US3432368A - Method for manufacturing nitride-containing low-carbon structural steels - Google Patents

Method for manufacturing nitride-containing low-carbon structural steels Download PDF

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US3432368A
US3432368A US529013A US3432368DA US3432368A US 3432368 A US3432368 A US 3432368A US 529013 A US529013 A US 529013A US 3432368D A US3432368D A US 3432368DA US 3432368 A US3432368 A US 3432368A
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steel
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nitride
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Hajime Nakamura
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IHI Corp
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    • 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

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  • FIG. 1 METHOD FOR MANUFACTURING NITRIDE-CONTAINING LOW-CARBON STRUCTURAL STEELS Shee t Filed Feb. 21, 1966 I FIG. 1
  • FIG. 2 8L mmekmwaimh TIME FIG. 2
  • the steel so produced has improved mechanical properties, particularly low temperature toughness.
  • This invention relates to an improved method :for manufacturing nitride-containing low-carbon structural steels.
  • this invention relates to an improved method for manufacturing nitride-containing low-carbon structural steels, the steel containing, by check analysis, carbon up to 0.25%, total nitrogen at least 0.012%, of which at least 0.010% is nitride nitrogen, the nitride being either that of aluminum, or of any one or more of the elements beryllium, columbium, vanadium, titanium or zirconium, the balance or the free uncombined nitrogen being less than 0.003%, the method comprises, (1) heating the steel to at least 1,300, (2) in the course of cooling from said temperature, either passing the temperature range of l,250 to 1,050 in at the most ten minutes or at a mean cooling rate of at least 20/min., (3) in the course of cooling further, either passing the temperature range of 750 to 600 in at least ten minutes or at a mean cooling rate of at the most 15/min., or holding at any temperature within said temperature range for at least ten minutes, (4) reheating the steel without cooling it to room temperatures, and
  • the primary purpose of this invention resides in the improvement of a manufacturing method for high quality structural steels, that is more economical in thermal expenditure than other known methods, and yet is one that can be practised or adapted readily in or to the current steelmakin-g processes as it requires no additional equipment.
  • the second purpose of this invention resides in the provision of inexpensive structural steels of improved mechanical properties, particularly the low temperature toughness,
  • FIG. 1 is a schematic diagram (not to scale) to show the first embodiment of the process of this invention
  • FIG. 2 is a similar diagram for the second embodiment of the process
  • FIG. 3 shows the precipitation behavior of aluminum nitride in isothermal heating treatment (curve A) and isothermal cooling treatment (curve B).
  • curve A isothermal heating treatment
  • curve B isothermal cooling treatment
  • This method of the invention comprises two major embodiments.
  • the first embodiment applies to steels of such nature that the content and kind of the alloying element or elements, other than but with due consideration to the carbon, nitrogen and nitride-former or -formers, make the steel to finish in the ferrite-pearlite double phase structure upon normalization treatment, namely when heated to a temperature above the A transformation point and cooled in air.
  • This kind of steel will be referred to as the first kind steel hereinafter.
  • the second embodiment applies to steels of such nature that the content and kind of the alloying element or elements, other than but with due consideration to the carbon, nitrogen and nitride-former or -formers, make the steel to finish in the martensite or bainite structure upon quenching treatment, namely when heated to a temperature above the A transformation point and quenched.
  • This kind of steel will be referred to as the second kind steel hereinafter.
  • the principal five-step process of the method of this invention lends itself to the first or the second kind of steel as follows.
  • the first kind steel is (1) heated to at least 1,300", (2) in the course of cooling therefrom, either cooled through the temperature range of 1,250'1,050 in at the most ten minutes or at a mean cooling rate of at least 20/min., working the steel if so desired, (3) in the couse of cooling further, either cooled through the temperature range of 750-600 in at least ten minutes or at a mean cooling rate of at the most 15/ min, or held at any temperature within said temperature range for at least ten minutes, (4) reheated to the normalization temperature without cooling to room temperatures, and (5) normalized.
  • This embodiment is schematically illustrated in FIG. 1.
  • the second kind steel is (1) heated to at least 1,300, (2) in the course of cooling therefrom, either cooled through the temperature range of 1,2501,050 in at the most ten minutes or at a mean cooling rate of at least 20/min., working the steel while being cooled, (3) in the course of cooling further, either cooled through the temperature range of 750-600 in at least ten minutes or at a mean cooling rate of at the most l5/min., or held at any temperature within said temperature range for at least ten minutes, (4) reheated to the quenching temperature without cooling to room temperatures, and (5) quenched or quench-and-tempered.
  • This embodiment process is schematically illustrated in FIG. 2.
  • the mechanical properties, particularly the low temperature notch toughness of the steel, can be improved further by repeating the steps (3) to (5) of either embodiment two or more times.
  • step (2) where a hot working is required for the second embodiment, whereas it is not mandatory for the first.
  • Those differences are attributed to the difference in amount and kind of alloying element or elements other than carbon, nitrogen and nitride-forming components, the latter being common to the steels of the first and the second kind.
  • the steel that is semifinished through ordinary procedures including soaking, blooming and slab rolling, is heated to a temperature in the A to 1,l range, rapidly cooled to room temperature therefrom, and tempered at a temperature between 150 and the A transformation point. This will be referred to as the known quench-and-tempering method hereinafter.
  • the steel is solution treated with regard to aluminum nitride, namely, heated to a temperature that is determined by the contents of nitrogen and aluminum so as to completely dissolve the aluminum nitride precipitates, rapidly cooled to l,000 at a rate of at least 90/min., heated to a temperature between the A and 950, whereafter the normalization is once or more times repeated.
  • This method will be referred to as the known normalization method hereinafter.
  • one of the peaks is located at the 1,250 to 1,050 range, namely in the gamma-iron range, while the other is at the 750 to 600 range, namely in the alpha-iron or ferrite range. It was found empirically, furthermore, that the rate of precipitation is far greater at the latter peak range than it is at the former, and that the aluminum nitride particles that precipitate in the latter range contribute more to the improvement of low temperature toughness of the steel than those obtained in the former.
  • the first point in this invention is to have aluminum nitride precipitate in the temperature range of 750 to 600, or from the ferrite matrix. In both embodiments of the process, this is achieved in step (3).
  • the second point is to suppress the precipitation of alluminum nitride, or to allow as little precipitation as possible while the steel is still austenitic.
  • the solution treatment temperature and the cooling rate through the 1,250 to 1,050 range is critical, as specified in the steps (1) and (2).
  • the higher the aluminum and nitrogen contents the higher the solution temperature should be chosen, but a complete dissociation of aluminum nitride as demanded in the known normalization method is not mandatory though desirable.
  • the faster the cooling rate from the solution temperature the better suppressed is the precipitation of aluminum nitride, but a rate as fast or faster than /min. as demanded in the known normalization method is not mandatory.
  • the third point is to recrystallize the steel into the finer granular structure, in which the aluminum nitride particles already precipitated in the 750 to 600 range act as effective nuclei.
  • a finer grain size structure can be obtained when said recrystallization is done by transformation, namely by normalization or quenching treatment. This is step (5).
  • the fourth point relates to the hot working that is to be performed concurrently with step (2), which is mandatory for the second kind of steels.
  • the degree or extent of said hot working should be determined for each steel and each deformation practice, but in the case of flat rolling, a reduction in thickness of at least 20% is necessary.
  • the fifth point is to reheat the steel, once it has been cooled through the 750 to 600 range, up to the subsequent heat treatment temperature without letting it cool to room temperatures.
  • This is step (4), by which a great quantity of heat is conserved to contribute to the improvement of heat economy. Also, the entire manufacturing procedure is much simplified and the production cost is reduced, Should the heat economy be disregarded in favor of other considerations, such as, for example, of production convenience, the steel may be allowed to cool through to room temperatures without affecting the quality of the product steel, provided other points are satisfied.
  • the second point is the choice and prescription of nitride-forming metallic element with respect to the nitrogen content.
  • aluminum of approximately 1.93 times the nitrogen should be theoretically sufiicient to convert all the nitrogen into aluminum nitride, but in practising this invention, at least approximately 2.5 times of aluminum with reference to the nitrogen content is necessary to bring the free nitrogen to the aforesaid unharmful level.
  • the precipitation temperature ranges of the nitrides of the first three are conveniently coincident with that of steps (4) and (5) in order to do an effective elimination of the free nitrogen off the matrix.
  • the precipitated particles of those three are known to contribute to the improvement of low temperature toughness of the steel.
  • Table 1 gives the chemical composition of steels by check analysis, the balance being substantially iron with incidental or unavoidable impurities, such as sulphur or phosphorus.
  • the steels of the L series are the first kind, those of the H series the second, while the K series relates to commercial steels of such nature as to Example 1
  • the steel L-l of Table 1 was (1) heated to 1,350", (2) cooled through the 1,270-1,000 range in eight minutes, no hot working, (3) held for fifteen minutes at 700, (4) reheated up therefrom, and (5) held for thirty minutes at 930 and cooled in air.
  • the mechanical properties of so made steel are shown in Table 2 as L-l-A.
  • Example 2 The steel L-l of Table 1 was (1) heated to 1,330, (2) hot rolled starting at l,270 and finishing at 1,000, giving a reduction in thickness of 30% while being cooled through the same temperature range in three minutes, the rest the same as in Example 1. This steel is shown in Table 2 as L1B.
  • Example 3 The steel L-2 of Table 1 was (1) heated to 1,330, (2) cooled through the 1,300-1,000 range at a mean cooling rate of 50/min., no hot working, (3) cooled through the 750600 range at a mean cooling rate of /min., (4) reheating from 550, and (5 the same as in Example 1. This is the steel L-2-A in Table 2.
  • Example 4 The steel H-1 of Table 1 was 1) heated to 1,350, (2) rolled starting at 1,350" and finishing at 1,050, giving a reduction in thickness of 45% while being cooled in ten minutes, (3) and (4) the same as in the Example 3, and (5) held for thirty minutes at 930, quenched in water, and held for one hour at 630-660, and cooled in air. This is the steel H-l-A in Table 2.
  • Example 5 The steel H-2 of Table 1 was (1) heated to 1,350, (2) rolled similarly as in the Example 4, except for the reduction in thickness which was 52%, 3) held for thirty minutes at 700, (4) reheated therefrom, and (5) the same as in the Example 4. This is the steel H-2-A in Table 2.
  • Example 6 The steel H-3 of Table 1 was (1) heated to 1,330", (2) rolled starting at 1,275 and finishing at 1,010", giving a reduction in thickness of 36% while being cooled at a mean cooling rate of 65/min., the rest the same as in the Example 5. This is the steel H-3-A in Table 2.
  • Example 7 The steel H-3 of Table 1 was (1) heated to 1,350, (2) rolled starting at 1,350 and finishing at 1,100, giving a reduction in thickness of 35% while being cooled through the 1,250-1,050 range at a mean cooling rate of 30/min., (3) cooled through the 750-600 range in twenty minutes, (4) reheated from 600, and (5) the same as in the Example 4. This is the steel H-3-B in Table 2.
  • Example 8 The steel K-l of Table l was (1) heated to 1,350, (2) cooled through the 1,270-1,000 range in eight minutes, no working, (3) held for fifteen minutes at 700, (4) reheated therefrom, and (5) held for thirty minutes at 930 and cooled in air.
  • Example 9 The steel K-2 of Table 1 was (1) heated to 1,350, (2) rolled starting at l,350 and finishing at 1,050, giving a reduction in thickness of 45% While being cooled through in ten minutes, (3) and (4) the same as in Example 3, and (5) held for thirty minutes at 930, quenched in water, held for one hour in the 630-660 range, and cooled in air.
  • Example 10 The steel H-l of Table 1 was (a) heated to 1,350, (b) rolled starting at 1,350 and finishing at 1,050", giving a reduction in thickness of 45 while being cooled through in ten minutes, (0) allowed to cool to room temperature, ((1) upon reheating to 930, heated through the 600-750 range in fifteen minutes, or at a mean heating rate of 10/min., and (e) held for thirty minutes at 930, quenched in water, tempered in the 630-660 range, and cooled in air.
  • This steel is shown as H-l-B in Table 2.
  • Al stands for acid soluble aluminum.
  • Example 10 34. 5 44. 7 41. 3 26. 2 -38 Example 1. 84. 1 46. 1 40. 1 30. 4 42 Example 2. 33. 8 46. 5 41. 1 25. 0 Example 3. 73. 6 80. 1 24. 9 20. 5 90 Example 4. 74. 1 83. 1 24. l 22. 3 104 Example 5. 97. 8 102. 4 23. 2 19. 0 71 Example 6. 94. 5 100. 3 24. 0 18. 5 68 Example 7. 27. 2 46. 0 41. 7 9. 0 +11 Example 8. 72. 6 81.9 25. 1 18. 5 -66 Exampe 9. 72. 0 82. 5 26. 0 24. 0 107 Example 10.
  • nitride-containing low-carbon structural steels the steel containing, by check analysis, carbon up to 0.25%, total nitrogen at least 0.012%, of which at least 0.010% is present as nitride the nitride being either aluminum nitride alone or supplemented by any one or more nitrides of beryllium, columbium, vanadium, titanium or zirconium, the free uncombined nitrogen being less than 0.003%, the method comprising, (1) heating the steel to at least 1,300 C., (2) in the course of cooling from said temperature, passing the temperature range of 1,250 C. to l,050 C.
  • step (5) is essentially the normalization treatment.
  • step (5) is essentially the quenching or quench-and-tempering treatment.
  • step (3) further cooling by passing the steel through the temperature range of 750 to 600 C. in at least ten minutes.

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3645801A (en) * 1968-12-20 1972-02-29 Bethlehem Steel Corp Method of producing rolled steel having high-strength and low-impact transition temperature
US3713812A (en) * 1970-08-03 1973-01-30 Steel Corp Ferritic stainless steels with improved drawability and resistance to ridging
US3726723A (en) * 1970-05-11 1973-04-10 American Metal Climax Inc Hot-rolled low alloy steels
US3773500A (en) * 1970-03-26 1973-11-20 Nippon Steel Corp High tensile steel for large heat-input automatic welding and production process therefor
US3925111A (en) * 1972-12-31 1975-12-09 Nippon Steel Corp High tensile strength and steel and method for manufacturing same
US4016740A (en) * 1973-12-27 1977-04-12 Nippon Steel Corporation Method and an apparatus for the manufacture of a steel sheet
US4060431A (en) * 1975-08-23 1977-11-29 Thyssen Edelstahlwerke Aktiengesellschaft Heat-treatable steel
US6190472B1 (en) * 1993-03-16 2001-02-20 Ovako Steel Ab Method of soft annealing high carbon steel
US20040108092A1 (en) * 2002-07-18 2004-06-10 Robert Howard Method and system for processing castings
US20050072549A1 (en) * 1999-07-29 2005-04-07 Crafton Scott P. Methods and apparatus for heat treatment and sand removal for castings
EP1561833A1 (de) * 2004-02-05 2005-08-10 Edelstahlwerke Südwestfalen GmbH Stahl zur Herstellung von hochfesten Bauteilen mit herausragender Tieftemperaturzähigkeit und Verwendungen eines solchen Stahls
US20050257858A1 (en) * 2001-02-02 2005-11-24 Consolidated Engineering Company, Inc. Integrated metal processing facility
US20050269751A1 (en) * 2001-02-02 2005-12-08 Crafton Scott P Integrated metal processing facility
US20060054294A1 (en) * 2004-09-15 2006-03-16 Crafton Scott P Short cycle casting processing
US20060103059A1 (en) * 2004-10-29 2006-05-18 Crafton Scott P High pressure heat treatment system
WO2007009517A1 (de) * 2005-07-19 2007-01-25 Rud Ketten Rieger & Dietz Gmbh U. Co. Kg Hochfeste stahlkette für den tieftemperaturbereich
US20070289713A1 (en) * 2006-06-15 2007-12-20 Crafton Scott P Methods and system for manufacturing castings utilizing an automated flexible manufacturing system
US20080011446A1 (en) * 2004-06-28 2008-01-17 Crafton Scott P Method and apparatus for removal of flashing and blockages from a casting
US20080236779A1 (en) * 2007-03-29 2008-10-02 Crafton Scott P Vertical heat treatment system
US11408062B2 (en) 2015-04-28 2022-08-09 Consolidated Engineering Company, Inc. System and method for heat treating aluminum alloy castings

Families Citing this family (2)

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US4033789A (en) * 1976-03-19 1977-07-05 Jones & Laughlin Steel Corporation Method of producing a high strength steel having uniform elongation
EP0022134B1 (fr) * 1979-06-08 1985-09-25 Henrik Giflo Acier d'armature à haute résistance mécanique

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US3155496A (en) * 1961-05-16 1964-11-03 Ishikawajima Harima Heavy Ind Manganese-molybdenum ductile steel
US3155549A (en) * 1961-03-11 1964-11-03 Ishikawajima Harima Heavy Ind Steel for high temperature cementation
US3328211A (en) * 1963-12-05 1967-06-27 Ishikawajima Harima Heavy Ind Method of manufacturing weldable, tough and high strength steel for structure members usable in the ashot-state and steel so made

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DE928651C (de) * 1942-04-24 1955-06-06 Otto Dr-Ing Kukla Verfahren zur Herstellung von Gegenstaenden mit hohen Guetewerten aus legierten oderunlegierten Staehlen
DE1184509B (de) * 1960-01-21 1964-12-31 Hoesch Ag Die Verwendung von Stahlblechen oder -baendern zur Herstellung von insbesondere schraubennahtgeschweissten Rohren

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Publication number Priority date Publication date Assignee Title
US3155495A (en) * 1961-03-11 1964-11-03 Ishikawajima Harima Heavy Ind Nitride containing ductile steel
US3155549A (en) * 1961-03-11 1964-11-03 Ishikawajima Harima Heavy Ind Steel for high temperature cementation
US3155496A (en) * 1961-05-16 1964-11-03 Ishikawajima Harima Heavy Ind Manganese-molybdenum ductile steel
US3328211A (en) * 1963-12-05 1967-06-27 Ishikawajima Harima Heavy Ind Method of manufacturing weldable, tough and high strength steel for structure members usable in the ashot-state and steel so made

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3645801A (en) * 1968-12-20 1972-02-29 Bethlehem Steel Corp Method of producing rolled steel having high-strength and low-impact transition temperature
US3773500A (en) * 1970-03-26 1973-11-20 Nippon Steel Corp High tensile steel for large heat-input automatic welding and production process therefor
US3726723A (en) * 1970-05-11 1973-04-10 American Metal Climax Inc Hot-rolled low alloy steels
US3713812A (en) * 1970-08-03 1973-01-30 Steel Corp Ferritic stainless steels with improved drawability and resistance to ridging
US3925111A (en) * 1972-12-31 1975-12-09 Nippon Steel Corp High tensile strength and steel and method for manufacturing same
US4016740A (en) * 1973-12-27 1977-04-12 Nippon Steel Corporation Method and an apparatus for the manufacture of a steel sheet
US4060431A (en) * 1975-08-23 1977-11-29 Thyssen Edelstahlwerke Aktiengesellschaft Heat-treatable steel
US6190472B1 (en) * 1993-03-16 2001-02-20 Ovako Steel Ab Method of soft annealing high carbon steel
US20070289715A1 (en) * 1999-07-29 2007-12-20 Crafton Scott P Methods and apparatus for heat treatment and sand removal for castings
US20050072549A1 (en) * 1999-07-29 2005-04-07 Crafton Scott P. Methods and apparatus for heat treatment and sand removal for castings
US7275582B2 (en) 1999-07-29 2007-10-02 Consolidated Engineering Company, Inc. Methods and apparatus for heat treatment and sand removal for castings
US7258755B2 (en) 2001-02-02 2007-08-21 Consolidated Engineering Company, Inc. Integrated metal processing facility
US7338629B2 (en) 2001-02-02 2008-03-04 Consolidated Engineering Company, Inc. Integrated metal processing facility
US20050257858A1 (en) * 2001-02-02 2005-11-24 Consolidated Engineering Company, Inc. Integrated metal processing facility
US20050269751A1 (en) * 2001-02-02 2005-12-08 Crafton Scott P Integrated metal processing facility
US7641746B2 (en) 2001-02-02 2010-01-05 Consolidated Engineering Company, Inc. Integrated metal processing facility
US20080264527A1 (en) * 2001-02-02 2008-10-30 Crafton Scott P Integrated metal processing facility
US6901990B2 (en) 2002-07-18 2005-06-07 Consolidated Engineering Company, Inc. Method and system for processing castings
US20040108092A1 (en) * 2002-07-18 2004-06-10 Robert Howard Method and system for processing castings
US20070107808A1 (en) * 2004-02-05 2007-05-17 Edelstahlwerke Sudwestfalen Gmbh Steel for production of high-strength components with excellent low-temperature toughness and uses of a steel of this type
EP1561833A1 (de) * 2004-02-05 2005-08-10 Edelstahlwerke Südwestfalen GmbH Stahl zur Herstellung von hochfesten Bauteilen mit herausragender Tieftemperaturzähigkeit und Verwendungen eines solchen Stahls
WO2005075693A1 (de) * 2004-02-05 2005-08-18 Edelstahlwerke Südwestfalen Gmbh Stahl zur herstellung von hochfesten bauteilen mit herausragender tieftemperaturzähigkeit und verwendungen eines solchen stahls
US20080011446A1 (en) * 2004-06-28 2008-01-17 Crafton Scott P Method and apparatus for removal of flashing and blockages from a casting
US20060054294A1 (en) * 2004-09-15 2006-03-16 Crafton Scott P Short cycle casting processing
US20090206527A1 (en) * 2004-10-29 2009-08-20 Crafton Scott P High pressure heat treatment system
US20060103059A1 (en) * 2004-10-29 2006-05-18 Crafton Scott P High pressure heat treatment system
US8663547B2 (en) 2004-10-29 2014-03-04 Consolidated Engineering Company, Inc. High pressure heat treatment system
WO2007009517A1 (de) * 2005-07-19 2007-01-25 Rud Ketten Rieger & Dietz Gmbh U. Co. Kg Hochfeste stahlkette für den tieftemperaturbereich
US20070289713A1 (en) * 2006-06-15 2007-12-20 Crafton Scott P Methods and system for manufacturing castings utilizing an automated flexible manufacturing system
US20080236779A1 (en) * 2007-03-29 2008-10-02 Crafton Scott P Vertical heat treatment system
US11408062B2 (en) 2015-04-28 2022-08-09 Consolidated Engineering Company, Inc. System and method for heat treating aluminum alloy castings

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