US3817747A - Carburization resistant high temperature alloy - Google Patents

Carburization resistant high temperature alloy Download PDF

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Publication number
US3817747A
US3817747A US00242980A US24298072A US3817747A US 3817747 A US3817747 A US 3817747A US 00242980 A US00242980 A US 00242980A US 24298072 A US24298072 A US 24298072A US 3817747 A US3817747 A US 3817747A
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Prior art keywords
alloy
alloys
silicon
chromium
aluminum
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Expired - Lifetime
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US00242980A
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English (en)
Inventor
J Schultz
Carron R Mc
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Huntington Alloys Corp
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International Nickel Co Inc
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Publication date
Application filed by International Nickel Co Inc filed Critical International Nickel Co Inc
Priority to US00242980A priority Critical patent/US3817747A/en
Priority to GB1530973A priority patent/GB1361960A/en
Priority to ZA732229A priority patent/ZA732229B/xx
Priority to CA167,685A priority patent/CA998543A/en
Priority to IT49308/73A priority patent/IT980120B/it
Priority to DE19732317915 priority patent/DE2317915B2/de
Priority to ES413544A priority patent/ES413544A1/es
Priority to DD170064A priority patent/DD103267A5/xx
Priority to FR7312923A priority patent/FR2179932B1/fr
Priority to NL737304976A priority patent/NL150849B/xx
Priority to BE129899A priority patent/BE798078A/xx
Priority to AT322273A priority patent/AT320998B/de
Priority to IN858/CAL/73A priority patent/IN139040B/en
Priority to JP4051673A priority patent/JPS5632381B2/ja
Application granted granted Critical
Publication of US3817747A publication Critical patent/US3817747A/en
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/053—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 30% but less than 40%

Definitions

  • the present invention relates to heat resistant alloys having excellent high temperature carburization, oxidation (including cyclic oxidation) and sulfidation resistance.
  • Another object of the invention is to provide heat and corrosion resistant alloy products and articles, including 3,817,747 Patented June 18, I974 products and articles for use in ethylene pyrolysis furnace tubes.
  • the present invention is directed to an alloy containing (by weight) from about 0.05% to about 0.15% carbon, from about 28% to about 35% chromium, from about 2.5% to about 6.0% aluminum, from about 10% to about 22% iron, from about 0.05% to about 0.8% titanium, up to about 1% silicon, the sum of the aluminum plus silicon being at least 3%, and the balance essentially nickel.
  • an alloy containing (by weight) from about 0.05% to about 0.15% carbon, from about 28% to about 35% chromium, from about 2.5% to about 6.0% aluminum, from about 10% to about 22% iron, from about 0.05% to about 0.8% titanium, up to about 1% silicon, the sum of the aluminum plus silicon being at least 3%, and the balance essentially nickel.
  • the use of the expression "balance essentially” in referring to the nickel content of the alloys does not exclude the presence of other elements commonly present as incidental constituents and impurities.
  • preferred alloys contemplated herein contain (by weight) from about 0.06% to 0.1% carbon, from about 30% to 34% chromium, from about 2.8% to 3.5% aluminum, from about 14% to 22% iron, from about 0.3% to 0.6% titanium, from about 0.4% to 0.6% silicon and the balance essentially nickel. Even more preferred alloys contain (by weight) from about 0.06% to 0.08% carbon, from about 31% to about 33% chromium, from about 2.9% to about 3.3% aluminum, from about 14% to about 17% iron, from about 0.3% to about 0.5% titanium, from about 0.4% to about 0.6% silicon and the balance essentially nickel.
  • the chromium content specified above herein is correlated according to the following mathematical relation (expressed in weight percent) to enable production of high creep-rupture strengths characteristic of the alloy: 28 Cr 39-(1.5A1+Si+Ti)-O.25(Fe-l6).
  • Alloys of the invention are characterized by a two-phase microstructure consisting of a gamma (face-centered cubic matrix with precipiated chromium-rich alpha prime (body-centered cubic) phase within the grains and at the grain boundaries.
  • a two-phase microstructure consisting of a gamma (face-centered cubic matrix with precipiated chromium-rich alpha prime (body-centered cubic) phase within the grains and at the grain boundaries.
  • the solution-treatment produces a larger grain size and the aging treatment precipitates the alpha prime phase, usually as fine, well-distributed bodies which may appear rod-like.
  • the alpha prime phase markedly enhances the strength of the alloy, approximately doubling the room temperature tensile strength when the aging treatment is employed. If the alloy is to be used for applications up to about 1500 F., the aging treatment is required to precipitate the alpha prime phase. At applications above about 1500 F., the alpha prime phase will precipitate during exposure and increase the strength; thus, the aging treatment may be unnecessary.
  • nickel is controlled in the amount of at least about 40% to provide a stable face-centered cubic matrix and the chromium is correlated to the contents of aluminum, silicon, titanium and iron according to the following mathematical relation (expressed in weight percent):
  • Chromium contributes carburization, oxidation and sulfidation resistance but must be controlled according to the foregoing relation to enable production of high creeprupture strengths characteristic of the alloy. Chromium levels substantially greater than those defined by the relation cause an excess of the alpha prime phase to form which does not dissolve at the solution temperature. The excess alpha prime phase inhibits grain growth in the alloy and results in a smaller grain size and reduced creeprupture strength. Chromium levels lower than about 28% result in decreased carburization, oxidation and sulfidation resistance and in an increased tendency for heatatfected-zone cracking during welding. Alloys which consistently manifest the best combination of creep strength, corrosion resistance and weldability contain chromium in accordance with the above relation and within the range of about 31% to 33%.
  • Aluminum enhances the carburization, oxidation and sulfidation resistance of the alloy. To maintain the desired carburization resistance it is essential that the aluminum content be maintained above about 2.5%. Aluminum at high levels above about 5% adversely affects the workability of the alloy. When workability is not a factor in producing the alloy, aluminum contents may be as high as about 6%. The best combination of properties is obtained when aluminum is maintained in a range of about 2.9% to 3.3%.
  • Silicon up to about 1% enhances carburization, oxidation and sulfidation resistance without significantly decreasing creep-rupture strength to achieve the desired combination of properties it is preferred to incorporate silicon in the range of about 0.4% to 0.6%. Silicon above about 1% adversely affects weldability.
  • Silicon and aluminum within their respective ranges, may be varied to produce the desired carburization properties provided their sum be at least about 3% and most beneficially at least 3.3%.
  • Titanium is employed as a deoxidizer and denitrifier to enhance the hot workability of the alloy.
  • a range of 0.3% to 0.6% titanium is preferred for this purpose.
  • Other elements such as zirconium from about 0.05% to about 0.5% or 0.8%, boron up to about 0.1%, calcium up to about 0.05% and magnesium up to about 0.05%, could also be used singly or in combination for this purpose, in lieu of or together with the titanium.
  • Zirconium and/or boron are particularly beneficial in conferring enhanced tensile ductility at temperatures on the order of about 1400 F.
  • At least about 0.05% carbon is necessary for high temperature strength, but should not substantially exceed about 0.15% in the interest of weldability.
  • a range of 0.06% to 0.1% is preferred but more advantageously is from 0.06% to 0.08%.
  • Iron above about 22% causes weld cracking while percentages below about 10%, apart from other factors, unnecessarily increase cost. Iron in the range of 14% to 22% is preferred, but is more advantageously from about 14% to about 17%.
  • Sulfur and phosphorus for example, should be 4 maintained at levels consistent with good steel-making practice, levels less than about 0.030% and 0.045%, respectively.
  • Table I sets forth the compositions of Alloys 1 through 11 which are examples of alloys within the invention and Alloys A through D which are outside the invention.
  • the series of alloys was vacuum melted in an electric induction furnace.
  • the nickel, chromium and iron were charged into the furnace and heated to 2900 F.
  • one-half of the aluminum and one-half of the titanium contents were added to the melts.
  • the melts were held until all bubbling and agitation ceased and were then cooled to 2700 F., at which point the remainder of the aluminum and titanium was added along with the silicon and a high carbon-chrome addition alloy.
  • the melts were then heated to 2750 F.
  • the creep-rupture results set forth in Table II were obtained using standard testing procedures. The specimens were first creep-rupture tested followed by room temperature measurement of elongation and reduction of area.
  • the carburization tests set forth in Table III were run at 2012 F. in a flowing gas mixture of hydrogen containing 2 volume percent methane.
  • the specimens were supported in ceramic fixtures and then inserted into a preheated tube furnace which was being flushed with argon. Following the argon flush, the hydrogen-methane gas mixture was introduced at a velocity of 0.5 cm./sec. over the specimens. At the end of each test period, the furnace was again flushed with argon and the specimens were removed to cool in air. The specimens were then lightly descaled to remove the oxide formed as the specimens were taken from the furnace, and the weight change of the specimens was measured. Descaling of all the test specimens was done with an 5.8.
  • White precision abrasive cleaning unit using 50 micron alumina propelled by dry C0 was the penetration measurement was the depth of metal showing carbon penetration and was measured metallographically on a Leitz measuring microscope. All specimens were etched in modified Murakamis reagent prior to making the measurements. All the tests were run for a period of hours.
  • the oxidation tests set forth in Table III were run in flowing air containing a controlled 5 volume percent water vapor at 2012 F.
  • the air velocity over the specimens was 0.5 cm./sec.
  • the tests were cyclic in that the specimens were removed from the furnace every 100 hours, cooled to room temperature, weighed and returned to the furnace. A total of 10 cycles (total test time of 1,000 hours) was employed. Test specimens were descaled at the end of the test following the procedures described above for the carburization tests.
  • Alloys 1 and A in Table II clearly reflects the disastrous elfect on creeprupture strength caused by a chromium content substantially in excess of that defined by the above relation.
  • the microstructures of the two alloys are shown, respectively, in FIGS. 1 and 2 of the drawing.
  • Alloy 1 is characterized by a large grain size and uniform distribution of the alpha prime phase which appears as fine, well distributed, darker-etching particles in the gamma matrix.
  • Alloy A is seen to be characterized by a relatively smaller grain size and by a substantially greater proportion of the darker-etching alpha prime phase which itself occurs as considerably larger particles than was the case in FIG. 1. It is important to note that this reduction in creep-rupture strength (a factor of 10) is caused by a chromium content only 2.5% higher than the chromium content determined in accordance with the foregoing relationship.
  • Alloy 11 is, at best, a marginal alloy within the broadest limits of the invention. As can be seen from Table III, this alloy while strikingly surperior to the prior art Alloys C and D (also Alloy B) in terms of its ability to resist carburization, nonetheless behaved poorly, comparatively, speaking, relative to Alloys 1-10, the latter all having a total aluminum plus silicon content over 3.3%
  • the weldability of the alloy is demonstrated by tests conducted on Alloys 1 through 3. Plates of Alloy 1 Were surface ground, gas tungsten-arc welded for bead-on-plate and thermal shock tests and visually examined at 10X for evidence of weld and heat-alfected zone defects.
  • the bcad-on-plate test was conducted at 11 volts, 250 amperes, with one pass at a travel speed of 16 inches per minute (i'p.m.) and an argon flow of 25 cubic feet per hour (cf./h.). Each test was conducted using a non-consumable tungsten electrode and no filler material.
  • One-half inch thick plate (60 V bevel) of Alloys 2 and 3 were manually gas tungsten-arc butt welded using the parent metal composition as filler /s" diameter).
  • the weld was conducted at 16 volts, 230 amperes, with 9 passes at a travel speed of approximately 3 i.p.rn. and an argon flow of 25 cf./h.
  • These joints were radiographically inspected and showed no indication of weld cracking. They were also cut into one-half inch wide transverse slices, polished and etched with Lepitos reagent. Examination at 10X for weld and heat-affected zone defects showed satisfactory welds with relatively few cracks.
  • the alloys of the invention are especially useful in applications involving the processing of hydrocarbons and sulfidizing and oxidizing materials at high temperatures.
  • Alloys of the invention may be either wrought or cast and exemplary articles include ethylene pyrolysis furnace tubes, piping, valves, vessels and other equipment used in industrial chemical plants.
  • exemplary articles include ethylene pyrolysis furnace tubes, piping, valves, vessels and other equipment used in industrial chemical plants.
  • the silicon can beup to 1.5 or 2%.
  • a nickel-base heat resistant alloy affording high temperature carburization, oxidation, cyclic oxidation and sulfidation resistance consisting essentially of about 0.05% to about 0.15% carbon, from about 28% to about 35% chromium, in which the chromium content is correlated according to the formula from which about 2.5% to about 6% aluminum, up to 2% silicon, with the sum of the aluminum plus silicon being at least 3% and the silicon not exceeding about 1% in respect of wrought weldable alloys, from about 10% to about 22% iron, from about 0.05 to about 0.8% titanium, and the balance essentially nickel.
  • a nickel-base alloy in accordance with claim 1 containing about 0.06% to about 0.1% carbon, about 30% to about 34% chromium, about 2.8% to about 3.5% aluminium, about 14% to about 22% iron, about 0.3% to about 0.6% titanium, and about 0.4% to about 0.6% silicon, the aluminum plus silicon being at least about 3.3%.
  • a nickel-base heat resistant alloy affording high temperature carburization, oxidation, cyclic oxidation and sulfidation resistance consisting essentially of about 0.06% to about 0.08% carbon, from about 31% to about 33% chromium, from about 2.9% to about 3.3% aluminum, from about 14% to about 17% iron, from 0.3% to about 0.5% titanium, from about 0.4% to about 0.6% silicon and the balance essentially nickel.
  • a nickel-base heat resistant alloy affording high temperature carburization, oxidation, cyclic oxidation and sulfidation resistance consisting essentially of about 0.05% to about 0.15% carbon, from about 28% to about 35% chromium, in which the chromium content is correlated according to the formula 28 Cr 39 LSAH-SH-Ti) 0.25(Fe16),
  • alloy being further charatcerized by a two-phase microstructure consisting of a gamma matrix with precipitated chromiumrich alpha prime phase within the grains and at the grain boundaries.
  • a nickel-base alloy in accordance with claim 10 containing about 0.06% to about 0.1% carbon, about 30% to about 34% chromium, about 2.8% to about 3.5% aluminum, about 14% to about 22% iron, about 0.3% to about 0.6% titanium, and about 0.4% to about 0.6% silicon, the aluminum plus silicon being at least about 3.3%.
  • a method in accordance with claim 12 further comprising reheating said alloy for about one hour at a temperature of about 1800' F. and quenching.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
  • Heat Treatment Of Articles (AREA)
US00242980A 1972-04-11 1972-04-11 Carburization resistant high temperature alloy Expired - Lifetime US3817747A (en)

Priority Applications (14)

Application Number Priority Date Filing Date Title
US00242980A US3817747A (en) 1972-04-11 1972-04-11 Carburization resistant high temperature alloy
GB1530973A GB1361960A (en) 1972-04-11 1973-03-30 Nickel-base heat-resistant alloys
ZA732229A ZA732229B (en) 1972-04-11 1973-04-02 Nickel-base heat-resistant alloys
CA167,685A CA998543A (en) 1972-04-11 1973-04-02 Carburization resistant high temperature alloy
IT49308/73A IT980120B (it) 1972-04-11 1973-04-09 Leghe di cromo nickel resistenti al calore ed oggetti prodotti con esse
ES413544A ES413544A1 (es) 1972-04-11 1973-04-10 Un metodo para la fabricacion de un componente industrial resistente a severas condiciones termicas y quimicas.
DE19732317915 DE2317915B2 (de) 1972-04-11 1973-04-10 Verfahren zum herstellen eines nickel-chrom-eisen-werkstoffs
DD170064A DD103267A5 (ru) 1972-04-11 1973-04-10
FR7312923A FR2179932B1 (ru) 1972-04-11 1973-04-10
NL737304976A NL150849B (nl) 1972-04-11 1973-04-10 Werkwijze voor de bereiding van een nikkel-chroom-aluminiumlegering en voorwerp, vervaardigd uit een dergelijke legering.
BE129899A BE798078A (fr) 1972-04-11 1973-04-11 Alliages a base de nickel
AT322273A AT320998B (de) 1972-04-11 1973-04-11 Hitzebeständige Legierung auf Nickel-Basis
IN858/CAL/73A IN139040B (ru) 1972-04-11 1973-04-11
JP4051673A JPS5632381B2 (ru) 1972-04-11 1973-04-11

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US (1) US3817747A (ru)
JP (1) JPS5632381B2 (ru)
AT (1) AT320998B (ru)
BE (1) BE798078A (ru)
CA (1) CA998543A (ru)
DD (1) DD103267A5 (ru)
DE (1) DE2317915B2 (ru)
ES (1) ES413544A1 (ru)
FR (1) FR2179932B1 (ru)
GB (1) GB1361960A (ru)
IN (1) IN139040B (ru)
IT (1) IT980120B (ru)
NL (1) NL150849B (ru)
ZA (1) ZA732229B (ru)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3984239A (en) * 1975-04-07 1976-10-05 The International Nickel Company, Inc. Filler metal
US4033767A (en) * 1975-09-19 1977-07-05 Chas. S. Lewis & Co., Inc. Ductile corrosion resistant alloy
US4102225A (en) * 1976-11-17 1978-07-25 The International Nickel Company, Inc. Low chromium oxidation resistant austenitic stainless steel
US4388125A (en) * 1981-01-13 1983-06-14 The International Nickel Company, Inc. Carburization resistant high temperature alloy
US4743318A (en) * 1986-09-24 1988-05-10 Inco Alloys International, Inc. Carburization/oxidation resistant worked alloy
US4780276A (en) * 1986-07-30 1988-10-25 The Unites States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Castable hot corrosion resistant alloy
WO1989001985A1 (en) * 1987-08-28 1989-03-09 Chas. S. Lewis & Co., Inc. Air meltable castable corrosion resistant alloy
US4882125A (en) * 1988-04-22 1989-11-21 Inco Alloys International, Inc. Sulfidation/oxidation resistant alloys
US4929288A (en) * 1988-01-04 1990-05-29 Borges Robert J Corrosion and abrasion resistant alloy
US20220025504A1 (en) * 2014-03-28 2022-01-27 Kubota Corporation Cast product having alumina barrier layer

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4731221A (en) * 1985-05-06 1988-03-15 The United States Of America As Represented By The United States Department Of Energy Nickel aluminides and nickel-iron aluminides for use in oxidizing environments
JPS6331535A (ja) * 1986-07-23 1988-02-10 Jgc Corp 炭素析出抑止性含炭素化合物処理装置
JPH028336A (ja) * 1988-06-28 1990-01-11 Jgc Corp 炭素析出抵抗性二層管

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR698724A (fr) * 1929-10-11 1931-02-03 Commentry Sa Procédé de traitement thermique des alliages à haute teneur en nickel et en chrome
FR1251688A (fr) * 1960-03-18 1961-01-20 Thomson Houston Comp Francaise Alliages réfractaires
FR1267470A (fr) * 1960-09-13 1961-07-21 Alliages nickel, chrome, aluminium résistant à la chaleur

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3984239A (en) * 1975-04-07 1976-10-05 The International Nickel Company, Inc. Filler metal
US4033767A (en) * 1975-09-19 1977-07-05 Chas. S. Lewis & Co., Inc. Ductile corrosion resistant alloy
US4102225A (en) * 1976-11-17 1978-07-25 The International Nickel Company, Inc. Low chromium oxidation resistant austenitic stainless steel
US4388125A (en) * 1981-01-13 1983-06-14 The International Nickel Company, Inc. Carburization resistant high temperature alloy
US4780276A (en) * 1986-07-30 1988-10-25 The Unites States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Castable hot corrosion resistant alloy
US4743318A (en) * 1986-09-24 1988-05-10 Inco Alloys International, Inc. Carburization/oxidation resistant worked alloy
WO1989001985A1 (en) * 1987-08-28 1989-03-09 Chas. S. Lewis & Co., Inc. Air meltable castable corrosion resistant alloy
US4853183A (en) * 1987-08-28 1989-08-01 Chas S. Lewis & Co., Inc. Air meltable castable corrosion resistant alloy and its process thereof
US4929288A (en) * 1988-01-04 1990-05-29 Borges Robert J Corrosion and abrasion resistant alloy
US4882125A (en) * 1988-04-22 1989-11-21 Inco Alloys International, Inc. Sulfidation/oxidation resistant alloys
AU601938B2 (en) * 1988-04-22 1990-09-20 Inco Alloys International Inc. Sulfidation/oxidation resistant alloy
US20220025504A1 (en) * 2014-03-28 2022-01-27 Kubota Corporation Cast product having alumina barrier layer
US11674212B2 (en) * 2014-03-28 2023-06-13 Kubota Corporation Cast product having alumina barrier layer

Also Published As

Publication number Publication date
CA998543A (en) 1976-10-19
FR2179932A1 (ru) 1973-11-23
IN139040B (ru) 1976-05-01
IT980120B (it) 1974-09-30
FR2179932B1 (ru) 1979-01-12
GB1361960A (en) 1974-07-30
BE798078A (fr) 1973-10-11
DE2317915B2 (de) 1976-11-25
AT320998B (de) 1975-05-10
ES413544A1 (es) 1976-06-01
JPS5632381B2 (ru) 1981-07-27
NL150849B (nl) 1976-09-15
NL7304976A (ru) 1973-10-15
DE2317915A1 (de) 1973-10-18
JPS4916616A (ru) 1974-02-14
ZA732229B (en) 1974-01-30
DD103267A5 (ru) 1974-01-12

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