Abstract:
A process for producing silicon steel strip of less than 0.30 mm thickness having cube-on-edge orientation, which comprises heating a silicon steel slab to 1300°-1400° C., hot rolling to hot band thickness, removing hot mill scale, cold rolling to intermediate thickness without annealing the hot rolled band, subjecting the intermediate thickness cold rolled material to an intermediate anneal at a temperature of 1010° to about 1100° C. with a total time of heating and soaking of less than about 180 seconds, cold rolling to a final thickness of less than 0.30 mm, decarburizing, applying an annealing separator, and finally annealing in conventional manner.

Description:
BACKGROUND OF THE INVENTION 
     This invention relates to the production of regular grade cube-on-edge oriented silicon steel strip and sheet of less than 0.30 mm thickness by a simplified process. More particularly, the process of the invention omits an anneal of the hot rolled material with consequent saving in energy costs and processing time, without sacrificing the magnetic properties. This is made possible by conducting an anneal of the cold rolled strip at intermediate thickness at a higher temperature than that of a conventional intermediate anneal. 
     The so-called &#34;regular grade&#34; silicon steel having the cube-on-edge orientation utilizes manganese and sulfur (and/or selenium) as a grain growth inhibitor. In contrast to this, &#34;high permeability&#34; silicon steel relies upon aluminum nitrides in addition to or in place of manganese sulfides and/or selenides as a grain growth inhibitor. 
     The process of the present invention is applicable only to regular grade grain oriented silicon steel, and hence purposeful aluminum and nitrogen additions are not utilized. 
     The conventional processing of regular grade grain oriented silicon steel strip and sheet comprises the steps of preparing a melt of silicon steel in conventional facilities, refining and casting in the form of ingots or strand cast slabs. The cast steel preferably contains, in weight percent, from about 0.02% to 0.045% carbon, about 0.04% to 0.08% manganese, about 0.015% to 0.025% sulfur and/or selenium, about 3% to 3.5% silicon, not more than about 50 ppm nitrogen, not more than about 30 ppm total aluminum, and balance essentially iron. 
     If cast into ingots, the steel is conventionally hot rolled into slabs. The slabs (whether obtained from ingots or continuously cast) are heated (or reheated) to a temperature of about 1300° to 1400° C. in order to dissolve the grain growth inhibitor prior to hot rolling, as disclosed in United States Pat. No. 2,599,340. The slabs are then hot rolled, annealed, cold rolled in two stages with an intermediate anneal, decarburized, coated with an annealing separator and subjected to a final anneal in order to effect secondary recrystallization. 
     Representative processes for producing regular grade cube-on-edge oriented silicon steel strip and sheet are disclosed in United States Pat. Nos. 4,202,711; 3,764,406; and 3,843,422. 
     The process of U.S. Pat. No. 4,202,711 includes hot rolling of a strand cast slab with a finish temperature greater than 900° C., an anneal of the hot band at 925° to 1050° C., pickling, cold rolling in two stages with an intermediate anneal within the temperature range of 850° to 950° C. and preferably at about 925° C. with a soak time of about 30 to 60 seconds. The material is then cold rolled to final thickness, decarburized, coated with an annealing separator and finally annealed in a hydrogen-containing atmosphere. 
     United States Pat. No. 2,867,558 discloses a process for producing cube-on-edge oriented silicon-iron wherein a hot reduced silicon-iron band containing more than 0.012% sulfur is cold reduced at least 40%, subjected to an intermediate anneal between 700° and 1000° C. to control the average grain size between about 0.010 and about 0.030 mm, further cold reduced at least 40% to final thickness, and finally annealed at a temperature of at least 900° C. It was alleged that excessive grain growth occurred at intermediate annealing temperatures above 945° C. unless relatively large amounts of sulfur and manganese (or titanium) were present in the silicon-iron. Thus, a sulfur content of 0.046% and a manganese content of 0.110% were required in order to avoid a grain size in excess of 0.030 mm when annealing at 975° C. for 15 minutes. 
     United States Pat. No. 2,867,559 discloses the effect of intermediate annealing time and temperature on grain size and percent of cube-on-edge orientation for a single composition selected from U.S. Pat. No. 2,867,558, containing 3.22% silicon, 0.052% manganese, 0.015% sulfur, 0.024% carbon, 0.076% copper, 0.054% nickel, and balance iron and incidental impurities. The intermediate annealing temperature disclosed in this patent ranged from 700° to 1000° C. and the total annealing times of 5 minutes or more. 
     United States Pat. No. 4,212,689 discloses that nitrogen should be decreased to a low level of not more than 0.0045% and preferably not more than 0.0025% in order to achieve a very high degree of grain orientation. The process involves an initial anneal of hot rolled silicon steel at 950° C., cold rolling to intermediate thickness, conducting an intermediate anneal at 900° C. for 10 minutes, and further processing in conventional manner except for an additional final annealing treatment. 
     Other patents of which applicant is aware include U.S. Pat. Nos. 3,872,704; 3,908,737 and 4,006,044. 
     SUMMARY OF THE INVENTION 
     Omission of the initial anneal of hot rolled band has been attempted previously in order to minimize energy costs, and it was found that this anneal could be omitted without sacrifice of magnetic properties when producing grain oriented strip and sheet having a final thickness greater than about 0.30 mm. However, worse magnetic properties were obtained by omission of the initial anneal for grain oriented strip and sheet of less than 0.30 mm thickness when following conventional practice. More particularly, both core loss and permeability were found to be affected adversely. The present invention involves the discovery that excellent magnetic quality can be obtained in strip and sheet material having a final thickness less than 0.30 mm when the initial anneal is omitted, primarily by increasing the temperature of the intermediate anneal after the first stage of cold rolling to a range of 1010° to about 1100° C. 
     According to the invention there is provided a process for producing cold reduced silicon steel strip and sheet of less than 0.30 mm thickness having the cube-on-edge orientation, comprising the steps of providing a slab of silicon steel containing about 3% to about 3.5% silicon, heating the slab to a temperature of about 1300° to 1400° C., hot rolling to hot band thickness with a finish temperature less than 1010° C., removing hot mill scale, cold rolling to an intermediate thickness without annealing the hot band, subjecting the cold rolled intermediate thickness material to an intermediate anneal at a temperature of 1010° to about 1100° C. with a total time of heating and soaking of less than about 180 seconds, cold rolling to a final thickness of less than 0.30 mm, decarburizing, coating the decarburized strip with an annealing separator, and subjecting the coated strip to a final anneal under reducing conditions at a temperature of about 1150° to 1250° C. to effect secondary recrystallization. 
     Preferably the composition of the slab consists essentially of, in weight percent, from about 0.020% to 0.040% carbon, about 0.040% to 0.080% manganese, about 0.015% to 0.025% sulfur and/or selenium, about 3.0% to 3.5% silicon, less than about 30 ppm total aluminum, and balance essentially iron. 
    
    
     DETAILED DESCRIPTION 
     In the present process melting and casting are conventional, and the steel is hot rolled to a preferred thickness of about 2 mm, with a preferred finish temperature of about 950° C. This is followed by removal of the hot mill scale, but the hot band is not annealed prior to the first stage of cold rolling. 
     The intermediate anneal after the first stage of cold rolling is conducted between 1010° and 1100° C. and preferably at about 1050° C. The total time of heating plus soaking is preferably less than 120 seconds. The soak at temperature is preferably less than 60 seconds and more preferably about 20 to 40 seconds. Preferably a non-oxidizing atmosphere, such as nitrogen or a nitrogen-hydrogen mixture, is used. 
     The relatively short duration of less than about 90 seconds soak time and 180 seconds total time for the high temperature intermediate anneal is in sharp contrast to the prior art procedures wherein a minimum of 5 minutes was used with an annealing temperature of 1000° C. (U.S. Pat. No. 2,867,559). 
     The minimum strip temperature of 1010° C. in the present invention contrasts with a maximum temperature of 950° C. used for a soak time of 30 to 60 seconds (U.S. Pat. No. 4,202,711). 
     It has been found that best results are obtained when the intermediate anneal is conducted with a relatively high heating rate, i.e. a heating time of less than 60 seconds to bring the intermediate thickness strip to annealing temperature. 
     Usual thicknesses for strip processed to final thicknesses less than 0.30 mm range from about 0.20 to about 0.28 mm. The intermediate thickness for such strip is about 1.8 to 2.8 times the final thickness and preferably about 2.3 times the final thickness. 
     Preliminary tests indicated that for final thicknesses of greater than 0.30 mm conventional processing, except for omission of the anneal of the hot band, affected magnetic quality only slightly, whereas the same processing applied to strip having a final thickness less than 0.30 mm adversely affected both core loss and permeability. The following data, wherein core loss was measured in watts per pound at 1.7 Tesla and permeability at 800 ampere turns per mm, are representative of these preliminary tests: 
     
         ______________________________________    Initial Anneal                 Without    982° C.                 Initial Anneal    Interm. Anneal                 Interm. Anneal    917° C.                 917° C.Thickness (mm)      P17; 60  Perm      P17; 60                                PermInterm.  Final   w/lb     H = 10  w/lb   H = 10______________________________________0.74   0.345   0.790    1830    0.794  18280.61   0.264   0.675    1834    0.761  1780______________________________________ 
    
     It will be apparent from the above tabulation that only a small change in core loss and permeability resulted from omission of the initial anneal at a final thickness of 0.345 mm, whereas at a final thickness of 0.264 mm, both core loss and permeability were substantially inferior, as compared to the values for that thickness using an initial anneal. 
     Subsequent tests in accordance with the process of the present invention demonstrated that an increase in the intermediate anneal temperature within the range of 1010° to about 1100° C. compensated for omission of an initial anneal of the hot band. 
     Center hot band samples were selected from two heats and tested in order to ascertain the effects of hot finish temperature and intermediate anneal temperature, without an initial anneal of the hot band material. The compositions of the hot band samples are set forth in Table I. Two different finishing temperatures were used for each of the compositions, and these are also set forth in Table I together with serial numbers assigned thereto for identification. Magnetic properties resulting from the variations in hot finishing temperature and intermediate anneal temperature are set forth in Table II. 
     Preliminary preparation of the hot band samples of Table I involved prerolling of strand cast slabs from a thickness of 203 mm to a thickness of 152 mm, reheating to 1400° C., hot rolling to a thickness of 1.93 mm, and scale removal. After cold reduction to the final thicknesses reported in Table II, decarburization was carried out at 830° C. in a mixture of wet H 2  and N 2 . The samples were then coated with magnesium oxide. After a conventional final box anneal at 1200° C. the sheets were sheared into Epstein samples and stress relief annealed prior to magnetic testing. 
     The data in Table II indicate the need for an intermediate anneal of at least 1010° C. when no initial anneal is used. A lower hot finishing temperature also appears beneficial. 
     The data in Table II further show that the thinner gages (0.224 mm) are more difficult to process but produce good results. The higher intermediate anneal is even more important and lower hot finishing temperatures are beneficial. 
     The best intermediate anneal temperature appears to be within the range of 1040° to 1065° C. for both the heats tested. 
     Intermediate anneal thermal cycles of samples reported in Table II were checked with thermocouples attached to strip samples, and soak times ranged from 25 seconds to 37 seconds. The specific relation between thickness, soak temperature and soak time for these samples are set forth in Table III. 
     Table IV shows the influence of extending the time of soak during the intermediate anneal at 955° C. In comparing the results with Table II it will be seen that the magnetic quality is not as good as the higher temperature soak for shorter times. The ability to use total annealing times of less than about 120 seconds increases productivity and hence is economically beneficial and cost effective. 
     Additional tests have been conducted on coils from five different commercial heats, utilizing samples from the front (F) and back (B) ends of the coils (order reversed from hot rolling). These tests compared magnetic properties directly under four different heat treatment conditions at two different final thicknesses and with different intermediate thicknesses. 
     Results of these additional tests are summarized in Table V. 
     Identification of heat treatment conditions reported in Table V is as follows: 
     A = Initial anneal at 1010° C. and intermediate anneal at 950° C. 
     B = Initial anneal at 1010° C. and intermediate anneal at 1060° C. 
     C = No initial anneal and intermediate anneal at 950° C. 
     D = No initial anneal and intermediate anneal at 1060° C. 
     Core loss and permeability values were measured in a manner similar to the tests reported hereinabove, i.e., watts per pound at 1.5 and 1.7 Tesla, and 800 ampere turns per mm. 
     The compositions of the steels utilized in the tests reported in Table V, analyzed at the hot band stage, ranged between 0.026% and 0.028% carbon, 0.058% and 0.064% manganese, 0.016% and 0.023% sulfur, 3.05% and 3.17% silicon, 36 and 49 ppm nitrogen, less than 30 ppm aluminum, less than 30 ppm titanium, and balance essentially iron. Hot roll finish temperatures ranged from about 980° to 990° C., and the processing was the same as that described above for steels of Table I. 
     It will be evident from the data of Table V that the average magnetic properties of those samples which were not subjected to an initial anneal (conditions C and D) were slightly inferior to those of the samples which were subjected to an initial anneal (conditions A and B), at a final thickness of 0.264 mm. However, the average permeability for Condition D samples compared very favorably with Condition A, and several samples exceeded a permeability of 1850. 
     At a final thickness of 0.224 mm the magnetic properties of samples not subjected to an initial anneal were inferior to those which were subjected to an initial anneal, but the marked superiority of condition D samples (in accordance with the invention) over those of condition C demonstrates the criticality of a minimum temperature of 1010° C. for the intermediate annealing step of the invention. 
     It is therefore apparent that the process of the present invention achieves the objective of producing regular grade cube-on-edge oriented silicon steel strip and sheet of less than 0.30 mm thickness without initial anneal of the hot band, while maintaining magnetic properties within acceptable limits. 
     
                       TABLE I______________________________________Compositions                                Hot Roll                                Finish  SerialHeat  % C    % Mn    % S  % Si ppm N Temp. °C.                                        No.______________________________________400826 .029   .064    .018 3.06 36    1000    1277                                 955    1280200693 .027   .057    .019 3.05 54    1004    1247                                 957    1250______________________________________ 
    
     
                       TABLE II______________________________________Magnetic Properties vs. Hot FinishingTemperature &amp; Intermediate Anneal          Final Gage                    Final Gage          0.264 mm  0.224 mm           Hot      Core.       Core  Serial   Finish   Loss        LossHeat No.  No.      Temp.    (P17) Perm  (P17) Perm______________________________________A - 955° C. Intermediate Anneal400826 1277     1000° C.                    .876  1713  1.015 1594200693 1247     1000° C.                    .699  1814  .768  1756           Avg.     .787  1763  .892  1675400826 1280      955° C.                    .689  1814  .876  1680200693 1250      955° C.                    .720  1809  .735  1774           Avg.     .704  1812  .806  1727B - 1010° C. Intermediate Anneal400826 1277     1000° C.                    .669  1840  .726  1776200693 1247     1000° C.                    .672  1846  .665  1817           Avg.     .670  1843  .696  1796400826 1280      955°C.                    .647  1853  .715  1778200693 1250      955° C.                    .622  1848  .604   1820           Avg.     .654  1850  .660  1799C - 1065° C. Intermediate Anneal400826 1277     1000° C.                    .672  1833  .693  1794200693 1247     1000° C.                    .670  1846  .660  1813           Avg.     .671  1840  .676  1804400826 1280      955° C.                    .638  1854  .622  1811200693 1250      955° C.                    .659  1850  .664  1804           Avg.     .648  1852  .663  1810______________________________________ 
    
     
                       TABLE III______________________________________Heating Time IntermediateThickness    Soak Temp.    Total Time                            Soak Timemm       °C.    sec.      sec.______________________________________0.61      955          98        370.48                   84        330.61     1010          98        270.48                   84        250.61     1065          98        290.48                   84        30______________________________________ 
    
     
                       TABLE IV______________________________________Intermediate Anneal Soak (955° C.) vs.Magnetic PropertiesSerialNo.    Core Loss Perm    Soak Time-sec.                              Total Time-sec.______________________________________(Intermediate Gage 0.61 mm- 0.264 mm Final Gage)1277   .876      1713    37        98  .805      1766    87        1471280   .689      1814    37        98  .690      1844    87        1471247   .699      1823    37        98  .683      1832    87        1471250   .720      1809    37        98  .676      1834    87        147(Intermediate Gage 0.48 mm- 0.224 mm Final Gage)1277   1.015     1594    33        84  .974      1624    87        1271280   .876      1680    33        33  .824      1712    84        841247   .768      1756    33        33  .749      1764    84        841250   .735      1774    33        33  .703      1789    84        84______________________________________ 
    
     
                                           TABLE V__________________________________________________________________________Magnetic Properties - Initial Anneal vs. No Initial AnnealA              B         C          DCore           Core      Core       CoreLoss           Loss      Loss       LossCoil No.P15   P17      Perm.          P15             P17                Perm.                    P15                       P17 Perm.                               P15                                  P17                                     Perm.__________________________________________________________________________Final Gage 0.224 mm, Intermed. Gage 0.51 mm 1F  .400   .594      1860          .403             .612                1847                    .633                       .986                           1633                               .419                                  .641                                     1840 1B  .412   .627      1860          .421             .633                1848                    .573                       .919                           1674                               .425                                  .650                                     1835 88F .421   .657      1836          .423             .656                1813                    .572                       .918                           1675                               .486                                  .794                                     1741 88B .399   .604      1846          .397             .593                1857                    .459                       .734                           1770                               .425                                  .646                                     1833103F .399   .595      1836          .403             .617                1839                    .557                       902 1683                               .424                                  .656                                     1831103B .401   .613      1843          .499             .727                1776                    .664                       1.02                           1615                               .471                                  .762                                     1767Avg. .405   .615      1842          .416             .640                1828                    .576                       .913                           1675                               .442                                  .692                                     1808Final Gage 0.264 mm, Intermed. Gage 0.61 mm 1F  .464   .686      1839          .442             .637                1863                    .497                       .773                           1787                               .480                                  .725                                    1818 1B  .456   .665      1851          .452             .647                1861                    .480                       .723                           1806                               .448                                  .657                                    1857 88F .445   .651      1848          .457             .672                1835                    .556                       .882                           1718                               .442                                  .643                                    1858 88B .440   .631      1858          .439             .633                1862                    .508                       .784                           1772                               .467                                  .691                                    1827103F .449   .649      1851          .441             .634                1859                    .453                       .670                           1833                               .441                                  .637                                    1852103B .449   .654      1849          .450             .653                1852                    .521                       .827                           1750                               .455                                  .657                                    1858Avg. .450   .658      1849          .447             .646                1855                    .502                       .785                           1794                               .456                                  .679                                    1845__________________________________________________________________________