EP3645763A1 - Retention of mechanical properties in steel alloys after processing and in the presence of stress concentration sites - Google Patents

Retention of mechanical properties in steel alloys after processing and in the presence of stress concentration sites

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Publication number
EP3645763A1
EP3645763A1 EP18824168.1A EP18824168A EP3645763A1 EP 3645763 A1 EP3645763 A1 EP 3645763A1 EP 18824168 A EP18824168 A EP 18824168A EP 3645763 A1 EP3645763 A1 EP 3645763A1
Authority
EP
European Patent Office
Prior art keywords
alloy
mpa
sheet
thickness
atomic percent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP18824168.1A
Other languages
German (de)
French (fr)
Other versions
EP3645763A4 (en
Inventor
Daniel James Branagan
Alla Sergueeva
Brian E. Meacham
Andrew E. Frerichs
Sheng Cheng
Scott Larish
Grant G. Justice
Andrew T. Ball
Jason K. Walleser
Logan J. TEW
Scott T. ANDERSON
Kurtis Clark
Taylor L. GIDDENS
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
United States Steel Corp
Original Assignee
Nanosteel Co Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanosteel Co Inc filed Critical Nanosteel Co Inc
Priority to EP21206702.9A priority Critical patent/EP3971314A1/en
Priority to EP21206699.7A priority patent/EP3971313A1/en
Publication of EP3645763A1 publication Critical patent/EP3645763A1/en
Publication of EP3645763A4 publication Critical patent/EP3645763A4/en
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B3/00Rolling 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
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/004Heat treatment of ferrous alloys containing Cr and Ni
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/005Heat treatment of ferrous alloys containing Mn
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/008Heat treatment of ferrous alloys containing Si
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0205Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226Hot rolling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B21B2001/225Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length by hot-rolling

Definitions

  • This disclosure is related to retention of mechanical properties in high strength steel at reduced thicknesses and which mechanical property performance is also retained at relatively high strain rates. These new steels can offer advantages for a myriad of applications where reduced sheet thickness is desirable.
  • the alloys herein are those that retain useful mechanical properties after introduction of a geometric discontinuity and an accompanying stress concentration.
  • LSS Low Strength Steels
  • HSS High Strength Steels
  • AHSS Advanced High Strength Steels
  • Advanced High Strength Steels are of primary interest for advanced engineering applications, and are classified by tensile strengths greater than 700 MPa and include such types as martensitic steels (MS), dual phase (DP) steels, transformation induced plasticity (TRIP) steels, and complex phase (CP) steels.
  • MS martensitic steels
  • DP dual phase
  • TRIP transformation induced plasticity
  • CP complex phase
  • tensile elongation of LSS, HSS and AHSS ranges from 25% to 55%, 10% to 45%, and 4% to 30%, respectively.
  • the body-in-white structure of an automobile is designed to provide a rigid structure that will protect the passenger while traveling at speed and in the case of a collision.
  • dynamic loading, rapid deformation, and energy dissipation occurs throughout the automobile and body-in- white structure in particular.
  • the time frame over which this occurs can be 100 ms. High strain rates are observed throughout the body-in-white structure during this time, and materials need to be able to withstand complex loads across a range of strain rates.
  • a low speed collision that occurs in a parking lot would result in a lower strain rate for body-in- white than would a collision at highway speeds.
  • the mechanical properties of materials for the body-in-white structure are measured by many means, including uniaxial tensile testing, across this range of strain rates such that their response during a collision can be predicted and design considerations taken into account.
  • High strain rates can result in a change in mechanical properties, limiting the maximum lightweighting that automobile designers are able to achieve by requiring additional thickness to maintain safety under high strain rate conditions.
  • Martensitic steels provide excellent strength yet require a quench as a final processing step to create the necessary micro structure. Quenching is difficult to control at a small scale and may potentially cause unacceptable distortion in small parts. Final processing may not be performed on the final part geometry but rather on sheet or foils in some applications. For thermally sensitive materials such as martensitic steels, thermal exposure during cutting to produce the final part may detrimentally alter the micro structure and compromise properties. Geometry effects also play a greater role in mechanical properties of ductile materials at the small scale, with the effects of stress concentrators, grain size, and thickness adversely changing the material's mechanical response to stress.
  • the present invention is directed at a method to retain mechanical properties in a metallic sheet alloy at reduced thickness comprising supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C, melting said alloy, cooling at a rate of ⁇ 250 K/s, and solidifying to a thickness of 25.0 mm up to 500 mm. This is followed by processing the alloy into sheet form with thickness Ti with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa).
  • the present invention relates to a method to retain mechanical properties in a metallic sheet alloy at relatively high strain rates comprising supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of ⁇ 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm. This is then followed by processing the alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa) when tested at a strain rate Si.
  • the present invention is directed at A method to retain mechanical properties in a metallic sheet alloy
  • a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of ⁇ 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm.
  • This is then followed by processing the alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa).
  • FIG.s are provided for illustrative purposes and are not to be considered as limiting any aspect of this invention.
  • FIG. 1 Summary of novel ductility achievement in alloys herein at reduced length scales.
  • FIG. 2 Summary of novel ductility achievement in the alloys herein at high strain rates.
  • FIG. 3 Summary of maintained ductility in the alloys herein with introduced stress concentration sites such as edge notches.
  • FIG. 4 Yield strength and ultimate tensile strength as a function of Alloy 2 sheet thickness.
  • FIG. 5 Tensile elongation as a function of Alloy 2 sheet thickness.
  • FIG. 6 Comparison of stress - strain curves for Alloy 2 sheet with different thicknesses.
  • FIG. 7 Effect of sheet thickness on tensile elongation of samples from various alloys.
  • FIG. 8 Effect of sheet thickness on yield strength in samples from various alloys.
  • FIG. 9 Effect of sheet thickness on ultimate tensile strength in samples from various alloys.
  • FIG. 10 SEM images of the microstructure in the center of Alloy 1 sheet samples with various thicknesses; a) 0.7 mm thick cold rolled sheet, b) 0.7 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, and d) 0.5 mm thick cold rolled and annealed sheet.
  • FIG. 11 SEM images of the microstructure in the center of Alloy 2 sheet samples with various thicknesses; a) 1.0 mm thick cold rolled sheet, b) 1.0 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.2 mm thick cold rolled sheet, and f) 0.2 mm thick cold rolled and annealed sheet.
  • FIG. 12 SEM images of the microstructure in the center of Alloy 27 sheet samples with various thicknesses; a) 0.8 mm thick cold rolled sheet, b) 0.8 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.4 mm thick cold rolled sheet, and f) 0.4 mm thick cold rolled and annealed sheet.
  • FIG. 13 SEM images of the microstructure in the center of Alloy 37 sheet samples with various thicknesses; a) 1.4 mm thick cold rolled sheet, b) 1.4 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.3 mm thick cold rolled sheet, and f) 0.3 mm thick cold rolled and annealed sheet.
  • FIG. 14 Schematic illustration of the ASTM D 638 Type V tensile specimen geometry; all dimensions are in millimeters.
  • FIG. 15 Schematic diagram of the direct tension split Hopkinson bar (SHB) device.
  • FIG. 16 Effect of strain rate on the tensile elongation at fracture for Alloy 2 sheet.
  • FIG. 17 Bright-field TEM micrographs of microstructure in gauge section of the sample from
  • FIG. 18 Bright- field TEM micrographs of microstructure in gauge section of the sample from
  • FIG. 19 Bright- field TEM micrographs of micro structure in gauge section of the sample from Alloy 2 sheet tested at strain rate of 100 s "1 ; a) lower magnification image, b) higher magnification image.
  • FIG. 20 Bright-field TEM micrographs of micro structure in gauge section of the sample from
  • FIG. 21 Bright- field TEM micrographs of micro structure in gauge section of the sample from
  • FIG. 22 Bright-field TEM micrographs of micro structure in gauge section of the sample from
  • FIG. 23 Feritscope measurements at the gauge section of the samples from Alloy 2 sheet tested at different strain rates.
  • FIG. 24 Schematic illustration of the notched tensile sample.
  • FIG. 25 Notch diameter with a constant depth of 0.5 mm effect; a) on tensile elongation and b)
  • FIG. 26 Half circle notch diameter effect; a) on tensile elongation and b) on ultimate tensile strength of the sheet from Alloy 2.
  • FIG. 27 SEM images of the fracture surface in the Sample 1 from Alloy 2 with a notch of 1 mm in diameter; a) in the center of the fracture cross section, b) near the edge of the fracture cross section.
  • FIG. 28 SEM images of the fracture surface in the Sample 2 from Alloy 2 with a notch of 6 mm in diameter; a) in the center of the fracture cross section, b) near the edge of the fracture cross section.
  • FIG. 1 represents a summary on mechanical property retention in the alloys herein when reduced in thickness.
  • the starting condition is to supply a metal alloy.
  • This metal alloy will preferably comprise at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C.
  • the alloy chemistry is melted, cooled at a rate of ⁇ 250 K/s, and solidified to a thickness of 25.0 mm and up to and including 500 mm.
  • the casting process can be done in a wide variety of processes including ingot casting, bloom casting, continuous casting, thin slab casting, thick slab casting, thin strip casting, belt casting etc.
  • Preferred methods would be continuous casting in sheet form by thin slab casting, thick slab casting, and thin strip casting.
  • Preferred alloys exhibit a fraction of austenite ( ⁇ -Fe) at least 10 volume percent up to 100 volume percent and all increments in between.
  • the alloy is then processed into sheet form with a thickness Ti that is in the range of 1.2 mm to 10.0 mm, and therefore includes thicknesses of 1.2 mm, 1.3 mm. 1.4 mm 1.5 mm.
  • the steps to produce this sheet at thickness Ti from the cast product can vary depending on specific manufacturing routes and specific targeted goals.
  • thick slab casting as one process route to get to sheet of this targeted thickness.
  • the alloy would be cast going through a water cooled mold typically in a thickness range of 150 to 300 mm in thickness.
  • the cast ingot after cooling would then be preferably prepared for hot rolling which may involve some surface treatment to remove surface defects including oxides.
  • the ingot would then go through a roughing mill hot roller which may involve several passes resulting in a transfer bar slab typically from 15 to 100 mm in thickness. This transfer bar would then go through successive / tandem hot rolling finishing stands to produce hot band coils which have a thickness Ti in the above referenced range from 1.2 mm to 10.0 mm.
  • Another example would be to preferably process the cast material through a thin slab casting process.
  • the newly formed slab goes directly to hot rolling without cooling down with auxiliary tunnel furnace or induction heating applied to bring the slab directly up to targeted temperature.
  • the slab is then hot rolled directly in multi-stand finishing mills which are preferably from 1 to 7 in number.
  • the strip is rolled into hot band coils with thickness Ti in the above referenced range of 1.2 mm to 10.0 mm in thickness.
  • bloom casting would be similar to the examples above but higher thickness might be cast typically from 200 to 500 mm thick and initial breaker steps would be needed to reduce initial cast thickness to allow it to go through a hot rolling roughing mill.
  • Strip casting would be similar but lower thickness might be cast of Ti having a value of 1.2 mm to 10.0 mm in thickness with preferably only one hot rolling stand directly after casting.
  • the specific process in going from the slab material in Step 1 to a preferred thickness Ti of 1.2 mm to 10 mm and then in Step 2 to a preferred thickness in the range of 0.2 mm to less than 1.2 mm may include hot rolling, cold rolling, and/or cold rolling followed by annealing.
  • the alloy thickness may preferably be 0.2 mm, 0.3 mm, 0.4 mm. 0.5 mm. 0.6 mm. 0.7 mm. 0.8 mm. 0.9 mm, 1.0 mm 1.1 mm up to by not including 1.2 mm.
  • Hot rolling is generally used to provide a preferred thickness from 1.2 mm to 10.0 mm and is typically done in roughing mills, finishing mills, and/or Steckel mills.
  • Cold rolling is preferred in Steps 1 and/or Step 2 and is generally done using tandem mills, Z-mills, and/or reversing mills.
  • the cold rolled material depending on property targets may be annealed to restore the ductility lost from the cold rolling process either partially or with restoration of ductility.
  • ductility is reduced and cold rolling will continue until or just before cracking is observed.
  • Restoration of the tensile ductility of the cold rolled sheet generally occurs with heat treatments at 700°C and above. Once the sheet is formed with thickness Ti specified in Step 2, the sheet will then exhibit a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa).
  • Preferred properties for alloys herein in Step 2 would be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa.
  • Step 3 the alloy is preferably cold rolled and annealed in similar manner as in Step 2 to thickness T 2 ⁇ Ti.
  • the thickness of the alloy in Step 3 is identified as T 2 and is less than the thickness Ti in Step 2.
  • FIG. 2 shows a summary on ductility retention of the present disclosure in the alloys herein at relatively high strain rates, that is where the alloys experience a strain rate of S 2 of >0.007 to 1200 s "1 .
  • Step 1 and Step 2 are identical to that described above in relation to FIG. 1.
  • the sheet will then exhibit a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa) when tested at strain rate Si, which is preferably at or below 0.007 s "1 and in the range from 0.007 to 0.0001 s "1
  • Preferred properties for this alloy would be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa.
  • Alloys herein are also shown to avoid brittle fracture when stress concentration sites are introduced such as notches at the sheet edge.
  • a stress concentration site herein is a location on the alloy sheet where stress can be concentrated, including but not limited to geometric discontinuities, such as a notch, hole, cut in the surface, crack, chipped portion, dent, etc.
  • FIG. 3 shows a summary on how changes in mechanical properties are retained in the alloys herein with the introduction of stress concentration sites such as edge notches.
  • Preferred properties for this alloy would again be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa.
  • the sheet that experiences a stress concentration is capable of exhibiting the following in response to a deformation: X 4 ⁇ 0.2Xi (%), an ultimate tensile strength Y 4 ⁇ 0.5Yi (MPa), and a yield strength Z 4 > O.6Z1 (MPa).
  • the preferred properties of the alloy in Step 3 are as follows: X 4 > 2.4%; Y 4 > 350 MPa, and Z 4 > 150 MPa.
  • the alloys herein comprise, consist essentially of, or consist of iron based metal alloys, having greater than 70 at. % Fe, and at least four or more elements selected from the following six (6) elements: Si, Mn, Cr, Ni, Cu, and C.
  • the level of impurities of other elements are in the range of 0 to 5000 ppm. Accordingly, if there is 5000 ppm of an element other than the selected elements identified, the level of such selected elements may then in combination be present at a lower level to account for the 5000 ppm impurity, such that the total of all elements present (selected elements and impurities) is 100 atomic percent.
  • the preferred levels of the elements may fall in the following ranges: Si (1.14 to 6.13), Mn (3.19 to 15.17), Cr (0.78 to 8.64); Ni (0.9 to 11.44), Cu (0.37 to 1.87), and C (0.67 to 3.68). Accordingly, it can be appreciated that if four (4) elements are selected, two of the six elements are not selected and may be excluded.
  • a particularly preferred level of Fe is in the range of 73.95 to 84.69 at. %.
  • the level of impurities of other elements are preferably controlled in the range of 0 to 5000 ppm (0 to 0.5 wt%).
  • Impurities can be present at various levels depending on the feedstock used. Impurity elements would commonly include the following elements; Al, Co, N, P, Ti, Mo, W, Ga, Ge, Sb, Nb, Zr, O, Sn, Ca, and S which if present would be in the range from 0 to 5000 ppm (parts per million) (0 to 0.5 wt%) at the expense of the desired elements noted above. Preferably, the level of impurities is controlled to fall in the range of 0 to 3000 ppm (0.3 wt%).
  • Step 1 in FIG. 1, FIG. 2 and FIG. 3 The melt was allowed to cool under vacuum for 200 seconds before the chamber was filled with argon to atmospheric pressure.
  • Laboratory casting corresponds to Step 1 in FIG. 1, FIG. 2 and FIG. 3 and provides slabs with thickness of 50 mm. Depending on equipment capability, slab thickness in Step 1 can vary from 25.0 to 500 mm.
  • a sample of between 50 and 150 mg from each alloy herein was taken in the as-cast condition. This sample was heated to an initial ramp temperature between 900°C and 1300°C depending on alloy chemistry, at a rate of 40°C/min. Temperature was then increased at 10°C/min to a max temperature between 1425°C and 1515°C depending on alloy chemistry. Once this maximum temperature was achieved, the sample was cooled at a rate of 10°C/min back to the initial ramp temperature before being reheated at 10°C/min to the maximum temperature.
  • DSC Differential Scanning Calorimetry
  • Laboratory Hot Rolling The alloys herein were preferably processed into a laboratory hot band by hot rolling of laboratory slabs at high temperatures.
  • Laboratory alloy processing is developed to simulate the hot band production from slabs produced by continuous casting.
  • Industrial hot rolling is performed by heating a slab in a tunnel furnace to a target temperature, then passing it through either a reversing mill or a multi-stand mill or a combination of both to reach the target gauge. During rolling on either mill type, the temperature of the slab is steadily decreasing due to heat loss to the air and to the work rolls so the final hot band is formed at a reduced temperature. This is simulated in the laboratory by heating in a tunnel furnace to between 1100°C and 1250°C, then hot rolling.
  • the laboratory mill is slower than industrial mills causing greater loss of heat during each hot rolling pass so the slab is reheated for 4 minutes between passes to reduce the drop in temperature, the final temperature at target gauge when exiting the laboratory mill commonly is in the range from 800°C to 1000°C, depending on furnace temperature and final thickness.
  • Tensile specimens were cut from laboratory hot band using wire EDM. Tensile properties were measured on an Instron mechanical testing frame (Model 3369), utilizing Instron's Bluehill control and analysis software. Samples were tested under displacement control at a constant displacement rate of 0.036 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 4.4xl0 "4 s "1 to 6.8xl0 "3 s "1 , depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used.
  • Tensile properties of the alloys in the hot rolled condition with a thickness from 1.8 to 2.3 mm are listed in Table 3 including magnetic phases volume percent (Fe%) that was measured by Feritscope.
  • the ultimate tensile strength values may vary from 913 to 2011 MPa with tensile elongation from 13.0 to 69.5%. The yield strength is in a range from 250 to 1313 MPa.
  • Mechanical properties of the hot band from steel alloys herein depend on alloy chemistry, processing conditions, and material mechanistic response to the processing conditions.
  • the relative magnetic phases volume percent was measured by Feritscope with the magnetic phases volume percent of 0.1 to 64.9 Fe% in a hot band depending on alloy chemistry. Note that the Table 3 properties correspond to Step 2 of FIG. 1, FIG. 2, and FIG. 3. Further processing of the hot band can additionally occur through cold rolling and annealing as shown for example in Case Example 1.
  • the hot band from alloys herein listed in Table 1 was cold rolled to final target gauge thickness of 1.2 mm through multiple cold rolling passes.
  • Cold rolling is defined as rolling at ambient temperature.
  • Hot band material was media blasted prior to cold rolling to remove surface oxides which could become embedded during the rolling process.
  • the resultant cleaned sheet material was rolled using a Fenn Model 061 2 high rolling mill. Sheet was fed through the rolls, and the roll gap is reduced for each subsequent pass until the desired thickness is achieved or the material hardens to the point where additional rolling does not achieve significant reduction in thickness. Annealing was applied before next rolling to recover ductility. Multiple cycles of cold rolling and annealing might be applied. Once the final gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM.
  • Tensile properties of 1.2 mm thick sheet from alloys herein after cold rolling are listed in Table 4.
  • the ultimate tensile strength values after cold rolling is in a range from 1360 to 2222 MPa; yield strength varies from 1006 to 2073 MPa and tensile elongation is recorded in the range from 4.2 to 37.2%.
  • the magnetic phases volume percent was measured by Feritscope in a range from 1.6 to 84.9 Fe% in a cold rolled sheet depending on alloy chemistry.
  • Table 4 Tensile Properties of 1.2 mm Thick Sheet from the Alloys After Cold Rolling
  • the samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process representing final treatment of sheet material in Step 2 in FIG. 1, FIG. 2 and FIG. 3.
  • Samples were loaded into a furnace preheated to 850°C, and held at temperature for 10 minutes, wrapped in foil and held under a steady argon flow to minimize oxidation damage. Samples were removed at temperature and allowed to air cool to ambient temperature before testing.
  • Tensile properties were measured on an Instron mechanical testing frame (Model 3369), utilizing Instron' s Bluehill control and analysis software.
  • Tensile properties of 1.2 mm sheet from alloys herein after annealing are listed in Table 5.
  • the ultimate tensile strength values of the annealed sheet from alloys herein is in a range from 725 to 2072 MPa; yield strength varies from 267 to 1428 MPa and tensile elongation is recorded in the range from 12.8 to 76.9%.
  • the relative magnetic phases volume percent was measured by Feritscope with the magnetic phases volume percent of 0.2 to 68.2 Fe% depending on alloy chemistry.
  • Properties of cold rolled and annealed sheet from Alloys herein corresponds to Step 2 in FIG. 1, FIG. 2 and FIG. 3.
  • This Case Example demonstrates properties of the sheet material from alloys herein with thickness of 1.2 to 1.4 mm and tested at strain rates from 4.4xl0 "4 s "1 to 6.8xl0 "3 s "1 .
  • the hot band from Alloy 2 was cold rolled into sheets with different thicknesses through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. Samples were left in the furnace for 10 minutes while the furnace purged with argon before being removed and allowed to air cool. The only exception was the final anneal for the 4.8 mm material. This anneal was an 850°C 20 min air cooled anneal, as opposed to the 10 minute anneal used for every other thickness.
  • FIG. 4 and FIG. 5 show the tensile properties of Alloy 2 sheet as a function of the thickness. Average tensile elongation is 53.7% for Alloy 2 sheet with thickness varying from 0.20 to 1.03 mm (as compared to average of 61.5% in Alloy 2 sheet with thickness of 1.2 mm). Slightly higher elongation is observed up to 66.4% in thicker sheet samples above 1.2 mm. The stress - strain curves in FIG. 6 also demonstrate consistent properties and stress-strain behavior in sheet samples with different thicknesses.
  • This Case Example demonstrates that high ductility maintained in the sheet with thickness in a wide range from 4.8 mm down to as small as 0.2 mm. Reduction in sheet thickness below 1.2 mm results in an average total elongation that is no less than that in the sheet with 1.2 mm thickness and above minus 7.8%. An average ultimate tensile strength is 25 MPa less than that in the corresponding sheet with 1.2 mm thickness and above and average yield strength is 67 MPa less.
  • the hot band from Alloy 1, Alloy 27, and Alloy 37 was cold rolled in to sheets with different thicknesses less than 1.2 mm through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process representing final treatment at sheet processing in Step 2 in FIG. 1. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. Samples were left in the furnace to 10 minutes while the furnace purged with argon before being removed and allowed to air cool.
  • tensile elongation is measured in the range from 44.9 to 51.1%, for Alloy 27 in the range from 63.8 to 73.8%, and for Alloy 37 in the range from 6.0 to 7.0%.
  • Tensile elongation as a function of the sheet thickness is illustrated in FIG. 6 for the selected alloys.
  • FIG. 8 and FIG. 9 show the yield strength and ultimate tensile strength of the sheet with different thicknesses for the selected alloys.
  • the ultimate tensile strength is in a range from 1203 to 1269 MPa in Alloy 1 sheet, from 972 to 1067 MPa in Alloy 27 sheet, and from 1493 to 1614 MPa in Alloy 37 sheet.
  • Yield strength varies from 375 to 444 MPa in Alloy 1 sheet, from 367 to 451 MPa in Alloy 27 sheet, and from 612 to 820 MPa in Alloy 37 sheet.
  • This Case Example demonstrates that tensile ductility of alloys herein is maintained event thickness as small as 0.2 mm demonstrating an average total elongation no less than that in the corresponding sheet with 1.2 mm thickness and above minus 7.3%.
  • An average ultimate tensile strength is a range of ⁇ 35 MPa of that in the corresponding sheet with 1.2 mm thickness and above with the yield strength in a range of ⁇ 98 MPa.
  • the hot band from Alloy 1, Alloy 2, Alloy 27, and Alloy 37 was cold rolled in to sheets with different thicknesses less than 1.2 mm through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. The microstructures of the cold rolled and annealed state were studied by SEM to show the structural change during processing.
  • FIG. 10 shows microstructures in Alloy 1 sheet samples with different thicknesses.
  • Cold rolled structure is shown in FIG. 10a and FIG. 10c in the center of the sheet with thickness of 0.7 and 0.5 mm, respectively.
  • the cold rolled sample bears the highly deformed microstructure in which grain boundaries are difficult to see.
  • the microstructure in these sheet samples after annealing is shown in FIG. 10b and FIG. lOd represented by the recrystallized structure with equiaxed grains and clear grain boundaries.
  • FIG. 11 shows microstructures in Alloy 2 sheet samples with different thicknesses.
  • Cold rolled structure is shown in FIG. 11a, FIG. 11c and FIG. l ie in the center of the sheet with thickness of 1.0, 0.5 and 0.2 mm, respectively.
  • the cold rolled sample bears the highly deformed microstructure in which grain boundaries are difficult to see.
  • the microstructure in these sheet samples after annealing is shown in FIG. l ib, FIG. l id and FIG. 1 If represented by recrystallized structure with equiaxed grains and clear grain boundaries.
  • the structure in the sheet samples from Alloy 27 is similar to Alloy 1 and Alloy 2 and is shown in FIG. 12.
  • the recrystallized microstructure in the sheet from Alloy 27 has fewer twins as compared to other studied alloys, as shown in FIG. 12b, FIG. 12d and FIG. 12f.
  • Alloy 37 is a different type of the alloy in which the annealing does not lead to the typical recrystallized structure formation.
  • FIG. 13 shows the structures at the center of the sheet from Alloy 37 with different thicknesses after cold rolling and after cold rolling and annealing. Only a small difference between the cold rolled and the annealed structures is observed. Corresponding samples at different thicknesses have effectively identical structures.
  • This Case Example demonstrates that microstructure is maintained in alloys herein after annealing of cold rolled sheet independently from the final sheet thickness.
  • the tensile properties of the material were characterized as a function of strain rate. Tensile samples were tested at 0.0007 s "1 , 0.7 s “1 , 10 s “1 , 100 s “1 , 500 s “1 and 1200 s “1 nominal strain rates in the ASTM D638 Type V tensile geometry shown in FIG. 14. Tensile samples tested at strain rates from 0.0007 s "1 to 500 s "1 were tested on an MTS servo-hydraulic test frame. Samples were inserted into grips and load was applied by raising the crosshead at speeds necessary to produce the nominal strain rates.
  • a slack adapter consisting of a cup and cone rod assembly was used at strain rates greater than 1 s "1 to allow the test frame to achieve the targeted constant strain rate prior to applying load to the specimen.
  • An instrumented bar was used at 500 s "1 to mitigate the effects of standing waves in the test apparatus that occurred during high strain rate testing.
  • a split Hopkinson bar (SHB) was used.
  • the SHB device was composed of 25.4 mm diameter 7075 Al incident and transmission bars, with the test specimen tightly gripped between the Al bars. Strain gauges were used on the transmission and incident bars to measure strain in the bars.
  • a striker tube was launched around the incident tube towards the striker plate to generate the tensile strain pulse and the strain within the sample was recorded.
  • a schematic diagram of the SHB is provided in FIG. 15.
  • Measured strain at failure is provided in Table 8. The measured strain is plotted as function of strain rate in FIG. 16. Table 9 provides the average ductility as measured by tensile elongation at failure for each nominal strain rate. Note that the average tensile elongation measured at all strain rates is close to the overall average of 55.5% across all strain rates. At strain rates from 0.0007 s "1 to 500 s "1 , the average tensile elongation at failure is within approximately +3% of the total average of all tests. Tests at 1200 s "1 were measured to possess higher tensile elongation at failure than all other tests, however due to the nature of this test methodology these values may be measured slightly higher than actual values. Ultimate tensile strength is measured in a range from 944 to 1187 MPa with yield strength from 347 to 512 MPa (Table 10).
  • Tensile properties in Tables 8 through 10 represents sheet material in Step 3 in FIG. 2.
  • microstructures of the samples from sheet from Alloy 2 tested at five different strain rates ranging from 0.0007 s "1 to 1200 s "1 (see Case Example #5) were studied by TEM.
  • pieces are cut from the gauge section of deformed samples by diamond saw. Grinding and polishing are then undertaken to make thin foils from the cut pieces. The polishing was conducted progressively with 9 ⁇ , 6 ⁇ and 1 ⁇ diamond suspension solution, and finally with 0.02 ⁇ silica. Foils with thickness of 70 to 80 ⁇ were obtained after the polishing. Discs of 3 mm in diameter were punched from the foils and the final polishing was fulfilled with electropolishing using a twin-jet polisher. The chemical solution used was a 30% Nitric acid mixed in Methanol base.
  • the TEM specimens may be ion-milled using a Gatan Precision Ion Polishing System (PIPS).
  • PIPS Gatan Precision Ion Polishing System
  • the ion-milling usually is done at 4.5 keV, and the inclination angle is reduced from 4° to 2° to open up the thin area.
  • the TEM studies were done using a JEOL 2100 high-resolution microscope operated at 200 kV.
  • FIG. 17 shows the bright-field TEM images of the sample tested at 1200 s "1 . It can be seen that deformation twins are prominent in the high rate deformed sample which are a forming of twinning which does not occur through mechanical deformation but during heat treatment. The twins are distinct and sharp, suggesting that they are newly formed from the deformation. With twinning being a deformation mode in the sample, phase transformation is reduced since the deformation twins maintain austenitic structure. Twinning as a method of deformation can be seen in the sample deformed at strain rates of 500, 100, 10,' and 0.7 s "1 , as shown in FIG. 18 through FIG. 21. The sample deformed at strain rate of 0.0007 s "1 has different structure as can be seen in FIG.
  • the magnetic phases volume percent which correlates to the transformed product phases, is highest in the case of deformation at low strain rate of 0.0007 s "1 .
  • This Case Example demonstrates the alteration of deformation mechanisms during deformation of the alloys herein with higher occurrence of twinning with increasing strain rate.
  • Deformation by twinning at high strain rates suppresses the phase transformation (i.e. means that the total amount of ferrite produced is reduced) allowing to the retention of relatively high tensile ductility of the sheet material in a wide range of strain rates.
  • Tensile specimens were cut from the sheet via wire EDM. The specimens had two notches, symmetric at about the center of the width and the length as showed in FIG. 24. Samples were tested in tension with one grip fixed and the other moving at a fixed rate of 0.125 mm/s displacement rate. Tensile properties were measured on an Instron mechanical testing frame, utilizing Instron' s Bluehill control and analysis software. All tests were run at ambient temperature in displacement control. A 50 mm gauge length was used centered on the notch. Stresses were calculated based on the nominal width not the notched width (FIG. 24).
  • Tensile properties of the Alloy 2 sheet samples as a function of notch diameter and notch depth are listed in Table 11. Tensile elongation of notched samples ranged from 12.4% to 40.7%, yield strength ranged from 298 to 420 MPa, and ultimate tensile strength ranged from 636 to 1123 MPa. Effect of notch diameter with constant depth of 0.5 mm on tensile properties of the sheet from Alloy 2 is illustrated in FIG. 25. Changes in tensile properties of the sheet with half circle notches as a function of notch diameter are shown in FIG. 26. This data represents sheet in Step 3 in FIG. 3.
  • This Case Example demonstrates an increase in tensile elongation of the notched samples from alloys herein with increasing notch diameter at constant depth. In the case of increasing depth, average elongation is shown to be independent of the notch depth (half circle).
  • FIG. 27 and FIG. 28 SEM images of fracture surface after tensile testing are shown for Sample 1 and Sample 2, respectively. Images are taken from the center of the fracture cross section and close to the edge. Both samples demonstrated ductile fracture. There is no difference in fracture mode between the center and the edge of the fracture cross section although finer structure is found closer to the edge.
  • the alloys herein may be utilized in variety of applications.
  • the alloys herein may be positioned in vehicular frame, vehicle chassis or vehicle panel.
  • the alloys herein may be utilized for a storage tank, freight car, or railway tank car.
  • Railway tank cars may specifically include tanks, jacketed tanks or tanks with a headshield.
  • Other applications include body armor, metallic shield, military vehicles, and armored vehicle Such applications apply to the alloys produced according to any one of FIG. 1, FIG. 2 and/or FIG. 3.

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Abstract

This invention is related to retention of mechanical properties in high strength steel at reduced thicknesses and which mechanical property performance is also retained at relatively high strain rates. These new steels can offer advantages for a myriad of applications where reduced sheet thickness is desirable. In addition, the alloys herein are those that retain useful mechanical properties after introduction of a geometric discontinuity and an accompanying stress concentration.

Description

Retention Of Mechanical Properties In Steel Alloys After Processing And In The Presence
Of Stress Concentration Sites
Field of Invention
This disclosure is related to retention of mechanical properties in high strength steel at reduced thicknesses and which mechanical property performance is also retained at relatively high strain rates. These new steels can offer advantages for a myriad of applications where reduced sheet thickness is desirable. In addition, the alloys herein are those that retain useful mechanical properties after introduction of a geometric discontinuity and an accompanying stress concentration.
Background
Steel is the engineering material of choice where cost, strength, and ductility are major factors. Accordingly, steel continues to be used in a myriad of applications in our daily lives, including in the construction of buildings, appliances, and automobiles. A large variety of steel alloys exist to achieve this range of needs, with targeted property ranges used for these wide ranging applications. Designations are provided for ranges of steel, which fit three distinct classes based upon measured properties, in particular maximum tensile strain and tensile stress prior to failure. These three classes are: Low Strength Steels (LSS), High Strength Steels (HSS), and Advanced High Strength Steels (AHSS). Advanced High Strength Steels (AHSS) are of primary interest for advanced engineering applications, and are classified by tensile strengths greater than 700 MPa and include such types as martensitic steels (MS), dual phase (DP) steels, transformation induced plasticity (TRIP) steels, and complex phase (CP) steels. As the strength level increases the trend in maximum tensile elongation (ductility) of the steel is negative, with decreasing elongation at high tensile strengths. For example, tensile elongation of LSS, HSS and AHSS ranges from 25% to 55%, 10% to 45%, and 4% to 30%, respectively.
An area where steel provides particular engineering advantages is in automobiles, with many different types of steels utilized throughout the car in various locations. Current consumer desires and governmental regulations are pushing automobile manufacturers to design vehicles that attain ever greater fuel efficiency. Automobile designers have identified weight reduction, particularly in the body-in-white structure, to have the greatest potential impact on improving fuel efficiency. The process of reducing automobile weight, known as lightweighting, can be accomplished through reducing the thickness of the body-in-white structure and increasing the geometric complexity of the various parts using high strength, high formability materials. Accordingly, increasingly high strength steels are desired throughout the automobile assembly in order to enable the thickness reduction and weight savings.
Safety must be kept constant or improved during the lightweighting process as well. Automobile highway speed limits are regularly increasing, and consumers expect safety performance to be a major part of automobile design. The body-in-white structure of an automobile is designed to provide a rigid structure that will protect the passenger while traveling at speed and in the case of a collision. During an automobile collision, dynamic loading, rapid deformation, and energy dissipation occurs throughout the automobile and body-in- white structure in particular. The time frame over which this occurs can be 100 ms. High strain rates are observed throughout the body-in-white structure during this time, and materials need to be able to withstand complex loads across a range of strain rates. For instance, a low speed collision that occurs in a parking lot would result in a lower strain rate for body-in- white than would a collision at highway speeds. The mechanical properties of materials for the body-in-white structure are measured by many means, including uniaxial tensile testing, across this range of strain rates such that their response during a collision can be predicted and design considerations taken into account. High strain rates can result in a change in mechanical properties, limiting the maximum lightweighting that automobile designers are able to achieve by requiring additional thickness to maintain safety under high strain rate conditions.
As advances in engineering and technology occur, there is an increasing drive to the small scale. Consumers, and by extension engineers / designers, are regularly searching for products that are size efficient. Consumers seek out products that accomplish the needed task while occupying the smallest volume possible. A good example of this phenomenon can be found in the electronics industry, where cell phones, tablets, and other devices are regularly reduced in size with consecutive design iterations. With the drive of products to smaller and smaller sizes, the demands on engineering materials that the products are made from increase dramatically. As the overall size of a part decreases, defects that are inherent in everyday manufacturing processes can result in significant reductions in material properties. High strength materials are particularly impacted by the reduction of part size to the small or very small due to the complex and often specialized processing required to achieve those properties.
Martensitic steels, for example, provide excellent strength yet require a quench as a final processing step to create the necessary micro structure. Quenching is difficult to control at a small scale and may potentially cause unacceptable distortion in small parts. Final processing may not be performed on the final part geometry but rather on sheet or foils in some applications. For thermally sensitive materials such as martensitic steels, thermal exposure during cutting to produce the final part may detrimentally alter the micro structure and compromise properties. Geometry effects also play a greater role in mechanical properties of ductile materials at the small scale, with the effects of stress concentrators, grain size, and thickness adversely changing the material's mechanical response to stress. Due to these facts, expensive engineering materials are often required for uses on small scale that are either thermally insensitive or have simple processing such as low alloyed or pure materials. Engineers would prefer to not use exotic materials for these applications; however everyday engineering materials are often unavailable for use at reduced thicknesses resulting in the slow adoption of smaller devices due to prohibitive cost and processing requirements.
Summary
In one embodiment, the present invention is directed at a method to retain mechanical properties in a metallic sheet alloy at reduced thickness comprising supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C, melting said alloy, cooling at a rate of < 250 K/s, and solidifying to a thickness of 25.0 mm up to 500 mm. This is followed by processing the alloy into sheet form with thickness Ti with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa). This is then followed by further processing the alloy into a second sheet with reduction in thickness T2 < Ti with the second sheet having a total elongation of X2 = Xi ± 10%, an ultimate tensile strength of Y2 = Yi ± 50 MPa, and a yield strength of Z2 = Zi ± 100 MPa.
In another embodiment the present invention relates to a method to retain mechanical properties in a metallic sheet alloy at relatively high strain rates comprising supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of < 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm. This is then followed by processing the alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa) when tested at a strain rate Si. This is then followed by deforming the sheet from the alloy at a strain rate S2 > Si with the sheet having a total elongation of X3 = Xi ±7%, ultimate tensile strength Y3 = Yi ± 200 MPa, and yield strength Z3 = Zi ± 50 MPa.
In yet another embodiment the present invention is directed at A method to retain mechanical properties in a metallic sheet alloy comprising supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of < 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm. This is then followed by processing the alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa). Then, one may introduce stress concentration sites and then deform the sheet from the alloy with the sheet having a total elongation of X4≥ 0.2Xi (%), an ultimate tensile strength Y4 > 0.5Yi (MPa), and a yield strength Z4 > O.6Z1 (MPa).
Brief Description of the Drawings
The detailed description below may be better understood with reference to the accompanying FIG.s which are provided for illustrative purposes and are not to be considered as limiting any aspect of this invention.
FIG. 1 Summary of novel ductility achievement in alloys herein at reduced length scales. FIG. 2 Summary of novel ductility achievement in the alloys herein at high strain rates. FIG. 3 Summary of maintained ductility in the alloys herein with introduced stress concentration sites such as edge notches.
FIG. 4 Yield strength and ultimate tensile strength as a function of Alloy 2 sheet thickness. FIG. 5 Tensile elongation as a function of Alloy 2 sheet thickness.
FIG. 6 Comparison of stress - strain curves for Alloy 2 sheet with different thicknesses. FIG. 7 Effect of sheet thickness on tensile elongation of samples from various alloys.
FIG. 8 Effect of sheet thickness on yield strength in samples from various alloys. FIG. 9 Effect of sheet thickness on ultimate tensile strength in samples from various alloys.
FIG. 10 SEM images of the microstructure in the center of Alloy 1 sheet samples with various thicknesses; a) 0.7 mm thick cold rolled sheet, b) 0.7 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, and d) 0.5 mm thick cold rolled and annealed sheet.
FIG. 11 SEM images of the microstructure in the center of Alloy 2 sheet samples with various thicknesses; a) 1.0 mm thick cold rolled sheet, b) 1.0 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.2 mm thick cold rolled sheet, and f) 0.2 mm thick cold rolled and annealed sheet.
FIG. 12 SEM images of the microstructure in the center of Alloy 27 sheet samples with various thicknesses; a) 0.8 mm thick cold rolled sheet, b) 0.8 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.4 mm thick cold rolled sheet, and f) 0.4 mm thick cold rolled and annealed sheet.
FIG. 13 SEM images of the microstructure in the center of Alloy 37 sheet samples with various thicknesses; a) 1.4 mm thick cold rolled sheet, b) 1.4 mm thick cold rolled and annealed sheet, c) 0.5 mm thick cold rolled sheet, d) 0.5 mm thick cold rolled and annealed sheet, e) 0.3 mm thick cold rolled sheet, and f) 0.3 mm thick cold rolled and annealed sheet.
FIG. 14 Schematic illustration of the ASTM D 638 Type V tensile specimen geometry; all dimensions are in millimeters.
FIG. 15 Schematic diagram of the direct tension split Hopkinson bar (SHB) device.
FIG. 16 Effect of strain rate on the tensile elongation at fracture for Alloy 2 sheet.
FIG. 17 Bright-field TEM micrographs of microstructure in gauge section of the sample from
Alloy 2 sheet tested at strain rate of 1200 s"1; a) lower magnification image, b) higher magnification image.
FIG. 18 Bright- field TEM micrographs of microstructure in gauge section of the sample from
Alloy 2 sheet tested at strain rate of 500 s"1; a) lower magnification image, b) higher magnification image. FIG. 19 Bright- field TEM micrographs of micro structure in gauge section of the sample from Alloy 2 sheet tested at strain rate of 100 s"1; a) lower magnification image, b) higher magnification image.
FIG. 20 Bright-field TEM micrographs of micro structure in gauge section of the sample from
Alloy 2 sheet tested at strain rate of 10 s"1; a) lower magnification image, b) higher magnification image.
FIG. 21 Bright- field TEM micrographs of micro structure in gauge section of the sample from
Alloy 2 sheet tested strain rate of 0.7 s"1; a) lower magnification image, b) higher magnification image.
FIG. 22 Bright-field TEM micrographs of micro structure in gauge section of the sample from
Alloy 2 sheet tested at strain rate of 0.0007 s"1; a) lower magnification image, b) higher magnification image.
FIG. 23 Feritscope measurements at the gauge section of the samples from Alloy 2 sheet tested at different strain rates.
FIG. 24 Schematic illustration of the notched tensile sample.
FIG. 25 Notch diameter with a constant depth of 0.5 mm effect; a) on tensile elongation and b)
on ultimate tensile strength of the sheet from Alloy 2.
FIG. 26 Half circle notch diameter effect; a) on tensile elongation and b) on ultimate tensile strength of the sheet from Alloy 2.
FIG. 27 SEM images of the fracture surface in the Sample 1 from Alloy 2 with a notch of 1 mm in diameter; a) in the center of the fracture cross section, b) near the edge of the fracture cross section. FIG. 28 SEM images of the fracture surface in the Sample 2 from Alloy 2 with a notch of 6 mm in diameter; a) in the center of the fracture cross section, b) near the edge of the fracture cross section.
Detailed Description of Preferred Embodiments
The retention of mechanical properties in the alloys herein at reduced thickness and relatively high strain rates is illustrated in FIG. 1 and FIG. 2. FIG. 1 represents a summary on mechanical property retention in the alloys herein when reduced in thickness. In Step 1 in FIG. 1, the starting condition is to supply a metal alloy. This metal alloy will preferably comprise at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C. The alloy chemistry is melted, cooled at a rate of < 250 K/s, and solidified to a thickness of 25.0 mm and up to and including 500 mm. The casting process can be done in a wide variety of processes including ingot casting, bloom casting, continuous casting, thin slab casting, thick slab casting, thin strip casting, belt casting etc. Preferred methods would be continuous casting in sheet form by thin slab casting, thick slab casting, and thin strip casting. Preferred alloys exhibit a fraction of austenite (γ-Fe) at least 10 volume percent up to 100 volume percent and all increments in between. The alloy is then processed into sheet form with a thickness Ti that is in the range of 1.2 mm to 10.0 mm, and therefore includes thicknesses of 1.2 mm, 1.3 mm. 1.4 mm 1.5 mm. 1.6 mm, 1.7 mm, 1.8 mm, 1.9 mm, 2.0 mm, 2.1 mm, 2.2 mm, 2.3 mm, 2.4 mm, 2.5 mm, 2.6 mm, 2.7 mm, 2.8 mm, 2.9 mm, 3.0 mm, 3.1 mm, 3.2 mm, 3.3 mm, 3.4 mm, 3.5 mm, 3.6 mm, 3.7 mm, 3.8 mm, 3.9 mm, 4.0 mm, 4.1 mm, 4.2 mm, 4.3 mm, 4.4 mm, 4.5 mm, 4.6 mm, 4.7 mm, 4.8 mm, 4.9 mm and 5.0 mm, 5.1 mm, 5.2 mm, 5.3 mm. 5.4 mm. 5.5 mm, 5.6 mm, 5.7 mm, 5.8 mm, 5.9 mm,
6.0 mm, 6.1 mm, 6.2 mm, 6.3 mm, 6.4 mm, 6.5 mm, 6.6 mm, 6.7 mm, 6.8 mm, 6.9 mm, 7.0 mm,
7.1 mm, 7.2 mm, 7.3 mm, 7.4 mm, 7.5 mm, 7.6 mm, 7.7 mm, 7.8 mm, 7.9 mm, 8.0 mm, 8.1 mm,
8.2 mm, 8.3 mm, 8.4 mm, 8.5 mm, 8.6 mm, 8.7 mm, 8.8 mm, 8.9 mm, 9.0 mm, 9.1 mm, 9.2 mm,
9.3 mm, 9.4 mm, 9.5 mm, 9.6 mm, 9.7 mm, 9.8 mm, 9.9 mm and 10.0 mm.
The steps to produce this sheet at thickness Ti from the cast product can vary depending on specific manufacturing routes and specific targeted goals. As an example, consider thick slab casting as one process route to get to sheet of this targeted thickness. The alloy would be cast going through a water cooled mold typically in a thickness range of 150 to 300 mm in thickness. The cast ingot after cooling would then be preferably prepared for hot rolling which may involve some surface treatment to remove surface defects including oxides. The ingot would then go through a roughing mill hot roller which may involve several passes resulting in a transfer bar slab typically from 15 to 100 mm in thickness. This transfer bar would then go through successive / tandem hot rolling finishing stands to produce hot band coils which have a thickness Ti in the above referenced range from 1.2 mm to 10.0 mm.
Another example would be to preferably process the cast material through a thin slab casting process. In this case, after casting typically forms 35 to 150 mm in thickness by going through a water cooled mold, the newly formed slab goes directly to hot rolling without cooling down with auxiliary tunnel furnace or induction heating applied to bring the slab directly up to targeted temperature. The slab is then hot rolled directly in multi-stand finishing mills which are preferably from 1 to 7 in number. After hot rolling, the strip is rolled into hot band coils with thickness Ti in the above referenced range of 1.2 mm to 10.0 mm in thickness. Note that bloom casting would be similar to the examples above but higher thickness might be cast typically from 200 to 500 mm thick and initial breaker steps would be needed to reduce initial cast thickness to allow it to go through a hot rolling roughing mill. Strip casting would be similar but lower thickness might be cast of Ti having a value of 1.2 mm to 10.0 mm in thickness with preferably only one hot rolling stand directly after casting.
Accordingly, the specific process in going from the slab material in Step 1 to a preferred thickness Ti of 1.2 mm to 10 mm and then in Step 2 to a preferred thickness in the range of 0.2 mm to less than 1.2 mm may include hot rolling, cold rolling, and/or cold rolling followed by annealing. Accordingly, in Step 2, the alloy thickness may preferably be 0.2 mm, 0.3 mm, 0.4 mm. 0.5 mm. 0.6 mm. 0.7 mm. 0.8 mm. 0.9 mm, 1.0 mm 1.1 mm up to by not including 1.2 mm. Hot rolling is generally used to provide a preferred thickness from 1.2 mm to 10.0 mm and is typically done in roughing mills, finishing mills, and/or Steckel mills. Cold rolling is preferred in Steps 1 and/or Step 2 and is generally done using tandem mills, Z-mills, and/or reversing mills. The cold rolled material depending on property targets may be annealed to restore the ductility lost from the cold rolling process either partially or with restoration of ductility. Typically as cold rolling proceeds and higher amounts of gauge reduction occurs, ductility is reduced and cold rolling will continue until or just before cracking is observed. Restoration of the tensile ductility of the cold rolled sheet generally occurs with heat treatments at 700°C and above. Once the sheet is formed with thickness Ti specified in Step 2, the sheet will then exhibit a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa). Preferred properties for alloys herein in Step 2 would be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa.
In Step 3, the alloy is preferably cold rolled and annealed in similar manner as in Step 2 to thickness T2 < Ti. In Step 3, comparing said alloy in Step 1 and after Step 2, the total elongation is maintained at the level where the total elongation X2 = Xi ± 10%,Y2 = Yi ± 50 MPa, and Z2 = Zi ± 100 MPa . The thickness of the alloy in Step 3 is identified as T2 and is less than the thickness Ti in Step 2. The preferred properties of the alloy in Step 3 are as follows: X2 = 2 to 90%; Y2 = 650 MPa to 2150 MPa and Z2 = 150 MPa to 1600 MPa.
FIG. 2 shows a summary on ductility retention of the present disclosure in the alloys herein at relatively high strain rates, that is where the alloys experience a strain rate of S2 of >0.007 to 1200 s"1 . Step 1 and Step 2 are identical to that described above in relation to FIG. 1. Once the sheet is formed with thickness from 1.2 mm to 10.0 mm, the sheet will then exhibit a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa) when tested at strain rate Si, which is preferably at or below 0.007 s"1 and in the range from 0.007 to 0.0001 s"1 Preferred properties for this alloy would be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa. In Step 3, the sheet with thickness from 0.2 mm to less than 1.2 mm is such that when deformed at an engineering strain rate S2 > Si and the alloy exhibits X3 = Xi ± 7%, ultimate tensile strength Y3 = Yi ± 200 MPa, and yield strength Z3 = Zi ± 50 MPa . The preferred properties of the alloy in Step 3 are as follows: X = 5 to 87%; Y = 500 MPa to 2300 MPa, and Z = 200 MPa to 1550 MPa.
Alloys herein are also shown to avoid brittle fracture when stress concentration sites are introduced such as notches at the sheet edge. A stress concentration site herein is a location on the alloy sheet where stress can be concentrated, including but not limited to geometric discontinuities, such as a notch, hole, cut in the surface, crack, chipped portion, dent, etc. FIG. 3 shows a summary on how changes in mechanical properties are retained in the alloys herein with the introduction of stress concentration sites such as edge notches. Once the sheet is formed with thickness from 1.2 mm to 10.0 mm in Step 2 , the sheet will then exhibit a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa). Preferred properties for this alloy would again be tensile elongation from 12 to 80%, ultimate tensile strength values from 700 to 2100 MPa, and yield strength is in a range from 250 to 1500 MPa. In Step 3, the sheet that experiences a stress concentration is capable of exhibiting the following in response to a deformation: X4≥ 0.2Xi (%), an ultimate tensile strength Y4≥ 0.5Yi (MPa), and a yield strength Z4 > O.6Z1 (MPa). The preferred properties of the alloy in Step 3 are as follows: X4 > 2.4%; Y4 > 350 MPa, and Z4 > 150 MPa.
Alloys
The chemical composition of the alloys herein is shown in Table 1 which provides the preferred atomic ratios utilized.
Table 1 Chemical Composition of Alloys (Atomic %)
Alloy Fe Cr Ni Mn Si Cu C
Alloy 16 76.88 2.63 3.74 9.18 5.13 1.65 0.79
Alloy 17 76.83 2.63 3.74 9.85 5.13 1.03 0.79
Alloy 18 76.57 2.63 3.06 10.17 5.13 1.65 0.79
Alloy 19 76.52 2.63 3.06 10.84 5.13 1.03 0.79
Alloy 20 78.02 1.13 3.06 10.84 5.13 1.03 0.79
Alloy 21 80.02 1.13 3.06 10.84 3.13 1.03 0.79
Alloy 22 76.70 2.63 3.40 10.01 5.13 1.34 0.79
Alloy 23 76.20 3.13 3.40 10.01 5.13 1.34 0.79
Alloy 24 75.70 3.63 3.40 10.01 5.13 1.34 0.79
Alloy 25 77.70 2.63 3.40 10.01 4.13 1.34 0.79
Alloy 26 75.70 2.63 3.40 10.01 6.13 1.34 0.79
Alloy 27 77.20 2.63 3.40 10.01 4.13 1.34 1.29
Alloy 28 75.20 2.63 3.40 10.01 6.13 1.34 1.29
Alloy 29 76.98 2.88 3.40 10.01 4.63 1.34 0.76
Alloy 30 77.23 2.88 3.15 10.01 4.63 1.34 0.76
Alloy 31 77.48 2.88 2.90 10.01 4.63 1.34 0.76
Alloy 32 77.73 2.88 2.65 10.01 4.63 1.34 0.76
Alloy 33 77.98 2.88 2.40 10.01 4.63 1.34 0.76
Alloy 34 74.59 2.61 0.00 15.17 3.59 1.86 2.18
Alloy 35 82.22 3.69 9.94 0.00 2.26 0.37 1.52
Alloy 36 76.17 8.64 0.90 11.77 0.00 1.68 0.84
Alloy 37 82.77 4.41 6.66 3.19 1.14 1.16 0.67
Alloy 38 76.55 0.78 0.72 14.43 3.42 0.42 3.68
Alloy 39 81.44 0.00 4.42 10.33 2.87 0.00 0.94
Alloy 40 81.00 1.22 0.89 13.45 2.66 0.78 0.00
Alloy 41 81.68 2.24 3.25 9.87 0.00 1.55 1.41 Alloy Fe Cr Ni Mn Si Cu C
Alloy 42 78.47 3.16 5.57 7.43 3.70 0.51 1.16
Alloy 43 79.73 3.34 7.02 4.95 3.22 0.46 1.28
Alloy 44 81.47 3.69 10.69 0.00 2.26 0.37 1.52
Alloy 45 80.72 3.69 11.44 0.00 2.26 0.37 1.52
Alloy 46 81.47 3.69 9.94 0.00 2.26 1.12 1.52
Alloy 47 80.72 3.69 9.94 0.00 2.26 1.87 1.52
Alloy 48 81.00 3.69 9.94 0.00 3.70 0.51 1.16
Alloy 49 82.84 1.85 9.94 0.00 3.70 0.51 1.16
Alloy 50 84.69 0.00 9.94 0.00 3.70 0.51 1.16
Alloy 51 82.30 3.69 4.97 3.67 3.70 0.51 1.16
Alloy 52 81.00 3.69 4.97 4.97 3.70 0.51 1.16
Alloy 53 79.70 3.69 4.97 6.27 3.70 0.51 1.16
Alloy 54 83.52 3.69 4.97 3.67 2.26 0.37 1.52
Alloy 55 82.22 3.69 4.97 4.97 2.26 0.37 1.52
Alloy 56 80.92 3.69 4.97 6.27 2.26 0.37 1.52
As can be seen from Table 1, the alloys herein comprise, consist essentially of, or consist of iron based metal alloys, having greater than 70 at. % Fe, and at least four or more elements selected from the following six (6) elements: Si, Mn, Cr, Ni, Cu, and C. The level of impurities of other elements are in the range of 0 to 5000 ppm. Accordingly, if there is 5000 ppm of an element other than the selected elements identified, the level of such selected elements may then in combination be present at a lower level to account for the 5000 ppm impurity, such that the total of all elements present (selected elements and impurities) is 100 atomic percent.
With regards to the above, and as can be further seen from Table 1, preferably, when Fe is present at a level of greater than 70 at. %, and one then selects the four or more elements from the indicated six (6) elements, or selects five or more elements, or selects all six elements to provide a formulation of elements that totals 100 atomic percent. The preferred levels of the elements, if selected, may fall in the following ranges: Si (1.14 to 6.13), Mn (3.19 to 15.17), Cr (0.78 to 8.64); Ni (0.9 to 11.44), Cu (0.37 to 1.87), and C (0.67 to 3.68). Accordingly, it can be appreciated that if four (4) elements are selected, two of the six elements are not selected and may be excluded. If five (5) elements are selected, one of the elements of the six can be excluded. Moreover, a particularly preferred level of Fe is in the range of 73.95 to 84.69 at. %. Again, the level of impurities of other elements are preferably controlled in the range of 0 to 5000 ppm (0 to 0.5 wt%).
Laboratory Slab Casting
Alloys were weighed out into 3,000 to 3,400 gram charges according to the atomic ratios in Table 1 using commercially available ferroadditive powders and a base steel feedstock with known chemistry. As alluded to above, impurities can be present at various levels depending on the feedstock used. Impurity elements would commonly include the following elements; Al, Co, N, P, Ti, Mo, W, Ga, Ge, Sb, Nb, Zr, O, Sn, Ca, and S which if present would be in the range from 0 to 5000 ppm (parts per million) (0 to 0.5 wt%) at the expense of the desired elements noted above. Preferably, the level of impurities is controlled to fall in the range of 0 to 3000 ppm (0.3 wt%).
Charges were loaded into a zirconia coated silica crucible which was placed into an Indutherm VTC800V vacuum tilt casting machine. The machine then evacuated the casting and melting chambers and flushed with argon to atmospheric pressure twice prior to casting to prevent oxidation of the melt. The melt was heated with a 14 kHz RF induction coil until fully molten, approximately from 5 to 7 minutes depending on the alloy composition and charge mass. After the last solids were observed to melt it was allowed to heat for an additional 30 to 45 seconds to provide superheat and ensure melt homogeneity. The casting machine then evacuated the chamber and tilted the crucible and poured the melt into a water cooled copper die. The melt was allowed to cool under vacuum for 200 seconds before the chamber was filled with argon to atmospheric pressure. Laboratory casting corresponds to Step 1 in FIG. 1, FIG. 2 and FIG. 3 and provides slabs with thickness of 50 mm. Depending on equipment capability, slab thickness in Step 1 can vary from 25.0 to 500 mm.
Thermal Analysis
A sample of between 50 and 150 mg from each alloy herein was taken in the as-cast condition. This sample was heated to an initial ramp temperature between 900°C and 1300°C depending on alloy chemistry, at a rate of 40°C/min. Temperature was then increased at 10°C/min to a max temperature between 1425°C and 1515°C depending on alloy chemistry. Once this maximum temperature was achieved, the sample was cooled at a rate of 10°C/min back to the initial ramp temperature before being reheated at 10°C/min to the maximum temperature. Differential Scanning Calorimetry (DSC) measurements were taken using a Netzsch Pegasus 404 DSC through all four stages of the experiment, and this data was used to determine the solidus and liquidus temperatures of each alloy, which are in a range from 1102 to 1505°C (Table 2). Depending on alloys chemistry, liquidus-solidus gap varies from 31 to 138°C. Thermal analysis provides information on maximum temperature for the following hot rolling processes that varies depending on alloy chemistry.
Table 2 Thermal Analysis of Selected Alloys
Alloy 33 1415 1462 48
Laboratory Hot Rolling The alloys herein were preferably processed into a laboratory hot band by hot rolling of laboratory slabs at high temperatures. Laboratory alloy processing is developed to simulate the hot band production from slabs produced by continuous casting. Industrial hot rolling is performed by heating a slab in a tunnel furnace to a target temperature, then passing it through either a reversing mill or a multi-stand mill or a combination of both to reach the target gauge. During rolling on either mill type, the temperature of the slab is steadily decreasing due to heat loss to the air and to the work rolls so the final hot band is formed at a reduced temperature. This is simulated in the laboratory by heating in a tunnel furnace to between 1100°C and 1250°C, then hot rolling. The laboratory mill is slower than industrial mills causing greater loss of heat during each hot rolling pass so the slab is reheated for 4 minutes between passes to reduce the drop in temperature, the final temperature at target gauge when exiting the laboratory mill commonly is in the range from 800°C to 1000°C, depending on furnace temperature and final thickness.
Prior to hot rolling, laboratory slabs were preheated in a Lucifer EHS3GT-B 18 furnace. The furnace set point varies between 1100°C to 1250°C, depending on alloy melting point and point in the hot rolling process, with the initial temperatures set higher to facilitate higher reductions, and later temperatures set lower to minimize surface oxidation on the hot band. The slabs were allowed to soak for 40 minutes prior to hot rolling to ensure they reach the target temperature and then pushed out of the tunnel furnace into a Fenn Model 061 2 high rolling mill. The 50 mm casts are hot rolled for 5 to 10 passes though the mill before being allowed to air cool. Final thickness ranges after hot rolling are preferably from 1.8 mm to 4.0 mm with variable reduction per pass ranging from 20% to 50%.
Tensile specimens were cut from laboratory hot band using wire EDM. Tensile properties were measured on an Instron mechanical testing frame (Model 3369), utilizing Instron's Bluehill control and analysis software. Samples were tested under displacement control at a constant displacement rate of 0.036 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 4.4xl0"4 s"1 to 6.8xl0"3 s"1, depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used.
Tensile properties of the alloys in the hot rolled condition with a thickness from 1.8 to 2.3 mm are listed in Table 3 including magnetic phases volume percent (Fe%) that was measured by Feritscope. The ultimate tensile strength values may vary from 913 to 2011 MPa with tensile elongation from 13.0 to 69.5%. The yield strength is in a range from 250 to 1313 MPa. Mechanical properties of the hot band from steel alloys herein depend on alloy chemistry, processing conditions, and material mechanistic response to the processing conditions. The relative magnetic phases volume percent was measured by Feritscope with the magnetic phases volume percent of 0.1 to 64.9 Fe% in a hot band depending on alloy chemistry. Note that the Table 3 properties correspond to Step 2 of FIG. 1, FIG. 2, and FIG. 3. Further processing of the hot band can additionally occur through cold rolling and annealing as shown for example in Case Example 1.
Table 3 Hot Band Tensile Properties of Alloys
Alloy 20 40.1 1337 376 0.3
Alloy 46 21.9 1917 826 46.0
Alloy 52 23.3 1598 366 24.5 Case Examples
Case Example #1 Tensile Properties of the Sheet at 1.2 mm Thickness
The hot band from alloys herein listed in Table 1 was cold rolled to final target gauge thickness of 1.2 mm through multiple cold rolling passes. Cold rolling is defined as rolling at ambient temperature. Hot band material was media blasted prior to cold rolling to remove surface oxides which could become embedded during the rolling process. The resultant cleaned sheet material was rolled using a Fenn Model 061 2 high rolling mill. Sheet was fed through the rolls, and the roll gap is reduced for each subsequent pass until the desired thickness is achieved or the material hardens to the point where additional rolling does not achieve significant reduction in thickness. Annealing was applied before next rolling to recover ductility. Multiple cycles of cold rolling and annealing might be applied. Once the final gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. Tensile properties were measured on an Instron mechanical testing frame (Model 3369), utilizing Instron' s Bluehill control and analysis software. All tests were run at ambient temperature in displacement control. Samples were tested under displacement control at a constant displacement rate of 0.036 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 4.4X10"4 s"1 to 6.8xl0"3 s"1, depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used.
Tensile properties of 1.2 mm thick sheet from alloys herein after cold rolling are listed in Table 4. The ultimate tensile strength values after cold rolling is in a range from 1360 to 2222 MPa; yield strength varies from 1006 to 2073 MPa and tensile elongation is recorded in the range from 4.2 to 37.2%. The magnetic phases volume percent was measured by Feritscope in a range from 1.6 to 84.9 Fe% in a cold rolled sheet depending on alloy chemistry. Table 4 Tensile Properties of 1.2 mm Thick Sheet from the Alloys After Cold Rolling
Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
17.5 1860 1336
19.7 1742 1014
Alloy 9 17.5 1732 1104 37.0 36.0
18.2 1732 1120
20.1 1715 1038
Alloy 10 20.5 1716 1280 40.3 35.1
20.5 1729 1173
13.9 1893 1320
Alloy 11 15.0 1906 1467 69.9 32.7
15.6 1875 1536
5.5 2125 1913
Alloy 12 5.9 2116 1720 57.0 33.8
4.2 2114 1675
22.8 1500 1182
Alloy 13 24.0 1523 1204 25.6 36.5
23.9 1518 1098
18.6 1790 1561
Alloy 14 20.2 1793 1436 52.1 34.5
17.9 1726 1491
5.0 2051 1784
Alloy 15 6.2 2073 2000 58.9 37.3
6.3 2057 1957
Alloy 16 19.9 1700 1413 42.0 36.9 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
19.7 1689 1436
21.1 1704 1302
20.1 1765 1379
Alloy 17 20.2 1759 1306 45.9 36.0
17.2 1764 1374
20.6 1708 1388
Alloy 18 20.0 1721 1326 44.1 37.3
18.9 1709 1369
18.9 1810 1213
Alloy 19 19.3 1807 1324 44.8 38.0
19.2 1806 1260
15.1 1864 1404
Alloy 20 16.2 1884 1461 54.8 38.3
17.1 1879 1512
18.6 1780 1374
Alloy 21 18.0 1785 1414 54.9 34.1
18.6 1786 1006
17.3 1759 1356
Alloy 22 21.3 1736 1196 43.9 38.0
18.8 1757 1304
19.3 1718 1240
Alloy 23 20.4 1728 1283 41.3 37.4
19.0 1727 1271 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
22.0 1709 1136
Alloy 24 12.6 1695 1256 36.8 37.5
14.8 1706 1258
19.8 1715 1326
Alloy 25 20.2 1704 1320 42.6 33.5
21.0 1700 1316
18.8 1822 1377
Alloy 26 48.5 35.6
17.9 1816 1327
30.7 1442 1146
Alloy 27 29.9 1360 1108 12.6 34.5
24.2 1428 1164
21.0 1625 1215
Alloy 28 26.6 1646 1187 20.6 37.5
23.9 1602 1172
18.1 1718 1483
Alloy 29 18.6 1712 1454 58.3 38.8
19.4 1720 1407
17.7 1770 1335
Alloy 30 17.7 1764 1430 44.6 39.9
17.9 1765 1515
17.5 1834 1524
Alloy 31 16.9 1831 1707 49.4 40.5
16.0 1837 1578 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
15.7 1890 1442
Alloy 32 14.8 1897 1563 50.2 41.1
15.4 1886 1676
15.4 1891 1533
Alloy 33 16.3 1889 1604 56.3 38.2
15.8 1895 1419
10.9 1519 1249
Alloy 34 9.4 1515 1037 1.6 39.0
10.8 1519 1345
16.2 2222 1693
Alloy 35* 16.4 2216 1735 73.7 19.6
16.2 2217 1657
16.4 1641 1116
Alloy 36 20.6 1604 1187 29.6 36.7
19.1 1623 1295
7.1 1949 1617
Alloy 37 6.6 1977 1824 84.9 36.3
6.5 1975 1834
7.0 1727 1539
Alloy 38 9.7 1721 1373 3.8 43.0
10.0 1717 1490
16.0 1869 1289
Alloy 39 50.0 36.5
19.0 1840 1471 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
19.0 1837 1245
15.6 1917 1238
Alloy 40 17.2 1913 1361 45.8 37.4
17.7 1917 1192
28.6 1452 1121
Alloy 41 31.1 1445 1101 26.4 39.2
31.1 1431 1231
21.4 1673 1516
Alloy 42 23.1 1686 1519 35.5 44.9
22.9 1675 1509
37.2 1656 1313
Alloy 43 31.2 1650 1304 38.1 39.2
30.0 1667 1332
19.6 2091 1623
Alloy 44 20.4 2095 1653 57.8 37.1
20.1 2098 1656
21.7 2028 1331
Alloy 45 22.8 2014 1313 50.9 40.9
22.6 2017 1334
18.5 2095 1755
Alloy 46* 18.5 2100 1754 62.2 29.3
19.3 2106 1773
Alloy 47 14.7 2024 1482 57.8 36.2 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
21.3 2020 1496
19.4 2024 1473
11.7 2197 2029
Alloy 48* 11.6 2197 1993 72.6 20.7
10.6 2197 2010
11.1 2138 1985
Alloy 49 11.6 2137 1948 76.6 11.3
11.1 2138 1964
8.7 2166 2041
Alloy 50* 8.0 2168 2060 83.3 26.7
8.5 2170 2073
11.9 2197 1904
Alloy 51* 11.0 2194 1917 68.4 21.0
12.0 2190 1897
15.2 2071 1788
Alloy 52 16.4 2068 1764 55.1 34.6
13.8 2073 1781
22.1 1908 1630
Alloy 53 23.5 1911 1584 45.3 38.5
24.3 1908 1590
7.9 2104 1675
Alloy 54* 5.8 2032 1673 57.5 30.3
7.4 2083 1646 Ultimate Magnetic Cold
Tensile Yield
Tensile Phases Volume Rolling
Alloy Elongation Strength
Strength Percent Reduction
(%) (MPa) (MPa) (Fe%) (%)
8.2 1738 1479
Alloy 55 11.0 1812 1497 44.5 38.1
11.5 1829 1486
28.8 1705 1386
Alloy 56 32.5 1703 1452 32.9 39.4
28.2 1747 1443
* Thickness of 1.2 mm was not achieved in these alloys due to high strength and equipment limitations. Alloys are tested at thickness from 1.3 to 1.4 mm.
The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process representing final treatment of sheet material in Step 2 in FIG. 1, FIG. 2 and FIG. 3. Samples were loaded into a furnace preheated to 850°C, and held at temperature for 10 minutes, wrapped in foil and held under a steady argon flow to minimize oxidation damage. Samples were removed at temperature and allowed to air cool to ambient temperature before testing. Tensile properties were measured on an Instron mechanical testing frame (Model 3369), utilizing Instron' s Bluehill control and analysis software. All tests were run at ambient temperature in displacement control at a constant displacement rate of 0.036 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 4.4xl0"4 s"1 to 6.8xl0"3 s"1, depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used.
Tensile properties of 1.2 mm sheet from alloys herein after annealing are listed in Table 5. The ultimate tensile strength values of the annealed sheet from alloys herein is in a range from 725 to 2072 MPa; yield strength varies from 267 to 1428 MPa and tensile elongation is recorded in the range from 12.8 to 76.9%. The relative magnetic phases volume percent was measured by Feritscope with the magnetic phases volume percent of 0.2 to 68.2 Fe% depending on alloy chemistry. Properties of cold rolled and annealed sheet from Alloys herein corresponds to Step 2 in FIG. 1, FIG. 2 and FIG. 3.
Table 5 Tensile Properties of 1.2 mm Thick Sheet from the Alloys after Annealing
Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
61.0 1238 450
53.9 1208 417
31.5 1440 338
33.1 1475 322
32.7 1483 312
Alloy 7 10.8
33.1 1481 347
31.3 1461 323
32.1 1472 332
56.2 1269 430
Alloy 8 61.3 1225 471 0.9
56.6 1277 421
56.2 1269 430
Alloy 9 61.3 1225 471 1.0
56.6 1277 421
54.3 1238 412
Alloy 10 56.9 1192 397 0.7
59.9 1238 412
41.3 1437 420
44.3 1434 424
Alloy 11 0.9
41.7 1464 412
43.5 1419 417
29.9 1574 379
Alloy 12 2.3
30.1 1571 374 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
29.7 1579 373
62.9 1097 367
Alloy 13 69.8 1121 375 1.0
68.9 1103 368
47.1 1363 372
46.7 1384 376
Alloy 14 1.1
43.8 1365 366
42.6 1386 370
24.2 1528 305
Alloy 15 24.8 1535 308 20.0
26.0 1534 315
54.6 1243 376
55.0 1258 422
Alloy 16 0.9
54.8 1237 376
55.9 1249 382
53.3 1333 406
50.0 1304 410
Alloy 17 0.4
53.6 1289 403
51.1 1323 392
55.2 1238 420
58.7 1198 414
Alloy 18 0.6
56.1 1235 425
53.2 1244 417 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
50.4 1273 451
50.5 1278 416
Alloy 19 0.8
51.0 1348 436
53.2 1299 414
43.4 1378 408
44.7 1362 406
Alloy 20 1.0
34.1 1308 429
28.7 1175 397
52.7 1298 340
46.9 1326 348
Alloy 21 1.6
35.4 1270 349
48.6 1324 350
54.8 1273 399
Alloy 22 54.1 1268 397 0.9
56.1 1297 408
59.3 1239 403
Alloy 23 59.5 1296 407 0.3
56.2 1255 409
60.0 1235 423
Alloy 24 60.1 1247 432 0.7
61.8 1237 428
56.8 1255 376
Alloy 25 0.3
51.6 1244 380 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
57.0 1217 382
51.0 1305 417
Alloy 26 50.0 1311 432 0.7
51.1 1319 433
59.7 1033 387
Alloy 27 53.8 975 368 0.5
63.0 1017 377
41.3 1128 480
45.7 1168 482
Alloy 28 0.2
47.2 1168 485
47.0 1168 492
58.4 1218 370
50.7 1250 386
Alloy 29 1.1
57.3 1251 378
55.1 1239 382
49.0 1297 383
Alloy 30 54.0 1318 445 1.1
53.3 1304 381
45.0 1299 382
47.5 1328 383
Alloy 31 1.2
52.3 1328 392
50.8 1328 397
Alloy 32 50.9 1380 420 1.1 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
43.1 1373 391
52.4 1371 390
45.6 1399 388
36.3 1383 396
Alloy 33 1.1
44.2 1418 398
34.4 1380 410
64.7 993 484
66.1 997 491
Alloy 34 0.3
66.2 994 481
66.3 994 491
14.0 2066 792
14.0 2072 775
Alloy 35* 60.1
14.5 2072 745
13.6 1971 775
50.1 1175 483
Alloy 36 50.9 1161 472 0.9
50.8 1190 471
13.2 1621 635
13.2 1607 645
Alloy 37 68.2
13.5 1586 574
13.4 1600 644
60.3 1134 499
Alloy 38 0.5
58.2 1141 500 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
60.4 1139 500
64.2 1138 490
20.2 929 372
16.2 725 375
Alloy 39 3.0
19.4 827 382
21.9 941 362
15.6 759 379
17.9 888 420
Alloy 40 0.6
17.0 839 368
18.0 849 431
53.0 889 312
Alloy 41 43.5 893 311 1.4
50.9 882 315
68.5 1126 381
74.7 1105 370
Alloy 42 1.4
75.2 1154 384
76.9 1141 375
51.3 1285 344
50.6 1296 352
Alloy 43 3.0
41.2 1132 341
62.4 1284 342
12.8 1898 1269
Alloy 44 57.5
14.0 1959 1272 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
14.1 1962 808
14.1 1961 1235
16.1 1875 540
15.5 1888 517
Alloy 45 51.3
16.0 1867 514
15.4 1878 546
14.2 2007 1125
14.3 2004 879
Alloy 46* 59.0
14.6 1998 866
13.5 2000 903
13.3 1888 1217
14.6 1877 1240
Alloy 47 53.6
13.0 1884 1237
14.2 1892 1253
15.2 1853 1128
Alloy 48* 15.0 1854 1130 59.1
15.4 1852 1131
15.3 1982 1409
15.6 1998 1399
Alloy 49 65.1
14.2 1964 1381
15.4 2008 1428
14.6 1833 1307
Alloy 50* 64.8
14.7 1846 1325 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
14.5 1844 1271
14.4 1844 1387
15.9 1940 1297
Alloy 51* 15.4 1937 1209 57.5
16.0 1929 1223
25.4 1722 314
24.6 1719 267
Alloy 52 23.2
23.8 1706 276
28.6 1717 319
47.3 1492 421
44.1 1514 420
Alloy 53 5.0
38.4 1478 401
48.9 1488 420
17.7 2012 569
17.1 2009 1053
Alloy 54* 50.8
17.0 2017 1158
16.8 2023 1140
35.0 1627 351
Alloy 55 39.6 1656 350 20.6
33.0 1657 358
42.2 1265 388
Alloy 56 41.2 1288 391 6.4
45.9 1345 395 Ultimate Average
Tensile Yield
Tensile Magnetic Phases
Alloy Elongation Strength
Strength Volume Percent
(%) (MPa) (MPa) (Fe%)
47.7 1289 387
* Thickness of 1.2 mm was not achieved in these alloys due to high strength and equipment limitations. Samples were tested at thickness from 1.3 to 1.4 mm.
This Case Example demonstrates properties of the sheet material from alloys herein with thickness of 1.2 to 1.4 mm and tested at strain rates from 4.4xl0"4 s"1 to 6.8xl0"3 s"1.
Case Example #2 Sheet Thickness Effect on Tensile Properties of Alloy 2
The hot band from Alloy 2 was cold rolled into sheets with different thicknesses through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. Samples were left in the furnace for 10 minutes while the furnace purged with argon before being removed and allowed to air cool. The only exception was the final anneal for the 4.8 mm material. This anneal was an 850°C 20 min air cooled anneal, as opposed to the 10 minute anneal used for every other thickness. The purpose of this change was to allow more time for the material to heat up as it was a much thicker sample. Tensile properties were measured on an Instron mechanical testing frame (Model 5984), utilizing Instron's Bluehill control and analysis software. All tests were run at ambient temperature in displacement control. All samples were tested at displacement rate of 0.125 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 9.1xl0"4 s"1 to 1.9xl0"3 s"1 depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used.
The results of tensile testing of the sheet from Alloy 2 processed to different thicknesses are listed in Table 6. In samples with thickness less than 1.2 mm representing Step 3 in FIG. 1, tensile strength varies from 1100 to 1190 MPa and yield strength is between 408 and 439 MPa. FIG. 4 and FIG. 5 show the tensile properties of Alloy 2 sheet as a function of the thickness. Average tensile elongation is 53.7% for Alloy 2 sheet with thickness varying from 0.20 to 1.03 mm (as compared to average of 61.5% in Alloy 2 sheet with thickness of 1.2 mm). Slightly higher elongation is observed up to 66.4% in thicker sheet samples above 1.2 mm. The stress - strain curves in FIG. 6 also demonstrate consistent properties and stress-strain behavior in sheet samples with different thicknesses.
Table 6 Sheet Thickness Effect on Tensile Properties of Alloy 2
Sample Thickness Tensile Elongation Ultimate Tensile Strength Yield Strength
(mm) (%) (MPa) (MPa)
0.41 51.6 1111 438
0.41 53.9 1120 439
0.41 51.1 1100 439
0.21 51.2 1125 434
0.20 51.0 1124 434
This Case Example demonstrates that high ductility maintained in the sheet with thickness in a wide range from 4.8 mm down to as small as 0.2 mm. Reduction in sheet thickness below 1.2 mm results in an average total elongation that is no less than that in the sheet with 1.2 mm thickness and above minus 7.8%. An average ultimate tensile strength is 25 MPa less than that in the corresponding sheet with 1.2 mm thickness and above and average yield strength is 67 MPa less.
Case Example #3 Thickness Effect on Tensile Properties of Sheet from Selected Alloys
The hot band from Alloy 1, Alloy 27, and Alloy 37 was cold rolled in to sheets with different thicknesses less than 1.2 mm through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process representing final treatment at sheet processing in Step 2 in FIG. 1. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. Samples were left in the furnace to 10 minutes while the furnace purged with argon before being removed and allowed to air cool. Tensile properties were measured on an Instron mechanical testing frame (Model 5984), utilizing Instron' s Bluehill control and analysis software. All tests were run at ambient temperature in displacement control. All samples were tested at the displacement rate of 0.125 mm/s, which resulted in sample strain rates, calculated from video strain measurements, ranging from 9.1xl0"4 s"1 to 1.9xl0"3 s"1 depending on several factors including, but not always limited to mechanical compliance, sample slippage, and settling of the wedge action grips used. . The results of tensile testing of the sheet from the alloys processed to different thicknesses are listed in Table 7 representing Step 3 in FIG. 1. For Alloy 1, tensile elongation is measured in the range from 44.9 to 51.1%, for Alloy 27 in the range from 63.8 to 73.8%, and for Alloy 37 in the range from 6.0 to 7.0%. Tensile elongation as a function of the sheet thickness is illustrated in FIG. 6 for the selected alloys. FIG. 8 and FIG. 9 show the yield strength and ultimate tensile strength of the sheet with different thicknesses for the selected alloys. The ultimate tensile strength is in a range from 1203 to 1269 MPa in Alloy 1 sheet, from 972 to 1067 MPa in Alloy 27 sheet, and from 1493 to 1614 MPa in Alloy 37 sheet. Yield strength varies from 375 to 444 MPa in Alloy 1 sheet, from 367 to 451 MPa in Alloy 27 sheet, and from 612 to 820 MPa in Alloy 37 sheet.
Table 7 Tensile Properties of the Sheet from Selected Alloys at Thickness < 1.2 mm
Tensile Ultimate Tensile Yield
Thickness
Alloy Elongation Strength Strength
(mm) (%) (MPa) (MPa)
0.37 67.1 1039 429
0.38 68.6 1040 427
0.38 69.5 1022 425
0.51 68.2 1060 451
0.52 68.5 1056 449
0.75 71.8 1019 413
0.76 71.1 1012 412
1.02 72.9 972 367
1.03 73.8 1005 380
1.04 71.7 1001 369
0.30 6.4 1579 727
0.32 6.0 1493 782
0.32 6.5 1523 790
0.50 6.6 1603 820
0.51 6.3 1614 754
Alloy 37 0.51 6.0 1602 775
0.75 6.7 1602 710
0.77 6.6 1590 612
0.99 6.9 1589 659
1.01 6.8 1588 673
1.01 6.9 1596 648
This Case Example demonstrates that tensile ductility of alloys herein is maintained event thickness as small as 0.2 mm demonstrating an average total elongation no less than that in the corresponding sheet with 1.2 mm thickness and above minus 7.3%. An average ultimate tensile strength is a range of ± 35 MPa of that in the corresponding sheet with 1.2 mm thickness and above with the yield strength in a range of ± 98 MPa.
Case Example #4 Microstructure in Sheet from Selected Alloys at Different Thicknesses
The hot band from Alloy 1, Alloy 2, Alloy 27, and Alloy 37 was cold rolled in to sheets with different thicknesses less than 1.2 mm through multiple cold rolling passes. Once the targeted gauge thickness was reached, samples were cut from each cold rolled sheet by wire EDM. The samples were annealed under conditions intended to simulate the thermal exposure expected during an industrial continuous annealing process. Samples were wrapped in stainless steel foil to prevent oxidation and loaded into a preheated furnace at 850°C. The microstructures of the cold rolled and annealed state were studied by SEM to show the structural change during processing. To prepare SEM samples, pieces were cut by EDM from the sheet and mounted in epoxy, and the sheet cross-sections were polished progressively with 9 μιη, 6 μιη and 1 μιη diamond suspension solution, and finally with 0.02 μιη silica. The SEM study was conducted using an EVO-60 scanning electron microscope manufactured by Carl Zeiss SMT Inc.
FIG. 10 shows microstructures in Alloy 1 sheet samples with different thicknesses. Cold rolled structure is shown in FIG. 10a and FIG. 10c in the center of the sheet with thickness of 0.7 and 0.5 mm, respectively. The cold rolled sample bears the highly deformed microstructure in which grain boundaries are difficult to see. The microstructure in these sheet samples after annealing is shown in FIG. 10b and FIG. lOd represented by the recrystallized structure with equiaxed grains and clear grain boundaries.
FIG. 11 shows microstructures in Alloy 2 sheet samples with different thicknesses. Cold rolled structure is shown in FIG. 11a, FIG. 11c and FIG. l ie in the center of the sheet with thickness of 1.0, 0.5 and 0.2 mm, respectively. The cold rolled sample bears the highly deformed microstructure in which grain boundaries are difficult to see. The microstructure in these sheet samples after annealing is shown in FIG. l ib, FIG. l id and FIG. 1 If represented by recrystallized structure with equiaxed grains and clear grain boundaries. The structure in the sheet samples from Alloy 27 is similar to Alloy 1 and Alloy 2 and is shown in FIG. 12. The recrystallized microstructure in the sheet from Alloy 27 has fewer twins as compared to other studied alloys, as shown in FIG. 12b, FIG. 12d and FIG. 12f.
Alloy 37 is a different type of the alloy in which the annealing does not lead to the typical recrystallized structure formation. FIG. 13 shows the structures at the center of the sheet from Alloy 37 with different thicknesses after cold rolling and after cold rolling and annealing. Only a small difference between the cold rolled and the annealed structures is observed. Corresponding samples at different thicknesses have effectively identical structures.
This Case Example demonstrates that microstructure is maintained in alloys herein after annealing of cold rolled sheet independently from the final sheet thickness.
Case Example #5: Strain Rate Effect on Tensile Ductility of the Sheet from Alloy 2
Slabs of Alloy 2 were cast according to the atomic compositions provided in Table 1. Following casting, the slabs were hot rolled through successively smaller roll gaps to produce hot band coils in the range of 2 to 5 mm thick, which were subsequently subjected to cold rolling and annealing cycles until the targeted thickness of approximately 1.4 mm was achieved representing sheet material in Step 2 in FIG. 2. Annealing was done in this case in the temperature range from 950 to 1050°C.
The tensile properties of the material were characterized as a function of strain rate. Tensile samples were tested at 0.0007 s"1, 0.7 s"1, 10 s"1, 100 s"1, 500 s"1 and 1200 s"1 nominal strain rates in the ASTM D638 Type V tensile geometry shown in FIG. 14. Tensile samples tested at strain rates from 0.0007 s"1 to 500 s"1 were tested on an MTS servo-hydraulic test frame. Samples were inserted into grips and load was applied by raising the crosshead at speeds necessary to produce the nominal strain rates. A slack adapter consisting of a cup and cone rod assembly was used at strain rates greater than 1 s"1 to allow the test frame to achieve the targeted constant strain rate prior to applying load to the specimen. An instrumented bar was used at 500 s"1 to mitigate the effects of standing waves in the test apparatus that occurred during high strain rate testing. At 1200 s"1 strain rate, a split Hopkinson bar (SHB) was used. The SHB device was composed of 25.4 mm diameter 7075 Al incident and transmission bars, with the test specimen tightly gripped between the Al bars. Strain gauges were used on the transmission and incident bars to measure strain in the bars. A striker tube was launched around the incident tube towards the striker plate to generate the tensile strain pulse and the strain within the sample was recorded. A schematic diagram of the SHB is provided in FIG. 15.
Strain in the tensile samples was measured by a mechanical extensometer at 0.0007 s"1 and 0.7 s"1 strain rates. Digital Image Correlation (DIC) was used to measure strain for samples tested at 10 s"1, 100 s"1, and 500 s"1. Five tensile samples were tested at all strain rates. In the case of one sample at 0.0007 s"1 strain rate, a malfunction occurred that resulted in the loss of the sample. Two samples tested at 1200 s"1 did not fail during testing.
Measured strain at failure is provided in Table 8. The measured strain is plotted as function of strain rate in FIG. 16. Table 9 provides the average ductility as measured by tensile elongation at failure for each nominal strain rate. Note that the average tensile elongation measured at all strain rates is close to the overall average of 55.5% across all strain rates. At strain rates from 0.0007 s"1 to 500 s"1, the average tensile elongation at failure is within approximately +3% of the total average of all tests. Tests at 1200 s"1 were measured to possess higher tensile elongation at failure than all other tests, however due to the nature of this test methodology these values may be measured slightly higher than actual values. Ultimate tensile strength is measured in a range from 944 to 1187 MPa with yield strength from 347 to 512 MPa (Table 10).
Tensile properties in Tables 8 through 10 represents sheet material in Step 3 in FIG. 2.
Table 8 Tensile Elongation of Alloy 2 Sheet Samples Tested at Different Strain Rates Nominal Strain Strain Elongation at
Measured Strain Rate
Rate Measurement Failure
Technique (s-1)
(s-1) (%)
0.7 Extensometer 0.644 57.1
0.7 Extensometer 0.682 53.7
0.7 Extensometer 0.632 54.4
0.7 Extensometer 0.634 54.5
0.7 Extensometer 0.650 52.5
10 DIC 5.83 49.5
10 DIC 6.03 50.4
10 DIC 6.07 54.6
10 DIC 6.02 49.5
10 DIC 5.78 54
100 DIC 65.7 55.7
100 DIC 87.9 52.7
100 DIC 88.5 56.2
100 DIC 86.2 54.5
100 DIC 85.4 57.1
500 DIC 438 57.0
500 DIC 442 57.3
500 DIC 440 56.2
500 DIC 414 57.5
500 DIC 425 56.1
1200 SHB 1169 64.9
1200 SHB 1222 67.7
1200 SHB 1152 63.1
Table 9 Average Tensile Elongation of Sheet from Alloy 2 at Each Strain Rate Strain
Nominal Strain Rate Elongation at Failure
Measurement
(s-1) Technique (%)
0.0007 Extensometer 52.8
0.7 Extensometer 54.4
10 DIC 52.0
100 DIC 55.2
500 DIC 56.8
1200 SHB 65.2
Overall Average 56.0
Table 10 Strength Characteristics of Alloy 2 Sheet Tested at Different Strain Rates
Nominal Strain Strain Measured Yield Ultimate Tensile Rate Measurement Strain Rate Strength Strength
(s-1) Technique (s-1) (MPa) (MPa)
100 DIC 65.7 483 956
100 DIC 87.9 499 944
100 DIC 88.5 488 953
100 DIC 86.2 505 956
100 DIC 85.4 459 948
500 DIC 438 425 1020
500 DIC 442 409 1030
500 DIC 440 500 1010
500 DIC 414 444 1030
500 DIC 425 512 1020
1200 SHB 1169 — 946
1200 SHB 1222 — 965
1200 SHB 1152 — 972
This Case Example demonstrates that tensile ductility of alloys herein is retained across a relatively large range of strain rates of 0.007 to 1200 s"1. A measured average ultimate tensile strength is 62 MPa lower at higher strain rates and average yield strength is 59 MPa lower.
Case Example #6 Strain Rate Effect on Microstructure in the Sheet from Alloy 2
The microstructures of the samples from sheet from Alloy 2 tested at five different strain rates ranging from 0.0007 s"1 to 1200 s"1 (see Case Example #5) were studied by TEM. For TEM study, pieces are cut from the gauge section of deformed samples by diamond saw. Grinding and polishing are then undertaken to make thin foils from the cut pieces. The polishing was conducted progressively with 9 μιη, 6 μιη and 1 μιη diamond suspension solution, and finally with 0.02 μιη silica. Foils with thickness of 70 to 80 μιη were obtained after the polishing. Discs of 3 mm in diameter were punched from the foils and the final polishing was fulfilled with electropolishing using a twin-jet polisher. The chemical solution used was a 30% Nitric acid mixed in Methanol base. In case of insufficient thin area for TEM observation, the TEM specimens may be ion-milled using a Gatan Precision Ion Polishing System (PIPS). The ion-milling usually is done at 4.5 keV, and the inclination angle is reduced from 4° to 2° to open up the thin area. The TEM studies were done using a JEOL 2100 high-resolution microscope operated at 200 kV.
FIG. 17 shows the bright-field TEM images of the sample tested at 1200 s"1. It can be seen that deformation twins are prominent in the high rate deformed sample which are a forming of twinning which does not occur through mechanical deformation but during heat treatment. The twins are distinct and sharp, suggesting that they are newly formed from the deformation. With twinning being a deformation mode in the sample, phase transformation is reduced since the deformation twins maintain austenitic structure. Twinning as a method of deformation can be seen in the sample deformed at strain rates of 500, 100, 10,' and 0.7 s"1, as shown in FIG. 18 through FIG. 21. The sample deformed at strain rate of 0.0007 s"1 has different structure as can be seen in FIG. 22 demonstrating a domination of dislocation with phase transformation during deformation that is evident from the Feritscope measurements in the sample gauges after deformation. As shown in FIG. 23, the magnetic phases volume percent, which correlates to the transformed product phases, is highest in the case of deformation at low strain rate of 0.0007 s"1.
This Case Example demonstrates the alteration of deformation mechanisms during deformation of the alloys herein with higher occurrence of twinning with increasing strain rate. Deformation by twinning at high strain rates suppresses the phase transformation (i.e. means that the total amount of ferrite produced is reduced) allowing to the retention of relatively high tensile ductility of the sheet material in a wide range of strain rates.
Case Example #7 Notch Effect on Tensile Properties of Sheet from Alloy 2
Slabs of Alloy 2 were cast according to the atomic compositions provided in Table 1. Following casting, the slabs were hot rolled through successively smaller roll gaps to produce hot band coils, which were subsequently subjected to cold rolling and annealing cycles until the targeted thickness of approximately 1.4 mm was achieved representing sheet in Step 2 in FIG. 3.
Tensile specimens were cut from the sheet via wire EDM. The specimens had two notches, symmetric at about the center of the width and the length as showed in FIG. 24. Samples were tested in tension with one grip fixed and the other moving at a fixed rate of 0.125 mm/s displacement rate. Tensile properties were measured on an Instron mechanical testing frame, utilizing Instron' s Bluehill control and analysis software. All tests were run at ambient temperature in displacement control. A 50 mm gauge length was used centered on the notch. Stresses were calculated based on the nominal width not the notched width (FIG. 24).
Tensile properties of the Alloy 2 sheet samples as a function of notch diameter and notch depth are listed in Table 11. Tensile elongation of notched samples ranged from 12.4% to 40.7%, yield strength ranged from 298 to 420 MPa, and ultimate tensile strength ranged from 636 to 1123 MPa. Effect of notch diameter with constant depth of 0.5 mm on tensile properties of the sheet from Alloy 2 is illustrated in FIG. 25. Changes in tensile properties of the sheet with half circle notches as a function of notch diameter are shown in FIG. 26. This data represents sheet in Step 3 in FIG. 3.
Table 11 Tensile Properties of Notched Specimens from Alloy 2 Sheet
Strain at Ultimate Tensile
Notch Diameter Notch Depth Yield Strength
Break Strength
(mm) (mm) (%) (MPa) (MPa)
2 1 23.0 875 345
4 2 15.6 764 371
4 2 18.7 816 372
4 2 17.9 811 377
6 3 12.4 636 314
6 3 13.1 646 308
6 3 12.9 651 298
2 0.5 22.8 926 405
2 0.5 26.3 992 405
2 0.5 25.8 992 397
4 0.5 27.4 982 394
4 0.5 32.8 1054 391
4 0.5 31.7 1056 396
6 0.5 34.8 1071 383
6 0.5 40.7 1123 384
This Case Example demonstrates an increase in tensile elongation of the notched samples from alloys herein with increasing notch diameter at constant depth. In the case of increasing depth, average elongation is shown to be independent of the notch depth (half circle).
Case Example #8 Ductile Fracture Surface in Notched Sample after Testing
SEM fracture analysis was performed on selected notched specimens from Alloy 2 sheet after tensile testing (see Case Example #7). Two samples with notch radius of 1.0 and 6.0 mm were selected for examination (Table 12). The SEM study was conducted using an EVO-60 scanning electron microscope manufactured by Carl Zeiss SMT Inc. Table 12 Samples for SEM Analysis
In FIG. 27 and FIG. 28, SEM images of fracture surface after tensile testing are shown for Sample 1 and Sample 2, respectively. Images are taken from the center of the fracture cross section and close to the edge. Both samples demonstrated ductile fracture. There is no difference in fracture mode between the center and the edge of the fracture cross section although finer structure is found closer to the edge.
This Case Example demonstrates that notch introduction into the sheet material from alloys herein does not cause brittle catastrophic failure. Notched samples after testing have demonstrated ductile fracture.
The alloys herein may be utilized in variety of applications. For example, the alloys herein may be positioned in vehicular frame, vehicle chassis or vehicle panel. In addition, the alloys herein may be utilized for a storage tank, freight car, or railway tank car. Railway tank cars may specifically include tanks, jacketed tanks or tanks with a headshield. Other applications include body armor, metallic shield, military vehicles, and armored vehicle Such applications apply to the alloys produced according to any one of FIG. 1, FIG. 2 and/or FIG. 3.

Claims

Claims
1. A method to retain mechanical properties in a metallic sheet alloy at reduced thickness comprising: a. supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C, melting said alloy, cooling at a rate of < 250 K/s, and solidifying to a thickness of 25.0 mm up to 500 mm; b. processing said alloy into sheet form with thickness Ti with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa); c. further processing said alloy into a second sheet with reduction in thickness T2 < Ti with the second sheet having a total elongation of X2 = Xi ± 10%, an ultimate tensile strength of Y2 = Yi ± 50 MPa, and a yield strength of Z2 = Zi ± 100 MPa.
2. The method of claim 1 wherein said at least 70 atomic percent iron is combined with five or more elements that are selected from Si, Mn, Cr, Ni, Cu, or C.
3. The method of claim 1 wherein said at least 70 atomic percent iron is combined with all six elements: Si, Mn, Cr, Ni, Cu, and C.
4. The method of claim 1 wherein the levels of the four elements that are selected are as follows:
Si (1.14 to 6.13 atomic percent), Mn (3.19 to 15.17 atomic percent), Cr (0.78 to 8.64 atomic percent); Ni (0.9 to 11.44 atomic percent), Cu (0.37 to 1.87 atomic percent).
5. The method of claim 1 wherein said alloy formed in step (b), exhibits Xi (12 % to 80%), Yi (700 MPa to 2100 MPa), and Zi (250 MPa to 1500 MPa).
6. The method of claim 1 wherein said alloy formed in step (b), exhibits a thickness from 1.2 mm to 10.0 mm.
7. The method of claim 1 wherein said alloy formed in step (c), exhibits X2 (2 to 90 %), Y2 (650 MPa to 2150 MPa), and Z2 (150 MPa to 1600 MPa).
8. The method of claim 1 wherein said alloy formed in step (c), exhibits a thickness from 0.2 mm to < 1.2 mm.
9. The method of claim 1 wherein said alloy formed in step (c) is positioned in a vehicular frame, vehicular chassis, or vehicular panel.
10. The method of claim 1 wherein said alloy formed in step (c) is positioned in a storage tank, freight car, or railway tank car.
11. A method to retain mechanical properties in a metallic sheet alloy at relatively high strain rates comprising: a. supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of < 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm; b. processing said alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa) when tested at a strain rate Si; c. deforming the sheet from said alloy at a strain rate S2 > Si with the sheet having a total elongation of X3 = Xi ±7%, ultimate tensile strength Y3 = Yi ± 200 MPa, and yield strength Z3 = Zi ± 50 MPa.
12. The method of claim 11 wherein said at least 70 atomic percent iron is combined with five or more elements that are selected from Si, Mn, Cr, Ni, Cu, or C.
13. The method of claim 11 wherein said at least 70 atomic percent iron is combined with all six elements: Si, Mn, Cr, Ni, Cu, and C.
14. The method of claim 11 wherein the levels of the four elements that are selected are as follows: Si (1.14 to 6.13 atomic percent), Mn (3.19 to 15.17 atomic percent), Cr (0.78 to 8.64 atomic percent); Ni (0.9 to 11.44 atomic percent), Cu (0.37 to 1.87 atomic percent).
15. The method of claim 11 wherein said alloy formed in step (b), exhibits Xi (12% to 80%), Yi (700 MPa to 2100 MPa), and Zi (250 MPa to 1500 MPa).
16. The method of claim 11 wherein the strain rate Si is 0.007 s"1 to 0.0001 s"1.
17. The method of claim 11 wherein said alloy formed in step (c), exhibits X3 (5% to 87%), Y3 (500 MPa to 2300 MPa), and Z3 (200 MPa to 1550 MPa).
18. The method of claim 11 wherein the strain rate S2 is >0.007 s"1 to 1200 s"1.
19. The method of claim 11 wherein said processing in step (c) comprises roll forming, metal stamping or hydroforming.
20. The method of claim 11 wherein said alloy formed in step (c) is positioned in a vehicular frame, vehicular chassis, or vehicular panel.
21. The method of claim 11 wherein said alloy formed in step (c) is positioned in a storage tank, freight car, or railway tank car.
22. The method of claim 11 wherein said alloy formed in step (c) is positioned in body armor, shield, military vehicle, or armored vehicle.
23. A method to retain mechanical properties in a metallic sheet alloy comprising: a. supplying a metal alloy comprising at least 70 atomic % iron and at least four or more elements selected from Si, Mn, Cr, Ni, Cu, or C and melting said alloy and cooling at a rate of < 250 K/s and solidifying to a thickness of 25.0 mm up to 500 mm; b. processing said alloy into sheet form with thickness from 1.2 mm to 10.0 mm with the sheet having a total elongation of Xi (%), an ultimate tensile strength of Yi (MPa), and a yield strength of Zi (MPa); c. introducing stress concentration sites and then deforming the sheet from said alloy with the sheet having a total elongation of X4≥ 0.2Xi (%), an ultimate tensile strength Y4 > 0.5Yi (MPa), and a yield strength Z4 > O.6Z1 (MPa).
24. The method of claim 23 wherein said at least 70 atomic percent iron is combined with five or more elements that are selected from Si, Mn, Cr, Ni, Cu, or C.
25. The method of claim 23 wherein said at least 70 atomic percent iron is combined with all six elements: Si, Mn, Cr, Ni, Cu, and C.
26. The method of claim 23 wherein the levels of the four elements that are selected are as follows: Si (1.14 to 6.13 atomic percent), Mn (3.19 to 15.17 atomic percent), Cr (0.78 to 8.64 atomic percent); Ni (0.9 to 11.44 atomic percent), Cu (0.37 to 1.87 atomic percent).
27. The method of claim 23 wherein said alloy formed in step (b), exhibits Xi (12% to 80%), Yi (700 MPa to 2100 MPa), and Zi (250 MPa to 1500 MPa).
28. The method of claim 23 wherein said processing in step (c) comprises roll forming, metal stamping or hydroforming.
29. The method of claim 23 wherein said alloy formed in step (c) is positioned in a vehicular frame, vehicular chassis, or vehicular panel.
30. The method of claim 23 wherein said alloy formed in step (c) is positioned in a storage tank, freight car, or railway tank car.
31. The method of claim 23 wherein said alloy formed in step (c) is positioned in body armor, shield, military vehicle, or armored vehicle.
EP18824168.1A 2017-06-30 2018-06-28 Retention of mechanical properties in steel alloys after processing and in the presence of stress concentration sites Withdrawn EP3645763A4 (en)

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