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EP0292061B1 - Corrosion-resistant alloy - Google Patents

Corrosion-resistant alloy Download PDF

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EP0292061B1
EP0292061B1 EP88200969A EP88200969A EP0292061B1 EP 0292061 B1 EP0292061 B1 EP 0292061B1 EP 88200969 A EP88200969 A EP 88200969A EP 88200969 A EP88200969 A EP 88200969A EP 0292061 B1 EP0292061 B1 EP 0292061B1
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alloy according
corrosion
structural components
alloy
making structural
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EP0292061A1 (en
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Manfred Dr. Rockel
Ernst Wallis
Michael Dr. Köhler
Ulrich Dr. Heubner
Rolf Kirchheiner
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VDM Nickel Technologie AG
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    • 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
    • C22C38/001—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
    • C22C38/18—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
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten

Definitions

  • the invention relates to a modified alloy according to material no. 1.4563 and its use.
  • This known alloy has the following composition:
  • This alloy was developed in order to be able to provide a material that is particularly corrosion-resistant to technical phosphoric acids.
  • the invention has for its object to further improve this known alloy in its corrosion properties without other properties being adversely affected.
  • this goal could be achieved by increasing the molybdenum content to 6 to 7% and also ensuring a nitrogen addition of 0.10 to 0.25%. Due to the increased molybdenum content, the resistance to pitting and crevice corrosion in chloride-containing media is significantly improved during the Nitrogen content stabilizes the austenitic structure and reduces its tendency to excrete TCP phases.
  • the nitrogen content is in the range 0.14 to 0.22%, preferably 0.16 to 0.20% or 0.18%.
  • Table 1 contains information on the chemical composition of 5 by 2 samples which have been subjected to the tests described below. Samples 11 and 12 are examples of the alloy according to the invention, while samples 21 and 22 relate to the starting alloy, which contains less molybdenum and no nitrogen. The table also shows 2 samples from 3 other test alloys. In the following, only the first digit of the sample number is used to identify the 5 different alloys.
  • Table 2 contains information on various properties of the 5 alloys tested for comparison.
  • the alloys are labeled 1 to 5.
  • Column 2 refers to the critical crevice corrosion temperature
  • column 3 to the critical pitting temperature, each in 6% FeCl3 solution.
  • Column 4 contains values for the Corrosion rates in technical phosphoric acid (H3PO4, 72%).
  • Column 5 shows the removal rates under conditions according to ASTM G 28, Practice B.
  • column 6 contains information on the sensitization time with regard to the resistance to intergranular corrosion , ranges being given in each case, because strong fluctuations must be expected.
  • the critical crevice corrosion and pitting temperatures are significantly higher in the alloy according to the invention than in the starting alloy. Temperatures are reached that have previously only been achieved with material 5, which is much higher alloyed.
  • the corrosion rates in technical phosphoric acid are in the range of the comparative alloy No. 2 designed for this purpose. The goal set here, namely to create a material in which the improvement of some properties is not at the expense of other properties.
  • the removal rate according to column 5 is smaller by more than a power of ten for the material according to the invention than for the comparison materials. This is particularly noteworthy because it has previously been assumed that molybdenum only improves the resistance of a material to corrosion in reducing acids. Apparently, the significant improvement now found in oxidizing acids is due to the combined effect of molybdenum and chromium.
  • the removal rates in monochloroacetic acid for three different materials are compared in FIG. 2, namely once for the base material and once for welded material.
  • the material 1 according to the invention performs better in all cases than the comparison materials 2 and 3.
  • test according to ASTM G 28, Practice A is used to examine materials for their resistance to intergranular corrosion. It is carried out in a boiling solution with 50% H2SO4 and 3.7% Fe2 (SO4) 3. Such conditions occur in practice, for example, when handling contaminated sulfuric acids.
  • the test according to ASTM G 28, Practice B, is used to determine the corrosion behavior of materials in strongly oxidizing acids containing metal ions.
  • a boiling solution with 23% H2SO4, 1.2% HCl, 1% FeCl3 and 1% CuCl2 is used. This simulates conditions such as those that occur in pickling plants.
  • Sour gas test tests have been developed to test the resistance to stress corrosion cracking under conditions such as can occur in deep boreholes when searching for natural gas and crude oil.
  • the material according to the invention showed no damage from stress corrosion cracking and no pitting corrosion.

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Abstract

Disclosed in an improvement in a known Ni-Cr-Fe alloy. The alloy of the invention contains 30 to 32% nickel; 26 to 28% chromium; 0.5 to 1.5% copper; 6 to 7% molybdenum; up to 2% manganese; up to 1.0% silicon; up to 0.2% aluminum; up to 0.03% carbon; 0.10 to 0.25% nitrogen; balance iron and usual impurities. The alloy of the invention has increased pitting corrosion potential and critical crevice corrosion and pitting corrosion temperatures whereas the resistance of the alloy to commercially pure phosphoric acid has not been decreased.

Description

Die Erfindung bezieht sich auf eine modifizierte Legierung gemäß Werkstoff Nr. 1.4563 sowie deren Verwendung.The invention relates to a modified alloy according to material no. 1.4563 and its use.

Diese bekannte Legierung weist folgende Zusammensetzung auf:

Figure imgb0001
This known alloy has the following composition:
Figure imgb0001

Diese Legierung ist entwickelt worden, um einen Werkstoff zur Verfügung stellen zu können, der insbesondere gegenüber technischer Phosphorsäuren korrosionsbeständig ist.This alloy was developed in order to be able to provide a material that is particularly corrosion-resistant to technical phosphoric acids.

Der Erfindung liegt die Aufgabe zugrunde, diese bekannte Legierung in ihren Korrosionseigenschaften noch weiter zu verbessern, ohne daß andere Eigenschaften negativ beeinflußt werden.The invention has for its object to further improve this known alloy in its corrosion properties without other properties being adversely affected.

Dieses Ziel konnte überraschenderweise durch die Merkude des Anspruchs 1 erreicht werden, indem man den Molybdängehalt auf 6 bis 7% anhebt und außerdem für einen Stickstoffzusatz von 0,10 bis 0,25% sorgt. Durch den erhöhten Molybdängehalt wird die Beständigkeit gegenüber Lochfraß- und Spaltkorrosion in chloridhaltigen Medien deutlich verbessert, während der Stickstoffgehalt das austenitische Gefüge stabilisiert und dessen Neigung zur Ausscheidung von TCP-Phasen herabsetzt.Surprisingly, this goal could be achieved by increasing the molybdenum content to 6 to 7% and also ensuring a nitrogen addition of 0.10 to 0.25%. Due to the increased molybdenum content, the resistance to pitting and crevice corrosion in chloride-containing media is significantly improved during the Nitrogen content stabilizes the austenitic structure and reduces its tendency to excrete TCP phases.

Besonders vorteilhafte Ergebnisse werden erzielt, wenn der Stockstoffgehalt im Bereich 0,14 bis 0,22% liegt, vorzugsweise bei 0,16 bis 0,20% bzw. bei 0,18%.Particularly advantageous results are achieved if the nitrogen content is in the range 0.14 to 0.22%, preferably 0.16 to 0.20% or 0.18%.

Die Legierung wird vorteilhafterweise verwendet als Werkstoff zur Herstellung von Bauteilen, die einer oder mehreren der folgenden Bedingungen genügen müssen:

  • a) In technischer Phosphorsäure mit einer Chloridionenkonzentration bis zu 1000 ppm soll die Abtragungsrate bei 100°C weniger als 0,20 mm/a betragen.
  • b) In wäßrigen neutralen Medien mit einer Chloridionenkonzentration in der Größenordnung von 20.000 ppm soll das Lochfraßpotential bei 75°C mindestens 1000 mVH und bei 90°C mindestens 800 mVH betragen.
  • c) In sauren Medien mit einer Chloridionenkonzentration von 50.000 ppm und mehr, wie z.B. in einer FeCl₃-Lösung, soll eine kritische Lochfraßtemperatur von mindestens 80°C und eine kritische Spaltkorrosionstemperatur von mindestens 50°C vorhanden sein.
  • d) Unter den Bedingungen gemäß ASTM G 28, Practice A, soll Beständigkeit gegen interkristalline Korrosion vorhanden sein.
  • e) Unter den Bedingungen gemäß ASTM G 28, Practice B, eine Abtragungsrate von weniger als 0,5 mm/a aufweisen müssen.
  • f) Unter den Bedingungen eines aggressiven Sauergas-Tests frei von Spannungsriß- und Lochfraßkorrosion sein müssen.
The alloy is advantageously used as a material for the production of components which must meet one or more of the following conditions:
  • a) In technical phosphoric acid with a chloride ion concentration up to 1000 ppm, the removal rate at 100 ° C should be less than 0.20 mm / a.
  • b) In aqueous neutral media with a chloride ion concentration in the order of 20,000 ppm, the pitting potential should be at least 1000 mV H at 75 ° C and at least 800 mV H at 90 ° C.
  • c) In acidic media with a chloride ion concentration of 50,000 ppm and more, such as in a FeCl₃ solution, a critical pitting temperature of at least 80 ° C and a critical crevice corrosion temperature of at least 50 ° C should be available.
  • d) Under the conditions of ASTM G 28, Practice A, resistance to intergranular corrosion should be present.
  • e) Under the conditions according to ASTM G 28, Practice B, an erosion rate of less than 0.5 mm / a.
  • f) Must be free of stress corrosion cracking and pitting corrosion under the conditions of an aggressive acid gas test.

Weitere Einzelheiten und Vorteile des Erfindungsgedankens werden anhand der nachfolgenden Tabellen und Diagramme näher erläutert.Further details and advantages of the inventive concept are explained in more detail with the aid of the tables and diagrams below.

Tabelle 1 enthält Angaben zu der chemischen Zusammensetzung von 5 mal 2 Proben, die den nachfolgend beschriebenen Prüfungen unterzogen worden sind. Die Proben 11 und 12 sind Beispiele der erfindungsgemäßen Legierung, während die Proben 21 und 22 sich auf die Ausgangslegierung beziehen, die weniger Molybdän und keinen Stickstoff enthält. Außerdem sind in der Tabelle je 2 Proben von 3 weiteren Versuchslegierungen aufgeführt. Im folgenden wird zur Kennzeichnung der 5 verschiedenen Legierungen jeweils nur die erste Ziffer der Probennummer benutzt.Table 1 contains information on the chemical composition of 5 by 2 samples which have been subjected to the tests described below. Samples 11 and 12 are examples of the alloy according to the invention, while samples 21 and 22 relate to the starting alloy, which contains less molybdenum and no nitrogen. The table also shows 2 samples from 3 other test alloys. In the following, only the first digit of the sample number is used to identify the 5 different alloys.

In Fig. 1 sind die gegen die Normal-Wasserstoff-Elektrode gemessenen Lochfraßpotentiale von 4 untersuchten Legierungen über der Prüftemperatur aufgetragen. Mit einem Blick ist zu erkennen, daß die erfindungsgemäße Legierung allen anderen Legierungen im Temperaturbereich oberhalb von 60°C deutlich überlegen ist. Die Werte wurden in belüftetem künstlichen Meerwasser potentiostatisch bestimmt. Außerdem ist unten noch das Redoxpotential (R) des Prüfmediums eingetragen.1 shows the pitting potentials measured against the normal hydrogen electrode of 4 alloys tested above the test temperature. It can be seen at a glance that the alloy according to the invention is clearly superior to all other alloys in the temperature range above 60 ° C. The values were determined potentiostatically in aerated artificial sea water. The redox potential (R) of the test medium is also entered below.

Tabelle 2 enthält Angaben zu verschiedenen Eigenschaften der 5 vergleichend untersuchten Legierungen. In Spalte 1 sind die Legierungen mit 1 bis 5 bezeichnet. Spalte 2 bezieht sich auf die kritische Spaltkorrosionstemperatur, Spalte 3 auf die kritische Lochfraßtemperatur, jeweils in 6%iger FeCl₃-Lösung. Spalte 4 enthält Werte für die Korrosionsraten in technischer Phosphorsäure (H₃PO₄, 72%). In Spalte 5 sind die Abtragungsraten bei Bedingungen gemäß ASTM G 28, Practice B, angegeben. In Spalte 6 sind schließlich Angaben für die Sensibilisierungszeit im Hinblick auf die Beständigkeit gegen interkristalline Korrosion aufgeführt, wobei jeweils Bereiche angegeben sind, weil insoweit mit starken Schwankungen gerechnet werden muß.Table 2 contains information on various properties of the 5 alloys tested for comparison. In column 1 the alloys are labeled 1 to 5. Column 2 refers to the critical crevice corrosion temperature, column 3 to the critical pitting temperature, each in 6% FeCl₃ solution. Column 4 contains values for the Corrosion rates in technical phosphoric acid (H₃PO₄, 72%). Column 5 shows the removal rates under conditions according to ASTM G 28, Practice B. Finally, column 6 contains information on the sensitization time with regard to the resistance to intergranular corrosion , ranges being given in each case, because strong fluctuations must be expected.

Die kritischen Spaltkorrosions- und Lochfraßtemperaturen liegen bei der erfindungsgemäßen Legierung deutlich höher als bei der Ausgangslegierung. Es werden Temperaturen erreicht, die bisher nur von dem wesentlich höher legierten Werkstoff Nr. 5 erreicht worden sind. Die Korrosionsraten in technischer Phosphorsäure liegen im Bereich der für diese Zwecke konzipierten Vergleichslegierung Nr. 2. Damit ist auch hier das gesteckte Ziel erreicht, nämlich einen Werkstoff zu schaffen, bei dem die Verbesserung einiger Eigenschaften nicht zu Lasten anderer Eigenschaften geht. Die Abtragungsrate gemäß Spalte 5 ist bei dem erfindungsgemäßen Werkstoff um mehr als eine Zehnerpotenz kleiner als bei den Vergleichswerkstoffen. Dies ist besonders bemerkenswert, weil man bisher annahm, daß Molybdän nur die Beständigkeit eines Werkstoffs gegen Korrosion in reduzierenden Säuren verbessert. Offenbar ist die jetzt festgestellte deutliche Verbesserung auch in oxidierenden Säuren auf die kombinierte Wirkung des Molybdäns und des Chrom zurückzuführen.The critical crevice corrosion and pitting temperatures are significantly higher in the alloy according to the invention than in the starting alloy. Temperatures are reached that have previously only been achieved with material 5, which is much higher alloyed. The corrosion rates in technical phosphoric acid are in the range of the comparative alloy No. 2 designed for this purpose. The goal set here, namely to create a material in which the improvement of some properties is not at the expense of other properties. The removal rate according to column 5 is smaller by more than a power of ten for the material according to the invention than for the comparison materials. This is particularly noteworthy because it has previously been assumed that molybdenum only improves the resistance of a material to corrosion in reducing acids. Apparently, the significant improvement now found in oxidizing acids is due to the combined effect of molybdenum and chromium.

Lediglich bei der Sensibilisierungszeit muß eine gewisse Verschlechterung der Werte hingenommen werden. Diese insbesondere für die Schweißbarkeit maßgebliche Eigenschaft ist aber in der Praxis nicht ernsthaft beeinträchtigt, da selbst der Werkstoff Nr. 3 mit einer Sensibilisierungszeit, die nur bei der Hälfte bzw. einem Drittel derjenigen der erfindungsgemäßen Legierung liegt, als gut schweißbar gilt. Zusammenfassend ist demnach festzustellen, daß mit der erfindungsgemäßen Legierung die im Vergleich zur Ausgangslegierung angestrebte Verbesserung des Eigenschaften beim Lochfraßpotential, bei der kritischen Spaltkorrosions- und Lochfraßtemperatur erreicht wurde, daß die Beständigkeit gegen technische Phosphorsäure sich nicht verschlechtert hat und daß lediglich mit einer Verkürzung der Sensibilisierungszeit hinsichtlich der IK-Beständigkeit gerechnet werden muß, womit jedoch keine Beeinträchtigung der Schweißbarkeit verbunden ist.A certain deterioration in the values only has to be accepted during the sensitization period. This property, which is particularly important for weldability, is not seriously impaired in practice, since even material no. 3 has a Sensitization time, which is only half or a third of that of the alloy according to the invention, is considered to be easy to weld. In summary, it can therefore be stated that, with the alloy according to the invention, the improvement in properties sought at the pitting potential, at the critical crevice corrosion and pitting temperature compared to the starting alloy, that the resistance to technical phosphoric acid has not deteriorated and that only with a shortening of the sensitization time with regard to the IK resistance, but this does not affect the weldability.

In Figur 2 sind die Abtragungsraten in Monochloressigsäure für drei verschiedene Werkstoffe gegenübergestellt, und zwar einmal für den Grundwerkstoff und einmal für geschweißtes Material. Der erfindungsgemäße Werkstoff 1 schneidet in allen Fällen besser ab als die Vergleichswerkstoffe 2 und 3.The removal rates in monochloroacetic acid for three different materials are compared in FIG. 2, namely once for the base material and once for welded material. The material 1 according to the invention performs better in all cases than the comparison materials 2 and 3.

Der Test nach ASTM G 28, Practice A, wird angewandt, um Werkstoffe auf ihre Beständigkeit gegen interkristalline Korrosion zu untersuchen. Er wird in einer siedenden Lösung mit 50% H₂SO₄ und 3,7% Fe₂(SO₄)₃ durchgeführt. Solche Bedingungen treten in der Praxis beispielsweise bei der Handhabung verunreinigter Schwefelsäuren auf.The test according to ASTM G 28, Practice A, is used to examine materials for their resistance to intergranular corrosion. It is carried out in a boiling solution with 50% H₂SO₄ and 3.7% Fe₂ (SO₄) ₃. Such conditions occur in practice, for example, when handling contaminated sulfuric acids.

Der Test nach ASTM G 28, Practice B, wird zur Feststellung des Korrosionsverhaltens von Werkstoffen in stark oxidierenden, metallionenhaltigen Säuren benutzt. Dabei wird eine siedende Lösung mit 23% H₂SO₄, 1,2% HCl, 1% FeCl₃ und 1% CuCl₂ angewandt. Damit werden Bedingungen simuliert, wie sie beispielsweise in Beizbetrieben auftreten.The test according to ASTM G 28, Practice B, is used to determine the corrosion behavior of materials in strongly oxidizing acids containing metal ions. A boiling solution with 23% H₂SO₄, 1.2% HCl, 1% FeCl₃ and 1% CuCl₂ is used. This simulates conditions such as those that occur in pickling plants.

Zum Nachprüfen der Beständigkeit gegenüber Spannungsrißkorrosion unter Bedingungen, wie sie in tiefen Bohrlöchern bei der Suche nach Erdgas und Erdöl auftreten können, sind Sauergas-Prüf-Tests entwickelt worden. Dabei werden die Materialproben beispielsweise in einer 25%igen NaCl-Lösung im Autoklaven 35 Tage bei 232°C, 50 bar CO₂, 10 bar H₂S und 10 bar H₂O in einer Dreieckbiegeprobe mit σB=0,95 × RPO,2 geprüft. Der erfindungsgemäße Werkstoff zeigte in einem solchen Test keine Schädigung durch Spannungsrißkorrosion und keine Lochfraßkorrosion.

Figure imgb0002
Figure imgb0003
 Sour gas test tests have been developed to test the resistance to stress corrosion cracking under conditions such as can occur in deep boreholes when searching for natural gas and crude oil. The material samples are tested, for example, in a 25% NaCl solution in an autoclave for 35 days at 232 ° C, 50 bar CO₂, 10 bar H₂S and 10 bar H₂O in a triangular bending sample with σ B = 0.95 × R PO, 2 . In such a test, the material according to the invention showed no damage from stress corrosion cracking and no pitting corrosion.
Figure imgb0002
Figure imgb0003

Claims (11)

1. An alloy having 30 to 32% nickel, 26 to 28% chromium, 0.5 to 1.5% copper, max. 2% manganese, 6 to 7% molybdenum and 0.10 to 0.25% nitrogen, max. 1.0% silicon, max. 0.2% aluminium, max. 0.03% carbon, residue iron, including unavoidable admixtures.
2. An alloy according to claim 1, characterized in that the nitrogen content is 0.14 to 0.22%.
3. An alloy according to claim 1, characterized in that the nitrogen content is 0.16 to 0.20%.
4. An alloy according to claim 1, characterized in that the nitrogen content is approximately 0.18%.
5. Use of the alloy according to claims 1 to 4 as a material for making structural components which must have satisfactory resistance to corrosion, more particularly pitting and/or crevice corrosion in aqueous, neutral or acid media with a high chloride ion concentration.
6. Use of the alloy according to claims 1 to 4 as a material for making structural components which must have an abrasion rate of less than 0.20 mm/a in technical phosphoric acid with a chloride ion concentration of up to 1000 ppm at 100°C.
7. Use of the alloy according to claims 1 to 4 as a material for making structural components which must have a pitting potential of at least 1000 mVH at 75°C and at least 800 mVH at 90°C in aqueous neutral media with a chloride ion concentration of the order of magnitude of 20000 ppm.
8. Use of the alloy according to claims 1 to 4 as a material for making structural components which must have a critical pitting temperature of at least 80°C and a critical crevice corrosion temperature of at least 50°C in acid media with a chloride ion concentration of 50000 ppm and above such as, for example, an FeCl₃ solution.
9. Use of the alloy according to claims 1 to 4 as a material for making structural components which must be resistant to intercrystalline corrosion in the conditions set forth in ASTM G 28, Practice A.
10. Use of the alloy according to claims 1 to 4 as a material for making structural components which must have an abrasion rate of less than 0.5 mm/a in the solution-annealed state in the conditions set forth in ASTM G 28, Practice B.
11. Use of the alloy according to claims 1 to 4 as a material for making structural components which must be free from stress cracking and pitting corrosion in the conditions of an aggressive oxygen test.
Wording on Fig. 1 = pitting potential in mVH.
Wording on Fig. 2 (top right) = days; (bottom left, left to right) = material No. 3 _ basic material _ welding material.
EP88200969A 1987-05-19 1988-05-14 Corrosion-resistant alloy Expired - Lifetime EP0292061B1 (en)

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KR880014124A (en) 1988-12-22
JPS6425936A (en) 1989-01-27
NO168313B (en) 1991-10-28
NO168313C (en) 1992-02-05
NO882157L (en) 1988-11-21
US4876065A (en) 1989-10-24
CA1334801C (en) 1995-03-21
EP0292061A1 (en) 1988-11-23
AU596745B2 (en) 1990-05-10
AU1637688A (en) 1988-11-24
NO882157D0 (en) 1988-05-18
KR960010598B1 (en) 1996-08-06
DE3716665A1 (en) 1988-12-08
BR8802449A (en) 1988-12-20
DE3861905D1 (en) 1991-04-11
ZA883561B (en) 1990-01-31
ES2021822B3 (en) 1991-11-16
ATE61420T1 (en) 1991-03-15

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