof shows that some of the grains have even attained a condition of cubic orientation. In this figure certain semi-circular lines, so marked, have been used to indicate positions of tilt of 45, 30 and 15.
- FIG. 3 shows diagrammatically the result of a first cold rolling stage at different percentages of reduction on the permeability of the product after the intermediate anneal.
- the permeability is important beoause it indicates among other things the degree of perfection of the azimuthal orientation. While the precise shape of the curve may vary with different formulae and difierent starting thicknesses, it Will be seen that the highest permeabilities in the first stage of cold rolling are attained with cold rolling reductions of about 55-80%. The skilled worker will also recognize that the permeabilities are not as high as those obtainable in finished commercial grade silicon-iron stocks having the most perfect cube-on-edge orientation. Nevertheless, a relatively high degree of straight grained permeabilities is attained at the first stage cold rolling reductions hereinabove taught, and is indicative of a relatively high degree of azimuthal orientation.
- a more usual operation will be to carry on the primary and secondary recrystallization as a part of the same heat treatment.
- the skilled worker in the art will understand that primary recrystallization occurs quite rapidly at a relatively low temperature, say 1300 F. to 1700 F.
- the secondary recrystallization takes time and occurs at temperatures roughly within 1900 F. to 2300 F. Consequently the primary recrystallization can be considered to occur and will normally be considered to occur while the material is being heated up to the tem perature for secondary recrystallization.
- a box annealing of the material in dry hydrogen i.e., hydrogen having a 50 dew point at about 2200 F.
- the silicon-iron stock usually but not necessarily in the form of stacked sheets spaced by a suitable annealing separator.
- the final heat treatment is preferably carried on in accordance with the teachings of the copending application of one of the inventors herein, Dale M. Kohler, and John M. Jackson entitled The Production of Oriented SiliconJron Sheets by Secondary Recrystallization, Serial No. 813,289, filed May 14, 1959.
- the last mentioned application teaches in essence the use of an atmosphere, in the final heat treatment, of hydrogen or a non-reactive gassuch as argon or helium, which atmosphere contains a very small amount (e.g., about 20 to 250 parts per million of hydrogen sulfide), of a highly polar compound such as hydrogen sulfide, sulphur dioxide, an exide of carbon, or a mixture of these.
- the highly polar compound is believed to be absorbed or adsorbed on the crystal planes atthe surfaces of the sheet stock so as to satisfy the positive unsatisfied charges there, the result being a shifting of the energies of crystals of differing orientations in such a way that the (100) [001] orientation becomes the lowest energy orientation by a substantial amount, making for a more positive and complete cubic texture orientation in the stock.
- the tendency toward secondary recrystallization in the cubic texture when the anneal is carried on as just described is so strong that in many instances an open, strand or. continuous anneal may be used.
- the usual practice, however, will be a box anneal with a soaking time of at least several hours at the highest temperature, a temperature of 2000 F. to 2300 F. being preferred. Excellent results are attained at a temperature of about 2200 F.
- Example A silicon-iron material containing 3.21% silicon was hot rolled to a thickness of .150 inch and box annealed at 1400 F. in air for a total time of 24 hours. It was then cold reduced to .050 inch and given an intermediate box anneal in hydrogen at a temperature of about 2200 F. for a time of about 80 hours in an atmosphere of dry hydrogen. Thereafter it was cold reduced to a thickness of about .010 inch and then subjected to a box anneal in dry hydrogen (50 dew point at 2200 F.). An annealing separator was used consisting essentially of magnesia in a thoroughly dehydrated state and containing a minute trace of sulphur. The anneal was at a temperature of about 2200 F. with a soaking period of 24 hours.
- the intermediate anneal will be the same as those set forth above. Since the percentage of reduction in the second cold rolling stage will be somewhat less, it becomes possible to start with a lighter hot rolled gauge and arrive at the same final gauge or gauges.
- the silicon-iron is hot rolled to about inch, and then is given a 70% reduction in the first cold rolling stage and iscarried down to about .033 inch, a second cold rolling with a 73% reduction will carry the material down to .009 inch. If the final gauge is to be .014 inch, only a 58% reduction would be required.
- the modified procedure now being described is not limited to the use of a hot rolled material of any particular thickness; but it will comprise a first cold rolling treatment with a reduction of at least about 55%, and a second cold rolling reduction of at least about 55%.
- the modified procedure can be depended upon to give permeabilities at least as high as about 1700 in the straight grain and cross grain directions. This permeability makes the stock less desirable for punched laminations in transformer cores; but the stock is less perfectly directional in the plane of the sheet, and therefore has a certain advantage in rotating electrical equipment. This is not to say tha the stock is non-directional. On the contrary, it approximates the character of a true cubic stock, but is characterized by a greater spread in the azimuthal orientation.
- a second cold rolling treatment at a somewhat lower reduction causes the tilting of the grains or crystals so that their faces come more nearly into parallelism with the surfaces of the sheet stock, but at the same time is less effective in preserving the azimuthal orientation.
- the secondary recrystallization is a surface energy recrystallization. It is believed that under this condition, the grains having their cube faces oriented to parallelism with the stock surfaces (or to within less than 5 of such parallelism) tend to grow in the secondary recrystallization at the expense of grains not so oriented. Thus, the result is a product having a high degree of face-orientation but a somewhat greater spread of azimuthal orientation.
- a process for the manufacture of silicon-iron sheet stock having cubic texture which comprises hot rolling silicon-iron containing substantially 2.5% to 4% silicon and a total oxide content of not more than 0.040% to an intermediate gauge, heat treating the hot rolled stock at a temperature of at least about 1400 F. but not substantially exceeding -l"800 F., cold rolling said stock with a reduction of at least about 55%, annealing the said stock at a temperature of about 2200 to 2350 F. in an atmosphere of hydrogen and for a sufficient length of time to recrystallize a substantial number of the grains of said.
- the stock after the said anneal having oxide inclusions less than about 0.005%, a carbon content not substantially greater than 0.010%, and a sulfur content not substantially greater than 0.005 again cold rolling said stock with a reduction of at least about 75 to reduce said stock to final gauge and further to orient the grains therein, and subjecting the cold rolled sheet stock first to a primary recrystallization anneal at a temperature of about l300 to about 1700 F.
- nuclei in a non-oxidizing atmosphere to produce cubic nuclei having their cube faces tilted at less than to the surface of the sheet stock, said nuclei having also at least about 75 of their cube edges aligned within 20 of the rolling direction, and second to an an neal at a temperature of about 2000" to about 2300 F. in a non-oxidizing atmosphere under conditions to produce secondary recrystallization by surface energy Whereby to cause said nuclei to grow by said secondary recrystallization at the expense of grains having substantially different orientations in said sheet stock.
- a process for the manufacture of silicon-iron sheet stock characterized by cubic texture which process comprises hot rolling a silicon-iron containing substantially 2.5% to 4% silicon, .03% to .15% manganese, .015% to .030% sulfur and .015% to .030% carbon, and containing no more than about 0.040% total oxide, the balance being iron with such impurities as are normal in the manufacture of high grade silicon-iron, heat treating the hot rolled silicon-iron at a temperature of substantially 1400 to 1800 F. and pickling it, cold rolling the siliconiron with a reduction of substantially 55% to 80%, heat treating the silicon-iron at a temperature of substantially 2200 to 2350 F. in hydrogen having a dew point of around -50 F.
- a process for the manufacture of silicon-iron sheet stock having cube-on-face texture which comprises hot rolling silicon-iron containing substantially 2.5% to 4% silicon and containing no more than about 0.040% total oxide to an intermediate gauge, subjecting the hot rolled stock to a recrystallization temperature and thereafter to a cleaning, cold rolling said stock with a reduction of at least about 55%, annealing the said stock at a temperature of about 2000 to 2350 F.
- nuclei in a non-oxidizing atmosphere to produce cubic nuclei having their cube faces tilted at less than 5 to the surface of the sheet stock, said nuclei having also about 75 of their cube edges aligned within 20 of the rolling direction, and second to an anneal at a temperature of about 2000 to about 2300 F. in a nonoxidizing atmosphere under conditions to cause said nuclei to grow by surface energy secondary recrystallization at the expense of grains having substantially different orientations in said sheet stock.
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- Mechanical Engineering (AREA)
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- Manufacturing & Machinery (AREA)
- Electromagnetism (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Metal Rolling (AREA)
- Heat Treatment Of Sheet Steel (AREA)
- Soft Magnetic Materials (AREA)
- Developing Agents For Electrophotography (AREA)
Priority Applications (10)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BE622386D BE622386A (en)) | 1959-06-11 | ||
GB18345/60A GB950082A (en) | 1959-06-11 | 1960-05-24 | The manufacture of silicon-iron having cubic texture |
FR828311A FR1272943A (fr) | 1959-06-11 | 1960-05-25 | Tôle de fonte au silicium et son procédé de fabrication |
DEA34859A DE1277287B (de) | 1959-06-11 | 1960-06-10 | Verfahren zur Herstellung von Eisen-Silicium-Blech mit Wuerfeltextur |
CH667660A CH432566A (de) | 1959-06-11 | 1960-06-11 | Verfahren zur Herstellung von Silicium-Eisen-Blech mit Würfeltextur |
US145540A US3130094A (en) | 1959-06-11 | 1961-10-13 | Manufacture of silicon-iron having cubic texture |
GB35311/62A GB974686A (en) | 1959-06-11 | 1962-09-17 | The manufacture of silicon-iron having cube-on-face texture |
FR910314A FR82812E (fr) | 1959-06-11 | 1962-09-24 | Tôle de fonte au silicium et son procédé de fabrication |
CH1179262A CH485857A (de) | 1959-06-11 | 1962-10-08 | Verfahren zur Herstellung von Silicium-Eisen-Blech mit Würfeltextur |
DEA41362A DE1293180B (de) | 1959-06-11 | 1962-10-11 | Verfahren zur Herstellung von Eisen-Silicium-Blech mit (100)[hkl]-Textur |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US81958959A | 1959-06-11 | 1959-06-11 | |
US145540A US3130094A (en) | 1959-06-11 | 1961-10-13 | Manufacture of silicon-iron having cubic texture |
Publications (1)
Publication Number | Publication Date |
---|---|
US3130094A true US3130094A (en) | 1964-04-21 |
Family
ID=26843076
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US145540A Expired - Lifetime US3130094A (en) | 1959-06-11 | 1961-10-13 | Manufacture of silicon-iron having cubic texture |
Country Status (6)
Country | Link |
---|---|
US (1) | US3130094A (en)) |
BE (1) | BE622386A (en)) |
CH (2) | CH432566A (en)) |
DE (2) | DE1277287B (en)) |
FR (1) | FR1272943A (en)) |
GB (2) | GB950082A (en)) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3333992A (en) * | 1964-06-29 | 1967-08-01 | Armco Steel Corp | Production of oriented silicon-iron using grain growth inhibitor during primary recrystallization heat treatment |
US3333993A (en) * | 1965-04-02 | 1967-08-01 | Armco Steel Corp | Production of thin, oriented siliconiron wherein grain growth inhibitor is added to primary recrystallization heat treatment atmosphere as function of mn content and final thickness |
US3640780A (en) * | 1970-06-25 | 1972-02-08 | United States Steel Corp | Method of producing electrical sheet steel with cube texture |
US3789647A (en) * | 1972-10-20 | 1974-02-05 | United States Steel Corp | Method of surface-conditioning heat-treating-furnace hearth rolls having sleeves of rebonded fused silica thereon by processing silicon steel strip |
US3849212A (en) * | 1972-02-22 | 1974-11-19 | Westinghouse Electric Corp | Primary recrystallized textured iron alloy member having an open gamma loop |
US3892605A (en) * | 1972-02-22 | 1975-07-01 | Westinghouse Electric Corp | Method of producing primary recrystallized textured iron alloy member having an open gamma loop |
EP0099617A3 (en) * | 1982-07-19 | 1984-06-06 | Allegheny Ludlum Steel Corporation | Method for producing cube-on-edge oriented silicon steel |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3632456A (en) * | 1968-04-27 | 1972-01-04 | Nippon Steel Corp | Method for producing an electromagnetic steel sheet of a thin sheet thickness having a high-magnetic induction |
JPS51151215A (en) * | 1975-06-21 | 1976-12-25 | Kawasaki Steel Corp | Process for manufacturing non-oriented silicon steel plate with low co re loss and high magnetic flux density |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2303343A (en) * | 1941-01-14 | 1942-12-01 | Carnegie Illinois Steel Corp | Silicon steel electrical strip |
US2307391A (en) * | 1938-10-14 | 1943-01-05 | American Rolling Mill Co | Art of producing magnetic material |
DE1009214B (de) * | 1954-03-27 | 1957-05-29 | Ver Deutsche Metallwerke Ag | Verfahren zur Erzeugung ausgepraegter Wuerfeltextur in magnetisierbaren Baendern undBlechen aus silizium- und/oder aluminiumhaltigen Eisenlegierungen |
US2992952A (en) * | 1955-12-01 | 1961-07-18 | Vacuumschmelze Ag | Method of manufacturing magnetic sheets |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2473156A (en) * | 1944-11-16 | 1949-06-14 | Armco Steel Corp | Process for developing high magnetic permeability and low core loss in very thin silicon steel |
US2599340A (en) * | 1948-10-21 | 1952-06-03 | Armco Steel Corp | Process of increasing the permeability of oriented silicon steels |
-
0
- BE BE622386D patent/BE622386A/xx unknown
-
1960
- 1960-05-24 GB GB18345/60A patent/GB950082A/en not_active Expired
- 1960-05-25 FR FR828311A patent/FR1272943A/fr not_active Expired
- 1960-06-10 DE DEA34859A patent/DE1277287B/de active Pending
- 1960-06-11 CH CH667660A patent/CH432566A/de unknown
-
1961
- 1961-10-13 US US145540A patent/US3130094A/en not_active Expired - Lifetime
-
1962
- 1962-09-17 GB GB35311/62A patent/GB974686A/en not_active Expired
- 1962-10-08 CH CH1179262A patent/CH485857A/de unknown
- 1962-10-11 DE DEA41362A patent/DE1293180B/de active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2307391A (en) * | 1938-10-14 | 1943-01-05 | American Rolling Mill Co | Art of producing magnetic material |
US2303343A (en) * | 1941-01-14 | 1942-12-01 | Carnegie Illinois Steel Corp | Silicon steel electrical strip |
DE1009214B (de) * | 1954-03-27 | 1957-05-29 | Ver Deutsche Metallwerke Ag | Verfahren zur Erzeugung ausgepraegter Wuerfeltextur in magnetisierbaren Baendern undBlechen aus silizium- und/oder aluminiumhaltigen Eisenlegierungen |
US2992952A (en) * | 1955-12-01 | 1961-07-18 | Vacuumschmelze Ag | Method of manufacturing magnetic sheets |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3333992A (en) * | 1964-06-29 | 1967-08-01 | Armco Steel Corp | Production of oriented silicon-iron using grain growth inhibitor during primary recrystallization heat treatment |
US3333993A (en) * | 1965-04-02 | 1967-08-01 | Armco Steel Corp | Production of thin, oriented siliconiron wherein grain growth inhibitor is added to primary recrystallization heat treatment atmosphere as function of mn content and final thickness |
US3640780A (en) * | 1970-06-25 | 1972-02-08 | United States Steel Corp | Method of producing electrical sheet steel with cube texture |
US3849212A (en) * | 1972-02-22 | 1974-11-19 | Westinghouse Electric Corp | Primary recrystallized textured iron alloy member having an open gamma loop |
US3892605A (en) * | 1972-02-22 | 1975-07-01 | Westinghouse Electric Corp | Method of producing primary recrystallized textured iron alloy member having an open gamma loop |
US3789647A (en) * | 1972-10-20 | 1974-02-05 | United States Steel Corp | Method of surface-conditioning heat-treating-furnace hearth rolls having sleeves of rebonded fused silica thereon by processing silicon steel strip |
EP0099617A3 (en) * | 1982-07-19 | 1984-06-06 | Allegheny Ludlum Steel Corporation | Method for producing cube-on-edge oriented silicon steel |
Also Published As
Publication number | Publication date |
---|---|
FR1272943A (fr) | 1961-10-06 |
GB950082A (en) | 1964-02-19 |
CH485857A (de) | 1970-02-15 |
GB974686A (en) | 1964-11-11 |
DE1293180B (de) | 1969-04-24 |
CH432566A (de) | 1967-03-31 |
DE1277287B (de) | 1968-09-12 |
BE622386A (en)) |
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