US20040156737A1 - Austenitic stainless steels including molybdenum - Google Patents

Austenitic stainless steels including molybdenum Download PDF

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US20040156737A1
US20040156737A1 US10/360,961 US36096103A US2004156737A1 US 20040156737 A1 US20040156737 A1 US 20040156737A1 US 36096103 A US36096103 A US 36096103A US 2004156737 A1 US2004156737 A1 US 2004156737A1
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stainless steel
austenitic stainless
niobium
molybdenum
manufacture
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James Rakowski
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ATI Properties LLC
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ATI Properties LLC
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Priority to US10/360,961 priority Critical patent/US20040156737A1/en
Assigned to ATI PROPERTIES, INC. reassignment ATI PROPERTIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: RAKOWSKI, JAMES M.
Assigned to PNC BANK, NATIONAL ASSOCIATION reassignment PNC BANK, NATIONAL ASSOCIATION SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ATI PROPERTIES, INC.
Priority to CA2513897A priority patent/CA2513897C/en
Priority to BR0407190-5A priority patent/BRPI0407190A/pt
Priority to CNA2004800035753A priority patent/CN1748042A/zh
Priority to KR1020177006044A priority patent/KR102042324B1/ko
Priority to KR1020057014549A priority patent/KR20050101199A/ko
Priority to CNA2008101463202A priority patent/CN101407890A/zh
Priority to EP04707747A priority patent/EP1592820B1/en
Priority to KR1020137032249A priority patent/KR20130140227A/ko
Priority to PCT/US2004/003045 priority patent/WO2004072316A1/en
Priority to JP2006503284A priority patent/JP4996243B2/ja
Priority to DK04707747T priority patent/DK1592820T3/da
Priority to KR1020127016194A priority patent/KR20120092157A/ko
Priority to KR20147035254A priority patent/KR20150003920A/ko
Priority to DE602004010368T priority patent/DE602004010368T2/de
Priority to ES04707747T priority patent/ES2297377T3/es
Publication of US20040156737A1 publication Critical patent/US20040156737A1/en
Assigned to ATI PROPERTIES, INC. reassignment ATI PROPERTIES, INC. RELEASE BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: PNC BANK, NATIONAL ASSOCIATION, AS AGENT FOR THE LENDERS
Priority to US15/437,180 priority patent/US20170164426A1/en
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D26/00—Shaping without cutting otherwise than using rigid devices or tools or yieldable or resilient pads, i.e. applying fluid pressure or magnetic forces
    • B21D26/02—Shaping without cutting otherwise than using rigid devices or tools or yieldable or resilient pads, i.e. applying fluid pressure or magnetic forces by applying fluid pressure
    • B21D26/033—Deforming tubular bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K31/00—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups
    • B23K31/02—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups relating to soldering or welding
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N13/00—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00
    • F01N13/18—Construction facilitating manufacture, assembly, or disassembly
    • F01N13/1805—Fixing exhaust manifolds, exhaust pipes or pipe sections to each other, to engine or to vehicle body
    • F01N13/1811—Fixing exhaust manifolds, exhaust pipes or pipe sections to each other, to engine or to vehicle body with means permitting relative movement, e.g. compensation of thermal expansion or vibration
    • F01N13/1816—Fixing exhaust manifolds, exhaust pipes or pipe sections to each other, to engine or to vehicle body with means permitting relative movement, e.g. compensation of thermal expansion or vibration the pipe sections being joined together by flexible tubular elements only, e.g. using bellows or strip-wound pipes
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/0014—Devices wherein the heating current flows through particular resistances
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/16—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor the conductor being mounted on an insulating base
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2530/00—Selection of materials for tubes, chambers or housings
    • F01N2530/02—Corrosion resistive metals
    • F01N2530/04—Steel alloys, e.g. stainless steel

Definitions

  • the present invention relates to oxidation and corrosion resistant austenitic stainless steels. More particularly, the present invention relates to austenitic stainless steels adapted for use in high temperature and corrosive environments, such as, for example, use in automotive exhaust system components.
  • the austenitic stainless steels of the invention find particular application in components exposed to temperatures up to 1800° F. (982° C.) and to corrosive environments, such as, for example, chloride-rich waters.
  • metal alloys selected for automotive exhaust system components are exposed to a range of demanding conditions.
  • Durability of automotive exhaust system components is critical because extended lifetimes are demanded by consumers, by federal regulations, and also under manufacturers' warranty requirements.
  • a recent development in these applications is the use of metallic flexible connectors, which act as compliant joints between two fixed exhaust system components.
  • Flexible connectors may be used to mitigate problems associated with the use of welded, slip, and other joints.
  • a material chosen for use in a flexible connector is subjected to a high temperature corrosive environment and must be both formable and have resistance to hot salt corrosion and various other corrosion types, such as, for example, intermediate temperature oxidation, general corrosion, and chloride stress corrosion cracking.
  • Alloys for use in automotive exhaust system flexible connectors often experience conditions in which elevated temperature exposure occurs after the alloy has been exposed to contaminants such as road deicing salts.
  • Halide salts can act as fluxing agents, removing the protective oxide scales which normally form on the connectors at elevated temperatures. Degradation of the connectors may be quite rapid under such conditions. Therefore, simple air oxidation testing may be inadequate to reveal true resistance to corrosive degradation in service.
  • Type 316Ti (UNS Designation S31635).
  • Type 316Ti stainless steel corrodes more rapidly when exposed to elevated temperatures and, therefore, is not generally used in automotive exhaust system flexible connectors when temperatures are greater than approximately 1200° F. (649° C.).
  • Type 316Ti is typically only used for automotive exhaust system components which do not develop high exhaust temperatures.
  • AL 625 is an austenitic nickel-based superalloy possessing excellent resistance to oxidation and corrosion over a broad range of corrosive conditions and displaying excellent formability and strength.
  • Alloys of UNS Designation N06625 generally comprise, by weight, approximately 20-25% chromium, approximately 8-12% molybdenum, approximately 3.5% niobium, and 4% iron. Although alloys of this type are excellent choices for automotive exhaust system flexible connectors, they are quite expensive compared to Type 316Ti alloys.
  • Automotive exhaust system component manufacturers may use other alloys for constructing exhaust system flexible connectors. However, none of those alloys provide high corrosion resistance, especially when exposed to elevated temperatures and corrosive contaminants such as road deicing salts.
  • the present invention addresses the above described needs by providing an austenitic stainless steel comprising, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum and less than 0.8% silicon.
  • the addition of molybdenum to the iron-base alloys increases their resistance to corrosion at high temperatures.
  • composition percentages herein are weight percentages based on total weight of the alloy.
  • the present invention also provides an austenitic stainless steel consisting essentially of, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, 0 to 0.1% carbon, 0 to 1.5% manganese, 0 to 0.05% phosphorus, 0 to 0.02% sulfur, less than 0.8% silicon, 0.15 to 0.6% titanium, 0.15 to 0.6% aluminum, 0 to 0.75% copper, iron, and incidental impurities.
  • the present invention further provides an austenitic stainless steel comprising, by weight, 9 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, 0 to 0.03% titanium, 0.15% to 0.6% aluminum, up to 0.1% carbon, 1 to 1.5% manganese, 0 to less than 0.8% silicon, 0.25 to 0.6% niobium, iron, and incidental impurities.
  • the present invention additionally provides an austenitic stainless steel consisting essentially of, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, 0 to 0.03% titanium, 0.15 to 0.6% aluminum, up to 0.1% carbon, 1 to 1.5% manganese, 0 to less than 0.8% silicon, 0.25 to 0.6% niobium, 0 to 0.75% copper, up to 0.05% phosphorus, up to 0.02% sulfur, up to 0.1 % nitrogen, iron, and incidental impurities.
  • an austenitic stainless steel consisting essentially of, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, 0 to 0.03% titanium, 0.15 to 0.6% aluminum, up to 0.1% carbon, 1 to 1.5% manganese, 0 to less than 0.8% silicon, 0.25 to 0.6% niobium, 0 to 0.75% copper, up to 0.05% phosphorus, up to 0.02% sulfur, up to
  • Certain embodiments of austenitic stainless steels according to the present invention exhibit enhanced resistance corrosion by salt at a broad temperature range up to at least 1500° F. (816° C.).
  • Articles of manufacture of the austenitic stainless steels as described above are also provided by the present invention.
  • the stainless steels of the present invention would find broad application as, for example, automotive components and, more particularly, as automotive exhaust system components and flexible connectors, as well as in other applications in which corrosion resistance is desired.
  • the alloys of the present invention exhibits excellent oxidation resistance at elevated temperatures and therefore, finds broad application in high temperature applications, such as heating element sheaths.
  • the present invention also provides methods of fabricating an article of manufacture from austenitic stainless steels comprising, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, and less than 0.8% silicon.
  • the present invention additionally provides methods of fabricating an article of manufacture wherein the method comprises forming at least a portion of the article of manufacture from an austenitic stainless steel comprising, by weight, 19 to 23% chromium, 30 to 35% nickel, 1 to 6% molybdenum, 0 to 0.03% titanium, 0.15 to 0.6% aluminum, up to 0.1% carbon, 1 to 1.5% manganese, 0 to less than 0.8% silicon, 0.25 to 0.6% niobium, iron, and incidental impurities.
  • Non-limiting examples of articles of manufacture that may be made using such method of the present invention include an automobile, an automotive exhaust system component, an automotive exhaust system flexible connector, a heating element sheath, and a gasket.
  • FIG. 1 is a graph of weight change data comparing the results of hot salt corrosion testing of flat coupon samples of an alloy of the present invention (Sample 2) and prior art alloys coated with 0.0, 0.05 and 0.10 mg/cm 2 salt layers and exposed for 72 hours to 1200° F. (649° C.);
  • FIG. 2 is a graph of weight change data comparing the results of hot salt corrosion testing of flat coupon samples of an alloy of the present invention (Sample 2) and prior art alloys coated with 0.0, 0.05 and 0.10 mg/cm 2 salt layers and exposed for 72 hours to 1500° F. (816° C.);
  • FIG. 3 is a graph of weight change data comparing the results of hot salt corrosion testing of welded teardrop samples of an alloy of the present invention (Sample 2) and prior art alloys coated with a nominal 0.10 mg/cm 2 salt layer and exposed to 1200° F. (649° C.);
  • FIG. 4 is a graph of weight change data comparing the results of hot salt corrosion testing of welded teardrop samples of an alloy of the present invention (Sample 2) and prior art alloys coated with a nominal 0.10 mg/cm 2 salt layer and exposed to 1500° F. (816° C.);
  • FIG. 5 is a graphical illustration of a typical corroded metal sample illustrating terms results of analysis procedure of ASTM G54—Standard Practice for Simple Static Oxidation Testing;
  • FIG. 6 is a depth of penetration graph comparing the results of measurements taken according to ASTM G54 for welded teardrop samples with a nominal 0.10 mg/cm 2 salt coating exposed to 1200° F. (649° C.) for a sample of the alloy of the present invention (Sample 2) and prior art alloys;
  • FIG. 7 is a depth of penetration graph comparing the results of measurements taken according to ASTM G54 for welded teardrop samples with a nominal 0.10 mg/cm 2 salt coating exposed to 1500° F. (816° C.) for a sample of the alloy of the present invention (Sample 2) and prior art alloys; and
  • FIGS. 8 - 12 are micrographs of alloy specimens including varying levels of titanium and niobium, and which were prepared as described in Example 2.
  • the present invention provides austenitic stainless steels resistant to corrosion at elevated temperatures.
  • the corrosion resistant austenitic stainless steels of the present invention find particular application in the automotive industry and, more particularly, in automotive exhaust system components.
  • Austenitic stainless steels are alloys including iron, chromium and nickel.
  • austenitic stainless steels are used in applications requiring corrosion resistance and are characterized by a chromium content above 16% and nickel content above 7%.
  • the process of corrosion is the reaction of a metal or metal alloy with their environment.
  • the corrosion resistance of a metal or alloy in a particular environment is generally determined at least partly by its composition, among other factors.
  • the byproducts of corrosion are generally metal oxides such as iron oxides, aluminum oxides, chromium oxide, etc.
  • the formation of certain oxides, particularly chromium oxide, on stainless steel is beneficial and effectively prevents further degradation of the underlying metal. Corrosion may be accelerated by the presence of heat or corrosive agents.
  • Corrosion resistance of stainless steels used in automotive applications is complicated by exposure to contamination from road deicing salts under conditions of elevated temperature. This exposure results in a complex form of corrosion due to the interaction between the oxides which form at elevated temperatures and the contaminating salts. Elevated temperature oxidation is typified by the formation of protective oxides by reaction of the metal directly with the oxygen in the air.
  • the road deicing salts which deposit on the automotive components may attack and degrade the protective oxide layer. As the protective layer degrades, the underlying metal is exposed to further corrosion.
  • Halide salts, particularly chloride salts tend to promote localized forms of attack such as pitting or grain boundary oxidation.
  • the present austenitic stainless steels include 1 to 6% molybdenum by weight. Molybdenum is added as an alloying agent to provide corrosion resistance, toughness, strength, and resistance to creep at elevated temperatures.
  • the austenitic stainless steels of the present invention also include 19 to 23 weight percent chromium, 30 to 35 weight percent nickel and less than 0.8 weight percent silicon.
  • the present austenitic stainless steels provides better elevated temperature corrosion resistance than the prior art type 316Ti alloys and, therefore, would enjoy more generalized application as an automotive exhaust component.
  • certain alloys within the present invention provide this corrosion resistance at a lower cost than the UNS Designation N06625 alloys because, for example, the present invention is an iron-base alloy, while the N06625 alloys are more expensive nickel-base superalloys.
  • the austenitic stainless steels of the present invention preferably contain greater than 2 weight percent of molybdenum. Another preferred embodiment of the present invention includes less than 4 weight percent molybdenum. This concentration of molybdenum provides improved corrosion resistance at a reasonable cost. Certain embodiments of alloys within the present invention may optionally contain additional alloying components, such as, for example, manganese, phosphorous, sulfur, and copper. Certain embodiments of the stainless steel of the present invention also may contain, for example, from 0.15 to 0.6 weight percent titanium, 0.15 to 0.6 weight percent aluminum, and other incidental impurities.
  • Electric heat element sheaths typically comprise a resistance conductor enclosed in a metal sheath.
  • the resistance conductor may be supported within and electrically insulated from the sheathing by a densely packed layer of refractory, heat-conducting material.
  • the resistance conductor may generally be a helically wound wire member while the refractory heat-conducting material may be granular magnesium oxide.
  • Certain embodiments of stainless steels of the present invention were prepared and evaluated for resistance to corrosion in high temperature, corrosive environments. Two heats were melted with a target composition including, by weight, 19 to 23% chromium and 30 to 35% nickel. The first alloy had a target molybdenum concentration of 2%, and the second alloy had a target molybdenum concentration of 4%.
  • the actual compositions of the heats of the invention are shown in Table 1 as Sample 1 and Sample 2. Sample 1 contained 1.81% molybdenum and Sample 2 contained 3.54% molybdenum.
  • the alloy Samples 1 and 2 were prepared by a conventional method, specifically, by vacuum melting the alloy components in concentrations to approximate the target specification.
  • the formed ingots were then ground and hot rolled at approximately 2000° F. (1093° C.) to about 0.1 inches thick by 7 inches wide.
  • the resulting plate was grit blasted and descaled in an acid.
  • the plate was then cold rolled to a thickness of 0.008 inches and annealed in inert gas.
  • the resulting plate was formed into both flat coupon and welded teardrop samples.
  • Type 332 is an austenitic stainless steel characterized by a composition similar to that of Samples 1 and 2, but includes no deliberately added molybdenum.
  • Type 332 is, generally, a nickel and chromium stainless steel designed to resist oxidation and carburization at elevated temperatures. The analysis of the Type 332 sample tested is shown in Table 1.
  • Type 332 typically is characterized as an alloy comprising approximately 32 weight percent nickel and approximately 20 weight percent chromium. Type 332 was chosen for comparison purposes to determine the improvement offered by the addition of molybdenum in Samples 1 and 2 to the corrosion resistance in hot salt corrosion testing.
  • AISI Type 316Ti (UNS Designation S31635) (Sample 4) and AL 625 (UNS Designation N06625) (Sample 5). These two alloys are currently employed in flexible connectors for automotive exhaust systems because they are formable and resist intermediate temperature oxidation, general corrosion, and chloride stress corrosion cracking, particularly in the presence of high levels of road contaminants such as deicing salts.
  • the composition of Samples 4 and 5 are shown in Table 1.
  • AISI Type 316Ti is a low cost alloy presently used in low temperature automotive exhaust system flexible connector applications.
  • AL 625 is a higher cost material which presently finds broad application, including use as automotive exhaust system flexible connectors subjected to temperatures in excess of 1500° F. (816° C.).
  • a test was devised to examine the elevated temperature corrosion and oxidation resistance of the above samples in the presence of deposited corrosive solids. Special corrosion tests have been developed to simulate these high temperature corrosive environments. Currently, most testing of alloy resistance to corrosion from salt at elevated temperatures can be categorized as a “cup” test or a “dip” test.
  • cup test a sample of alloy is placed in a cup, generally of Swift or Erichsen geometry. The cup is then filled with a known volume of aqueous test solution having known salt concentration. The water in the cup is evaporated in an oven, leaving a salt coating on the sample. The sample is then exposed to elevated temperature under either cyclic or isothermal conditions and the sample's resistance to salt corrosion is assessed.
  • dip test a sample, either flat or in a U-bend configuration, is dipped in an aqueous solution having known salt concentration. The water is evaporated in an oven, leaving a coating of salt on the sample. The sample may then be assessed for resistance to salt corrosion.
  • the samples may be exposed to at least one 72-hour thermal cycle at an elevated temperature in a muffle furnace in still lab air or any other environmental conditions as desired. Preferably, a dedicated test furnace and labware should be used for this test in order to avoid cross-contamination from other test materials. After exposure, the samples and any collected non-adherent corrosion products are independently weighed. The results are reported as a specific weight change relative to the original (uncoated) specimen weight as previously described.
  • the typical exposure cycle was 72 hours at the elevated temperature in still lab air. After exposure the specimens were weighed. Any non-adherent corrosion products were collected and weighed separately. Any calculated weight gains or losses of the samples are due to the reaction of metal species with the atmosphere and any remaining salt from the coating. The amount of applied salt is generally much less than the weight change due to interaction with the environment, and as such can generally be discounted.
  • the coated specimens were exposed in the automated thermogravimetric cyclic oxidation laboratory setup. Every 24 hours the salt coating on each sample was removed by evaporation and the samples were then weighed so as to determine weight loss or gain caused by exposure to the environment. After weighing, the salt coatings were reapplied and the test was continued.
  • Table 2 summarizes the tests carried out on each of Samples 1 through 5.
  • TABLE 2 Test specimen stock identification matrix Grade Coupon testing Teardrop testing Sample 1 Present Invention — — Sample 2 Present Invention 0.008′′ thick 0.061′′ thick Sample 3 T-332 0.008′′ thick 0.058′′ thick Sample 4 T-316Ti 0.008′′ thick 0.062′′ thick Sample 5 AL625 0.008′′ thick 0.059′′ thick
  • FIG. 1 is a graph of weight change data comparing the results of hot salt corrosion testing of flat coupon samples of an alloy of the present invention (Sample 2) and prior art alloys coated with a 0.0, 0.5 and 0.10 mg/cm 2 salt layer and exposed for 72 hours to 1200° F. (649° C.).
  • the change in weight was determined by subtracting the initial weight of the sample by the final weight of the sample and, then, dividing this result by the initial surface area of the flat coupon sample.
  • the higher cost AL625 superalloy, Sample 5 exhibited a weight gain of approximately 1.7 mg/cm 2 under these test conditions. This weight gain is consistent with the formation of the protective layer of metal oxides on the surface of the alloy and minimal spalling of this protective layer.
  • the alloy of the present invention, Sample 2 exhibited almost no weight change under the test conditions.
  • the presence of about 4 weight percent molybdenum in Sample 2 increased the hot salt corrosion resistance of the alloy of the invention relative to the prior art T-332 alloy, Sample 3.
  • Sample 3 showed almost no weight change for the sample without a salt coating or with a coating of 0.05 mg/cm 2 . However, when exposed to a salt concentration of 0.10 mg/cm 2 , Sample 3 showed a degradation of the protective oxidation layer and a weight loss of greater than 1.5 mg/cm 2 .
  • the alloy of the present invention displayed a strong resistance to hot salt oxidation corrosion in this testing.
  • the molybdenum concentration in Sample 2 increased the corrosion resistance of the alloy over the corrosion resistance of the T332 alloy, Sample 3.
  • FIGS. 3 and 4 are graphs of the weight change data comparing the results of hot salt corrosion testing of welded teardrop samples of an alloy of the present invention (Sample 2) and prior art alloys coated with a nominal 0.10 mg/cm 2 salt layer and exposed to 1200° F. (649° C.) and 1500° F. (816° C.), respectively.
  • sample 2 an alloy of the present invention
  • prior art alloys coated with a nominal 0.10 mg/cm 2 salt layer and exposed to 1200° F. (649° C.) and 1500° F. (816° C.), respectively.
  • T316Ti again performed very poorly and proved to be an unacceptable alloy for elevated temperature corrosive environments. All other tested samples were substantially equivalent in performance as shown in both FIGS.
  • the tested alloy of the present invention displayed the greatest resistance to corrosion under these conditions with less than 1% weight loss and no additional weight change after approximately the first 30 hours of the test. This compares favorably with the performance of the higher performance prior art alloy AL625, Sample 5, which lost approximately 3% of its initial weight over the length of testing at 1500° F. (816° C.).
  • the tested alloy of the present invention better resisted hot salt oxidation compared with the other tested alloys.
  • Weight change information alone is generally an incomplete parameter for measuring the total effect of degradation in a highly aggressive environment. Attack in highly aggressive environments, such as in hot salt oxidation corrosion, is often irregular in nature and can compromise a significantly larger portion of the cross-section of an alloy component than would appear to be affected from analysis of weight change data alone. Therefore, metal loss (in terms of percentage of remaining cross-section) was measured in accordance with ASTM-G54 Standard Practice for Simple Static Oxidation Testing.
  • FIG. 5 illustrates the definitions of the parameters derived from this analysis.
  • Test Sample 30 has an initial thickness, T o , shown as distance 32 in FIG. 5.
  • the percentage of metal remaining is determined by dividing the thickness of the test sample after exposure to the corrosion testing, T ml , shown as distance 34 , by the initial thickness, 32 .
  • the percentage of unaffected metal is determined by dividing the thickness of the test sample showing no signs of corrosion, T m , shown as distance 36 in FIG. 4, by the initial thickness, 32 .
  • the alloy of the present invention showed the greatest percentage of unaffected area remaining after testing at both temperatures. This result indicates that the molybdenum retards the degradation and separation of the protective oxidation layer. The remaining cross-section and the percentage of unaffected area remaining after testing are approximately equal, about 90%. This indicates that hot salt corrosion of the alloys of the present invention is uniform across the surface of the test coupon and that premature failure should not occur due to localized failure. Conversely, this type of localized corrosion was exhibited by the prior art T-332 alloy, Sample 3. The analysis of Sample 3 indicated slight pitting, a potential for localized failure.
  • Austenitic stainless steels can be subject to sensitization when exposed to high temperatures.
  • sensitization is the intergranular precipitation of chromium carbides in austenitic stainless steel when the steel is exposed to temperatures in the approximate range of 800-1500° F. (427-816° C.).
  • a result of sensitization is that regions of the affected grains are depleted in chromium content, promoting susceptibility to intergranular corrosion in the presence of aqueous chlorides.
  • the present inventor prepared and tested five 50 lb. VIM heats having the chemical compositions shown in Table 3.
  • Table 3 identifies the heats as Heats 6-10 so as to distinguish them from Samples 1-5 in above Example 1.
  • the heats included varying additions of the carbide-forming elements titanium and niobium.
  • Heat 6 was formulated with an aim of zero titanium and zero niobium, and was found to include residuals levels of 0.002% titanium and 0.003% niobium.
  • Heat 7 was formulated as a titanium-stabilized heat with an aim of 0.3% titanium and zero niobium, and was found to include 0.320% titanium and 0.003% niobium.
  • Heat 7 represented an alloy similar in composition to Sample 2 in Example 1 above.
  • Heats 8-10 were formulated to include varying levels of addition of niobium and an aim of zero titanium, and were found to include 0.24-0.46% niobium and a residuals level of 0.002% titanium. Accordingly, the susceptibility to sensitization of Heat 6, which was substantially free of both titanium and niobium, and Heat 7, which was titanium-stabilized and substantially free of niobium, were compared with that of Heats 8-10, which included significant niobium and were substantially free of titanium.
  • each of the five heats was rolled to 0.075 inch thickness and solution annealed at 2050° F. (1121° C.) for 2 minutes time-at-temperature. Samples were sheared from each of the annealed finished panels and tested for sensitization according to the ASTM A262 (Practice A) test procedure, as revised in 2002.
  • ASTM A262 (Practice A) test procedure involves deliberately exposing samples to a sensitizing heat treatment (1 hour at a 1200° F. (649° C.) furnace temperature), and then mounting, polishing and etching the samples to reveal the microstructure of each sample. The samples are then compared to reference micrographs, and each sample's revealed microstructure is classified as being in one of the following three categories:
  • FIGS. 8 and 9 Representative micrographs of the observed microstructures of the samples from Heat 6 and Heat 7 are shown in FIGS. 8 and 9, respectively.
  • FIGS. 11 - 12 are representative micrographs of the observed structures of the samples from Heats 8 (lowest level of intentional niobium addition), 9, and 10 (highest level of intentional niobium addition.
  • the micrographs of FIGS. 10 - 12 appear essentially the same despite significant variation in the niobium content.
  • TABLE 4 Sensitization test results Heat 6 Heat 7 Heat 8 Heat 9 Heat 10 Observed Ditch Mixed, biased Step Step Step Step Structure to ditch
  • the Heat 7 sample exhibited more ditching of grain boundaries than not, indicating severe but not total sensitization.
  • an unexpected and surprising result of the tests is that by modifying the composition of Heat 7 to substitute an addition of niobium for all or substantially all of the titanium in Heat 7, the resulting alloys, embodied in Heats 8-10, were not subject to sensitization at a level observable in the tests.
  • niobium more effectively prevents sensitization than titanium in austenitic stainless steels of the type tested.
  • the addition of too high a level of niobium may result in over-stabilized material, wherein the excess stabilizing element produces inclusions that may detrimentally affect, for example, corrosion, mechanical properties, fatigue life, surface finish, and formability.
  • the addition of too little niobium may produce an under-stabilized material. It is believed that providing at least 0.25% and up to 0.6% niobium in, for example, an alloy having the general composition of Sample 2 in Example 1, will significantly reduce sensitization without significantly impairing other important properties of the alloy.
  • alloys of the present invention including 0.25-0.6% niobium can tolerate the presence of titanium up to 0.03% and exhibit improved sensitization properties. It also appears from the sensitization test results that a carbon-to-niobium ratio of about 1:10 provides sufficient stabilization to significantly inhibit sensitization.
  • the improved sensitization performance of Heats 8-10 should manifest itself in the form of improved corrosion resistance at high temperatures in the presence of aqueous chlorides.
  • An additional advantage of substituting niobium for some or all titanium is that there may be no need for a stabilizing anneal (an intermediate temperature heat treatment designed to pre-form stabilizing carbides), thereby allowing standard solution or mill-annealed material to be used without the danger of sensitization during service.
  • one aspect of the present invention is directed to an austenitic stainless steel comprising, by weight, 19% to 23% chromium, 30% to 35% nickel, 1% to 6% molybdenum, 0 to 0.03% titanium, 0.15% to 0.6% aluminum, up to 0.1% carbon, 1% to 1.5% manganese, 0 to less than 0.8% silicon, 0.25% to 0.6% niobium, and iron.
  • an austenitic stainless steel comprising, by weight, 19% to 23% chromium, 30% to 35% nickel, 1% to 6% molybdenum, 0 to 0.03% titanium, 0.15% to 0.6% aluminum, up to 0.1% carbon, 1% to 1.5% manganese, 0 to less than 0.8% silicon, 0.25% to 0.6% niobium, and iron.
  • such alloy is referred to hereinafter as the “niobium-containing stainless steel of the present invention” or, more simply, as the “niobium-containing stainless steel”.
  • the niobium-containing stainless steel of the present invention includes 0.3% to 0.5% niobium. It is believed that a niobium content within this range provides a further cushion against the possibility of under-and over-stabilization, while still providing improved sensitization properties.
  • the niobium-containing stainless steel of the present invention includes 19% to 21.5% chromium, and may include about 21% chromium.
  • Increasing molybdenum content enhances resistance to corrosion and, in particular, localized corrosion such as pitting and crevice corrosion.
  • the addition of molybdenum is generally more effective at improving pitting/crevice corrosion than the addition of chromium. Adding too high a level of molybdenum, however, results in sigma phase formation at temperatures greater than about 1000° F. (538° C.). Sigma phase reduces corrosion resistance and can make the alloy brittle at room temperature.
  • molybdenum is relatively expensive. Thus, in general, the level of molybdenum should be minimized while still providing the desired level of corrosion resistance.
  • certain embodiments of the niobium-containing stainless steel of the present invention may include 2% to 4% molybdenum, while other embodiments include 1% to 2.7% molybdenum.
  • the stainless steel includes about 2.5% molybdenum.
  • titanium When present at high levels, titanium causes surface defects. Titanium also forms inclusions in the presence of carbon and nitrogen, which adversely affects formability and fatigue resistance. Accordingly, in certain embodiments, the titanium content of the niobium-containing stainless steel of the present invention is restricted to the range of 0 to 0.01%, while in other embodiments is restricted to 0 to 0.005%.
  • Carbon content dictates the amount of carbides that will form when carbon solubility is exceeded.
  • the addition of carbon beyond the solubility limit is generally accompanied by increasing levels of stabilizing elements, such as titanium and niobium, so as to form an excess of carbides, which enhance high temperature creep strength.
  • stabilizing elements such as titanium and niobium
  • Such higher carbon additions can adversely affect the ability to roll to thin gauge, harm formability, and reduce fatigue strength.
  • certain embodiments of the niobium-containing stainless steel include no more than 0.03% carbon. Other embodiments include no more than 0.025% carbon.
  • Certain embodiments of the niobium-containing stainless steel also may include one or both of 0.15% to 0.4% aluminum, and up to 0.4% silicon.
  • the niobium-containing stainless steel includes one or more of about 0.30% aluminum, about 0.020% carbon, and about 0.30% silicon.
  • the niobium-containing stainless steel may include up to 0.75% copper, while certain embodiments of the steel may include up to 0.4% copper. In one form, the niobium-containing stainless steel includes about 0.3% copper.
  • Sulfur content preferably is minimized to avoid adversely affecting hot workability.
  • Phosphorus is an impurity that can adversely affect properties at too high a level. Accordingly, in certain forms, the niobium-containing stainless steel is limited to no greater than 0.05% phosphorus and/or no greater than 0.02% sulfur.
  • the niobium-containing stainless steel includes no more than 0.1% nitrogen, in certain other embodiments includes no more than 0.025% nitrogen, and in one form includes about 0.020% nitrogen.
  • an additional aspect of the present invention is directed to an austenitic stainless steel comprising, by weight, 19% to 21.5% chromium, 30% to 35% nickel, 1% to 2.7% molybdenum, 0 to 0.03% titanium, 0.15% to 0.4% aluminum, up to 0.025% carbon, 1% to 1.5% manganese, 0 to less than 0.8% silicon, 0 to 0.75% copper, 0.25% to 0.6% niobium, and iron.
  • the niobium-containing stainless steel includes, by weight, 21.5% chromium, 34.5% nickel, 2.5% molybdenum, 0.02% carbon, 1.2% manganese, no greater than 0.03% titanium, 0.5% niobium, up to 0.05% phosphorus, up to 0.02% sulfur, 0.30% silicon, 0.30% aluminum, 0.30% copper, 0.020% nitrogen, iron and incidental impurities.
  • a further aspect of the present invention is directed to an austenitic stainless steel including molybdenum and niobium and consisting essentially of, by weight, 19% to 23% chromium, 30% to 35% nickel, 1% to 6% molybdenum, 0 to 0.03% titanium, 0.15% to 0.6% aluminum, up to 0.1% carbon, 1% to 1.5% manganese, 0 to less than 0.8% silicon, 0.25% to 0.6% niobium, 0 to 0.75% copper, up to 0.05% phosphorus, up to 0.02% sulfur; up to 0.1% nitrogen, iron and incidental impurities.
  • Incidental impurities may include, for example, residual levels of impurities derived from scrap and other materials from which the alloys are produced.
  • another form of the present invention is directed to an austenitic stainless steel including molybdenum and niobium and consisting essentially of, by weight, 19% to 21.5% chromium, 30 to 35% nickel, 1% to 2.7% molybdenum, 0 up to 0.03% titanium, 0.15% to 0.4% aluminum, up to 0.025% carbon, 1 % to 1.5% manganese, 0 to less than 0.8% silicon, 0.25% to 0.6% niobium, up to 0.05% phosphorus, up to 0.02% sulfur, up to 0.1% nitrogen, iron and incidental impurities.
  • the present invention also encompasses articles of manufacture made wholly or partially from austenitic stainless steels as set forth in the present disclosure, and further encompasses methods of making such articles.
  • articles of manufacture examples include automobiles, automotive exhaust system components (such as , for example, automotive exhaust system flexible connectors), heating element sheaths, and gaskets.
  • automotive exhaust system components such as , for example, automotive exhaust system flexible connectors
  • heating element sheaths and gaskets.
  • the steel When producing automotive exhaust system flexible connectors from the niobium-containing stainless steel, the steel may be made by electric furnace/AOD melting, casting, hot rolling, and then multi-stage rolling on a cluster mill to light gauge.
  • the light gauge material may be bright annealed and slit to a relatively narrow strip having a thickness of, for example, 0.006-0.010 inch.
  • the continuous coil of material is welded into a tube on an automated tube mill, and then hydroformed into a corrugated flexible connector bellows. This requires that the material have a consistent edge, a relatively clean and stabilized microstructure free of gross defects, a surface free of scale, and high intrinsic ductility and fracture toughness.
  • Those having ordinary skill will be familiar with suitable methods of processing material for use as automotive exhaust system flexible connectors. Accordingly, further description of such methods is considered unnecessary.

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US10/360,961 US20040156737A1 (en) 2003-02-06 2003-02-06 Austenitic stainless steels including molybdenum
DE602004010368T DE602004010368T2 (de) 2003-02-06 2004-02-03 Austenitischer rostfreier stahl mit molybdenum
ES04707747T ES2297377T3 (es) 2003-02-06 2004-02-03 Aceros inoxidables austeniticos que contienen molibdeno.
EP04707747A EP1592820B1 (en) 2003-02-06 2004-02-03 Austenitic stainless steels including molybdenum
JP2006503284A JP4996243B2 (ja) 2003-02-06 2004-02-03 モリブデンを含むオーステナイト系ステンレス鋼
CNA2004800035753A CN1748042A (zh) 2003-02-06 2004-02-03 含钼的奥氏体不锈钢
KR1020177006044A KR102042324B1 (ko) 2003-02-06 2004-02-03 몰리브덴을 함유하는 오스테나이트계 스테인레스 강
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CNA2008101463202A CN101407890A (zh) 2003-02-06 2004-02-03 含钼的奥氏体不锈钢
CA2513897A CA2513897C (en) 2003-02-06 2004-02-03 Austenitic stainless steels including molybdenum
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