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WO2011029165A1 - Alliages à haute résistance à la corrosion trouvant une application dans des soupapes de moteurs - Google Patents

Alliages à haute résistance à la corrosion trouvant une application dans des soupapes de moteurs Download PDF

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Publication number
WO2011029165A1
WO2011029165A1 PCT/BR2009/000294 BR2009000294W WO2011029165A1 WO 2011029165 A1 WO2011029165 A1 WO 2011029165A1 BR 2009000294 W BR2009000294 W BR 2009000294W WO 2011029165 A1 WO2011029165 A1 WO 2011029165A1
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WO
WIPO (PCT)
Prior art keywords
alloys
mass
alloy
internal combustion
combustion engine
Prior art date
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Ceased
Application number
PCT/BR2009/000294
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English (en)
Portuguese (pt)
Inventor
Celso Antonio Barbosa
David Delagostini Jarreta
Alexandre Sokolowski
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Villares Metals SA
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Villares Metals SA
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Filing date
Publication date
Application filed by Villares Metals SA filed Critical Villares Metals SA
Priority to PCT/BR2009/000294 priority Critical patent/WO2011029165A1/fr
Publication of WO2011029165A1 publication Critical patent/WO2011029165A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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

Definitions

  • the present invention deals with a precipitation hardened Fe-Ni-Cr superalloy for application to internal combustion engine valves, having as main characteristics the high heat resistance, the precipitation of N3 (AI, Ti, Nb) and carbides of niobium and titanium in their microstructure, and superior oxidation resistance over state-of-the-art alloys.
  • the alloy design based on its microstructural aspects, also allows the alloy of the present invention to have properties equivalent to or superior to the high nickel alloys employed in internal combustion engine valves, associated with the significant reduction in alloy cost due to lower nickel content.
  • the alloy of the present invention is intended for the manufacture of valves, which application requires of the alloy a need for various properties, namely: high temperature oxidation resistance and heat resistance, given the high temperatures involved in the application.
  • High performance is an industry trend, such as exhaust valves, which are parts exposed to the highest temperatures and high mechanical stresses in an internal combustion engine. These requests High temperatures require the use of nickel-based superalloys, which have high costs.
  • NCF 751 alloy which has a very high cost due to its high nickel content above 70%. In this sense, lower nickel alloys with properties of hot strength, corrosion resistance and microstructural stability over long periods in temperature have been developed.
  • prior art alloy NCF3015 JIS3015D - US Patent 5,660,938) and patent alloy 5,951,789.
  • Oxidation resistance at elevated temperatures is the property to be evaluated for corrosion, with reference to the good performance of NCF 751.
  • NCF 751 alloy is the most important material to be replaced.
  • the alloys of the present invention meet all these needs.
  • the properties of Fe-Ni-Cr alloys used in exhaust valves are closely related to the presence of intermetallic phases, alloying elements and carbides in their microstructures.
  • Intermetallic phases are very important for high temperature resistance.
  • a composition that gives the material the necessary corrosion resistance in the medium of use is very important.
  • the performance of alloying elements in the formation of these phases has been carefully analyzed and modified in relation to the traditional concept.
  • the present invention utilizes the use of niobium in relatively high amounts (higher than prior art alloys) as an alloying element, mainly in the form of fine intermetallic precipitate.
  • Chromium is responsible for the formation of the chromium oxide passivating film on the surface of the material, which prevents the progression of the corrosive process.
  • Aluminum is also an intermetallic former formed by niobium, Ni 3 (AI, Nb), improving the heat resistance of the material. In addition, aluminum acts to improve the hot oxidation resistance of the alloy.
  • the morphology of these precipitates is determined by the surface energy of the ⁇ / ⁇ ' interface and the elastic energy generated by the misalignment of the ⁇ and ⁇ ' lattices, being determined primarily by the lattice deformation. If this deformation is small, the morphology that will minimize surface energy and volume deformation energy will be spherical. However, if the lattice deformation is considerably large, the morphology of the precipitates will not be spherical but cubic. When the lattice mismatch is up to 0.02% the ⁇ ' precipitates are spherical, in the case of mismatch between 0.5 and 1.0% these precipitates are cubic, and above .25% assume platelet shape.
  • Niobium presents a lower precipitation kinetics of the ordered Ni 3 Nb phase than when compared to elements such as titanium and aluminum in the Ni 3 phases (Ti, AI).
  • high levels of niobium lead to precipitation of the ordered phase y " (N3Nb), similar to the ⁇ ' phase.
  • N3Nb ordered phase y "
  • niobium When added to the alloy at lower levels, niobium only increases the volume of gamma precipitates. line and the solubilization temperature of this phase, bringing its hardening effect to even higher temperatures.
  • alloy element compositions which, by weight percentage, consist of:
  • Maximum 1.0 copper preferably maximum 0.5 copper, typically maximum 0.1% copper.
  • Chromium is used to give the alloy resistance to corrosion and oxidation at high temperatures, so its content should be greater than 10% for exhaust valve superalloys. Content above 25% threatens the stability of the microstructure due to the tendency of formation of phases such as the sigma phase and alpha line ( ⁇ and ⁇ '), which deteriorate the ductility. On the other hand, contents above 16% by mass show a positive response to improved oxidation resistance at elevated temperatures. Thus, it was decided that the chromium content of the alloys would be between these limits, preferably between 16.0% and 22.0%, typically 18.6%. Titanium and niobium are carbide formers.
  • titanium and niobium contents should be added to the alloy of the present invention according to the relationship Nb + 2 Ti, which accounts for the atomic mass difference of the two elements, so for the desired effect on the heat resistance properties, the Nb + 2 ⁇ ratio should be greater than 3.0% and typically equal to 4.2%.
  • a wide range for the Nb element is between 0.9 to 4.0% (by mass), with an intermediate range of 1.2 to 3.5% (by mass) of Nb and a narrow range of 1.5 to 3.0% (by mass) of Nb, or an even narrower range of 1.8 to 2.5%.
  • Nb In addition to improving heat resistance, Nb also improves weldability of the ⁇ "phase precipitation hardened superalloys, and furthermore improves corrosion resistance in sulfating environments such as diesel engines.
  • Nb can be partially replaced by tantalum (Ta) on equiatomic bases.
  • Ta is also an intermetallic phase former with nickel and strongly stabilizes primary carbides, being equally beneficial for hot hardness and abrasion resistance.
  • the increase in the amount of niobium showed effect on the heat resistance properties.
  • the mechanism is not fully defined, in the alloys of the present invention the niobium content not combined with carbon must form different intermetallic than titanium intermetallic ps, probably of the two-line gamma type ( ⁇ "), very stable to coalescence and thus , effective in improving the properties of high temperature resistance.
  • niobium causes, for the same ratio content (Nb + 2 Ti), to decrease the total titanium percentage of the alloy.
  • Studies of the present invention have shown that such a decrease is also beneficial for improving oxidation resistance at elevated temperatures - a property also essential in high temperature working valves.
  • the ratio (Nb + 2 Ti) should therefore have a minimum content of 1.2% niobium, preferably niobium above 1.5%, with the ideal niobium content equal to or greater than greater than 1.8%.
  • the content of these elements cannot be excessively high, as it would promote the formation of coarse intermetals, impairing the mechanical properties of the alloy in terms of mechanical strength and ductility, as well as increasing the cost of the alloy.
  • the ratio value (Nb + 2 Ti) should be below 8.0%, preferably below 7.0%.
  • Carbon is added with the intention of combining with titanium and niobium to form carbides which precipitate on grain boundaries and improve creep alloy strength as they make it difficult to deformation mechanisms by "grain boundary slip".
  • the carbon content should preferably be above 0.03% and below 0.06, preferably 0.05%.
  • Aluminum is very important for gamma phase ( ⁇ ') precipitation, and therefore for high temperature resistance. Another extremely important function of aluminum in the alloy is to increase oxidation resistance at high temperatures by increasing the formation of Al 2 O 3 during heating. However, aluminum contents should be restricted as very high amounts of this element may lead to deterioration of resistance at high temperatures and hot workability due to the formation of nitrides and phases such as ⁇ and ⁇ during long heating times.
  • the aluminum content therefore, should be between 0.5% and 4.0%, preferably between 1.0% and 3.0%, typically equal to 2.0%.
  • Copper should be controlled at low levels because this element is deleterious for some properties, especially high temperature oxidation which is the great improvement obtained in the alloys of the present invention.
  • no nickel alloy or superalloy uses copper and once added this element cannot be removed by steelmaking processes. This means that the internal scrap, that is, the leftovers of the production process cannot be reused in the process of other alloys, significantly increasing the production cost or even making the production of the alloy unfeasible. Therefore, in the alloys of the present invention the copper content should be below 1.0%, preferably below 0.5% and typically below 0.1%.
  • US Patent 5,951,789 has a high copper content, which is its main disadvantage compared to the alloys of the present invention, for these reasons of hot oxidation and scrap contamination.
  • Residuals Other elements such as manganese, tungsten, molybdenum, sulfur, phosphorus and those normally obtained as normal residues. In the process of manufacturing steel or liquid nickel alloys, they should be understood as impurities, related to the steelmaking deoxidation processes or inherent to the manufacturing processes. Therefore, the manganese, tungsten and molybdenum content is limited to 5.0%, preferably below 2.0%, due to the destabilization of the relationship between the austenite and ferrite phases, as well as possible effects on the intermetallic phases present in the alloy. Phosphorus and sulfur segregate into grain boundaries and other interfaces and should therefore be below 0.20%, preferably below 0.05%, preferably maximum 0.005%.
  • the alloy as described may be produced by conventional or special processes such as melting in electric or vacuum furnaces, whether or not followed by remelting processes. Casting can be done in ingots by conventional casting or continuous casting, or even by other manufacturing processes involving liquid metal disaggregation and further aggregation, such as powder metallurgy and the spray forming or continuous casting process.
  • the end products can be obtained after hot or cold forming, end products being produced in the form of wire rod, blocks, bars, wires, plates, strips, or even can be products in the raw state of solidification.
  • Figure 1 compares the hot strength of alloys of the present invention (PI) to prior art alloys ET1 and ET2, from the strength limit of these alloys at various temperatures.
  • Figure 2 presents the results of the oxidation resistance test.
  • Alumina ceramic crucibles were used as sample holders during the test. The progress of the oxidation process at 800 ° C was evaluated for 400 hours when stabilization of the corrosion process could be observed. The test was performed so that all samples of all alloys involved had identical dimensions, so as to have identical contact surface.
  • EXAMPLE To define the alloy compositions of the present invention, various alloys were produced and compared to those of the prior art. Chemical compositions are shown in Table 1, hereinafter referred to as PI the alloys of the present invention and ET the alloys of the prior art; ET1 alloy corresponds to NCF 751 and ET2 alloy corresponds to NCF 3015 (US 5,660,938); The ratios: (Nb + 2 Ti) and (Ti / Al) in Table 1 are also quantified.
  • Table 1 shows the significant reduction of the nickel content of the alloy in the compositions of the present invention in relation to the ET1 alloy, generating significantly lower cost. The addition of different niobium contents in the alloys of the present invention and the aluminum and titanium contents is also observed.
  • Table 1 Chemical compositions of two prior art alloys (ET1 and ET2) and alloys of the present invention (PI1 to PI4). Percent by mass and balance in iron.
  • the alloys of the present invention show an important advantage - in achieving high mechanical and corrosion properties without the need for high copper contents.
  • copper is a major contaminant of nickel alloy scraps because copper cannot be removed by the scrap remelting process and thus leftovers of high copper materials cannot be used in the manufacture of alloys. which have a limitation on the maximum content of copper contained.
  • copper tends to be deleterious to the high temperature corrosion properties.
  • Ti / Al The differences between titanium and aluminum contents between the different alloys can be assessed by the ratio (Ti / Al), which is very important for the properties of hot oxidation resistance and conformability of the alloys. This ratio (Ti / Al) is also shown in Table 1.
  • Ingot melting was performed in a close procedure for the six alloys (ET1, ET2, PI1, PI2, PI3 and PI4) in a vacuum induction furnace, and casting was made in cast iron ingot molds, producing an ingot with about 55 kg. After solidification, the ingots were forged and rolled into 18 mm diameter round gauges. In addition to these alloys, the typical composition of US Patent 5,951,789 is also presented for comparison (called ET3).
  • Table 2 shows the hardness of ET1, ET2, P11, PI2,
  • Table 2 Response to heat treatment of prior art alloys (ET1, ET2 and ET3) and alloys of the present invention (PM, PI2, PI3 and PI4). Hardness results in HB after solubilization at 050 ° C and aging at 750 ° C for 1 hour and 4 hours.
  • the alloys of the present invention were also superior to ET1 alloy, as shown in Table 3 and Figure 2; It is observed that the higher the chromium and aluminum content and the lower the titanium content, the higher the oxidation resistance of the alloy, being the better resistance observed for the PI3 alloy. This occurs for two reasons. Firstly, because a higher chromium and aluminum content provides greater and faster formation of the chromium oxide or aluminum oxide passivating layer on the surface of the material. Second, by the effect of titanium on destabilizing the oxide layer formed on the surface of the ferro-nickel-chromium alloys and thus decreasing the oxidation resistance on the higher content alloys. For example, it is interesting to note that among the high chromium alloys (PM, PI2, PI3 and PI4), the one with the lowest titanium content (PI3) exhibits superior hot oxidation resistance under the test conditions.
  • Table 3 Mass gain (in mg / cm 2 ) after 100, 300 and 400 hours in air atmosphere (at 800 ° C). The lower the mass gain, the greater the oxidation resistance of the material.
  • the property of resistance to hot oxidation can also be evaluated as a function of the ratio (Ti / Al).
  • Figure 3 shows this analysis for the alloys of the present invention (PM to PI4) and prior art (ET1). From these results, it is clearly noted that the alloys of the present invention are in the optimum range of Ti / Al ratio for optimizing the hot oxidation resistance property, represented by the inverse mass gain (in mg / cm 2 ) after 400 hours at 800 ° C in atmosphere (air). Therefore, comparison of the state-of-the-art alloys with the alloys of the present invention showed that the introduction of higher chromium, niobium and aluminum contents, accompanied by the reduction of titanium contents promote improvement in the properties of hot strength, creep, resistance to oxidation and wear. A summary of such effects is shown in Table 4. PM, PI2, PI3 and PI4 alloys always show superiority to prior art alloys in terms of all observed properties. Highlighting the PI3 and PI4 alloys, which show the best results.
  • the alloys of the present invention in addition to the economic advantage of working with lower nickel content, also have better properties.
  • the alloys of the present invention have superior levels of properties at high temperature, thus being important improvements for industrial application in combustion engine valves or even other components employed in high temperature and corrosive environments. And furthermore, they can be produced without scrap contamination problems by employing low copper content.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

L'invention concerne des alliages de faible coût résistant aux sollicitations mécaniques associées à de hautes températures, résistant à la corrosion, présentant une haute aptitude au formage et répondant aux diverses sollicitations inhérentes aux conditions d'utilisation dans une soupape d'échappement ou d'admission pour moteurs à combustion interne. Ces alliages présentent, comme caractéristiques principales, une précipitation de Ni3Nb dans leur microstructure, laquelle comprend, en pourcentage en masse: entre 0,01 et 0,15% de C, jusqu'à 3,0% de Mn, jusqu'à 1% de Si, entre 18,6 et 25,0% de Cr, entre 25,0 et 49% de Ni, jusqu'à 0,50% de Mo, jusqu'à 0,50% de W, jusqu'à 0,50% de V, jusqu'à 0,5% de Cu, entre 1,0 et 3,0% d'Al, entre 0,5 et 2,5% de Ti, entre 1,0 et 6,0% de Nb, entre 0,001 et 0,02% de B, entre 0,001 et 0,1% de Zr et jusqu'à 2,0% de Co, à condition que (Ni + Co) ne dépasse pas 50,0% en masse et ne soit pas inférieur à 25% en masse, et que le rapport Al/Ti soit inférieur à 2,0, le reste se composant de fer et des impuretés inévitablement présentes dans le procédé de fabrication de l'alliage.
PCT/BR2009/000294 2009-09-09 2009-09-09 Alliages à haute résistance à la corrosion trouvant une application dans des soupapes de moteurs Ceased WO2011029165A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110465667A (zh) * 2019-09-25 2019-11-19 广西科技大学 一种涡轮增压器叶片及其制备方法
CN114752845A (zh) * 2021-01-08 2022-07-15 宝武特种冶金有限公司 一种节镍型高碳铁基高温合金及其制备方法
US11525172B1 (en) 2021-12-01 2022-12-13 L.E. Jones Company Nickel-niobium intermetallic alloy useful for valve seat inserts

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5660938A (en) * 1993-08-19 1997-08-26 Hitachi Metals, Ltd., Fe-Ni-Cr-base superalloy, engine valve and knitted mesh supporter for exhaust gas catalyzer
US20080008617A1 (en) * 2006-07-07 2008-01-10 Sawford Maria K Wear resistant high temperature alloy
US20090081074A1 (en) * 2007-06-07 2009-03-26 Celso Antonio Barbosa Wear resistant alloy for high temprature applications

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5660938A (en) * 1993-08-19 1997-08-26 Hitachi Metals, Ltd., Fe-Ni-Cr-base superalloy, engine valve and knitted mesh supporter for exhaust gas catalyzer
US20080008617A1 (en) * 2006-07-07 2008-01-10 Sawford Maria K Wear resistant high temperature alloy
US20090081074A1 (en) * 2007-06-07 2009-03-26 Celso Antonio Barbosa Wear resistant alloy for high temprature applications

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110465667A (zh) * 2019-09-25 2019-11-19 广西科技大学 一种涡轮增压器叶片及其制备方法
CN110465667B (zh) * 2019-09-25 2022-04-22 广西科技大学 一种涡轮增压器叶片及其制备方法
CN114752845A (zh) * 2021-01-08 2022-07-15 宝武特种冶金有限公司 一种节镍型高碳铁基高温合金及其制备方法
CN114752845B (zh) * 2021-01-08 2023-09-08 宝武特种冶金有限公司 一种节镍型高碳铁基高温合金及其制备方法
US11525172B1 (en) 2021-12-01 2022-12-13 L.E. Jones Company Nickel-niobium intermetallic alloy useful for valve seat inserts

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