EP2796580B1 - Composition d'alliage - Google Patents

Composition d'alliage Download PDF

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Publication number
EP2796580B1
EP2796580B1 EP14161255.6A EP14161255A EP2796580B1 EP 2796580 B1 EP2796580 B1 EP 2796580B1 EP 14161255 A EP14161255 A EP 14161255A EP 2796580 B1 EP2796580 B1 EP 2796580B1
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EP
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Prior art keywords
alloy
hafnium
zirconium
alloy composition
carbon
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EP14161255.6A
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German (de)
English (en)
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EP2796580A1 (fr
Inventor
Bryce Conduit
Gareth Conduit
Howard Stone
Mark Hardy
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Rolls Royce PLC
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Rolls Royce PLC
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum

Definitions

  • the present invention relates to an alloy composition, particularly though not exclusively, to an alloy composition suitable for use in refractory (i.e. high temperature) applications.
  • the invention further relates to a forging die comprising the alloy composition.
  • Prior alloy compositions comprising molybdenum are known, particularly for use in refractory applications such as fusion and fission reactors, rocket engine nozzles, furnace structural components and forging dies for forming components from high strength alloys. Such applications require high hardness (as measured according to the Vickers hardness test) at a particular operating temperature.
  • known molybdenum based alloy compositions have insufficient strength for some applications, particularly at high temperatures such as 1000 to 1100 °C, and may have a high cost of production.
  • compositions of prior molybdenum based alloys are given in table 1, given in terms of weight percentages. TZM is described in further detail in US patent 3275434 . Further prior molybdenum based alloys are described in "The Engineering Properties of Molybdenum Alloys" by F F Schmidt and H R Ogden. International patent publication WO9622402 also describes Molybdenum alloys with a range of compositions prepared by the addition of silicon and boron in amounts defined by the area of a ternary system phase diagram bounded by the points Mo-1.0 % Si-0.5 % B, Mo-1.0 % Si-4.0 % B, Mo-4.5 % Si-0.5 % B, and Mo-4.5 % Si-4.0 B.
  • Rhenium may also comprise an amount of Rhenium.
  • the inclusion of rhenium in a molybdenum alloy is thought to improve ductility, recrystallization temperature and strength.
  • rhenium is an expensive elemental addition, due to its relative scarcity in the earth's crust. Rhenium containing alloys may therefore have an unacceptably high cost of production.
  • the present invention describes an alloy composition and an article comprising the alloy composition which seeks to overcome some or all of the above problems. All percentage amounts are given in terms of weight percentages unless otherwise specified.
  • an alloy composition consisting of, in weight per cent, between 7% and 14% hafnium between 5% and 10% niobium, between 0.9% and 1.1% titanium, between 0.5% and 2% zirconium, between 0.1% and 0.7% tungsten and 0.05% and 0.3% carbon, and, optionally, an amount less than 2% tantalum wherein the balance consists of molybdenum and incidental impurities, wherein the titanium may be bonded with oxygen to form titanium oxide and wherein the tantalum may be bonded with oxygen to form tantalum oxide.
  • the described alloy has a high hardness at temperatures of between 1,000 and 1,100 °C, and is consequently suitable for a wide range of uses, including for example refractory articles.
  • the relatively high amount of hafnium has been found to form hafnium carbide (HfC), which acts as a strengthener.
  • HfC hafnium carbide
  • the alloy can also be produced at a lower cost compared to previous high strength molybdenum alloys.
  • the alloy composition may comprise between 8.5% and 9.5% hafnium, and preferably may comprise between 8.9% and 9.1% hafnium, and may comprise 9% hafnium.
  • the alloy composition may comprise between 0.15% and 0.25% carbon, and may comprise between 0.19% and 0.21% carbon, and may comprise 0.2% carbon.
  • the alloy may further comprise between 0.8 and 1.9% zirconium, may comprise between 0.8% and 1.0% zirconium, and may comprise 0.9% zirconium.
  • the zirconium may be bonded with the carbon present in the alloy to form zirconium carbide (ZrC).
  • the alloy composition may consist of between 7% and 14% hafnium, between 0.05% and 0.3% carbon and between 0.7% and 2% zirconium, wherein the balance comprises molybdenum. It has been found that a molybdenum based alloy having the above composition has a particularly high hardness and strength, having an ultimate tensile strength (UTS) of up to 984 Mega Pascals (MPa).
  • UTS ultimate tensile strength
  • the alloy may comprise 1% Ti.
  • the titanium may be bonded with oxygen to form titanium oxide (TiO 2 ).
  • TiO 2 has been found to further increase the strength of the alloy by providing dispersion strengthening, and / or solid solution strengthening.
  • the alloy may comprise between 5 and 6% Nb, and may comprise between 5.5 and 5.9% Nb, and may comprise 5.7% Nb.
  • NbC niobium carbide
  • the presence of Nb in the alloy composition has been found to form niobium carbide (NbC) with the carbon present in the alloy composition, which acts as a strengthener in addition to the strengthening provided by the HfC.
  • Nb can be used to provide further strengthening at a lower cost compared to further amounts of HfC.
  • the alloy may comprise between 0.3% and 0.7% tungsten, and may comprise 0.5% tungsten.
  • the addition of tungsten is thought to act as a solid solution strengthener, thereby increasing the strength of the alloy.
  • the tantalum may bond with oxygen in the alloy composition to form tantalum oxide. Tantalum oxide is thought to also act as a solid solution strengthener, thereby increasing the strength of the alloy.
  • the presence of metal oxides in the alloy composition is thought to provide dispersion solution strengthening, which will further increase the strength of the alloy.
  • the alloy composition may have an ultimate tensile strength of between 680 MPa and 760 MPa at a temperature of 1,000 °C.
  • an article comprising an alloy in accordance with the first aspect of the invention.
  • the article may comprise a forging die.
  • the alloy is particularly suitable for in use in a forging die, since the alloy provides a very high strength at high temperatures.
  • the alloy composition may consist of, in weight per cent, between 8.9% and 9.1% hafnium, between 5.5% and 5.9% niobium, between 0.9% and 1.1% titanium, between 0.8% and 1% zirconium, between 0.3% and 0.7% tungsten and 0.19 and 0.21% carbon, wherein the balance comprises molybdenum and incidental impurities.
  • Table 2 shows the compositional ranges of a first alloy composition
  • tables 3 and 4 show second and third alloy compositions respectively.
  • a back scattered electron image of the microstructure of the composition of table 4 is shown in Fig. 2 .
  • the nominal alloy composition is thought to have an ultimate tensile strength (UTS), of between approximately 680 MPa and 760 MPa at a temperature of 1,000 °C, which is supported by evidence from Vicker's hardness tests. This is an improvement in UTS of approximately 350 to 550 MPa at a temperature of 1,000 °C compared to prior molybdenum based alloy compositions such as TZM. Alloy compositions within the claimed range may have a UTS of up to 985 MPa.
  • UTS ultimate tensile strength
  • the alloy composition described in table 2 consists essentially of between 7% and 14% hafnium, between 0.05% and 0.3% carbon and between 0.7% and 2% zirconium, wherein the balance comprises molybdenum.
  • the alloy may also contain incidental impurities, such as oxygen, may which be incorporated in the surface of the alloy as the alloy oxidises during manufacture or in use.
  • the hafnium and the zirconium may be present either as elemental hafnium or zirconium, or as hafnium carbide and zirconium carbide respectively, or as a mixture of the two. In some cases, the zirconium could be omitted from the composition, while still resulting in an alloy composition having improved properties compared to prior compositions.
  • hafnium carbide hafnium carbide
  • HfC strengthening hafnium carbide
  • the amount of hafnium carbide in the composition is much greater than in previous compositions. That such a large amount of hafnium in the composition provides a benefit, was a surprising result from this research.
  • zirconium in the amounts specified in table 2 is thought to further increase the strength of the composition by the formation of particle strengthening zirconium carbide (ZrC).
  • Table 3 describes a second compositional range of an alloy composition comprising between 0.19 and 0.21% carbon, between 0.8 and 1.0% zirconium, and between 8.9 and 9.1% hafnium, with the balance of the composition being molybdenum.
  • the second compositional range further comprises niobium in an amount between 5.5 and 5.9%, titanium in an amount between 0.9 and 1.1%, and tungsten (W) in an amount between 0.3 and 0.7%.
  • niobium may be present as either elemental niobium, or may bond with the carbon present within the alloy composition to form niobium carbides.
  • the presence of niobium in the range specified in table 2 is thought to further increase the strength of the composition at both high and low temperatures, both by forming niobium carbides (NbC) and by solid solution strengthening.
  • titanium in the ranges specified in table 3 promotes the formation of dispersion strengthening titanium dioxide (TiO 2 ) in combination with oxygen impurities, which has the effect of further increasing the strength of the alloy composition in comparison to alloy compositions which lack titanium.
  • tungsten carbide has a relatively small contribution to the strengthening of the composition, and so may optionally be omitted from the composition, particularly in view of the increased processing costs inherent in tungsten containing alloy compositions. Indeed, an alloy comprising only molybdenum, hafnium and carbon in the amounts specified is necessary to provide an alloy having superior tensile strength at high temperatures relative to prior alloys.
  • One or more of titanium, niobium and tungsten may be omitted from the alloy, and the remaining components increased accordingly, in order to provide an alloy having the desired balance of material properties and cost.
  • Table 4 describes an example of a nominal composition of a molybdenum alloy in accordance with the present invention.
  • the alloy consists of substantially 5.7% niobium, 1.0% titanium, 0.2% carbon, 0.9% zirconium, 9.0% hafnium and 0.5% tungsten, with the balance of the composition (i.e. approximately 82.7%) comprising molybdenum.
  • Incidental impurities may also be present in the alloy composition, such as oxygen for example.
  • Figure 1 shows a graph of the UTS of the alloy at various temperatures, ranging from 0°C to 1400°C. As can be clearly seen, the nominal composition has a UTS of 770 ⁇ 90 MPa at 1000°C. This is a significant improvement on prior alloy compositions.
  • the alloy is produced by a powder processing method.
  • the powder processing method comprises melting and gas atomisation to form particles having a diameter of less than approximately 5 ⁇ m.
  • a billet is then formed by hot isostatic pressing (HIP) of the particles.
  • HIP hot isostatic pressing
  • the powder is subjected to heat at temperatures of approximately 2000°C at approximately 100 Mpa for approximately 4 hours.
  • Fig. 2 shows a sample of alloy having the nominal composition described in table 4.
  • the sample was produced using an arc-cast method.
  • the lighter areas of the sample are hafnium carbide precipitates within the alloy matrix.
  • the hafnium carbide precipitates are segregated to the interdentritic regions with molybdenum rich primary dendrites in the sample. More uniform, fine dispersions of hafnium carbide can be produced using a powder metallurgy process. This will be expected to improve the properties of the alloy further.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Powder Metallurgy (AREA)

Claims (9)

  1. Composition d'alliage constituée, en pourcentage en poids, de 7 % à 14 % d'hafnium, de 5 % à 10 % de niobium, de 0,9 % à 1,1 % de titane, de 0,5 % à 2 % de zirconium, de 0,1 % à 0,7 % de tungstène et de 0,05 % à 0,3 % de carbone, et, éventuellement, d'une quantité inférieure à 2 % de tantale, le reste étant constitué de molybdène et d'impuretés accidentelles, le titane pouvant être lié à l'oxygène pour former de l'oxyde de titane et le tantale pouvant être lié à l'oxygène pour former de l'oxyde de tantale.
  2. Composition d'alliage selon la revendication 1, la composition comprenant entre 8,5 % et 9,5 % d'hafnium, et pouvant comprendre entre 8,9 % et 9,1 % d'hafnium, et pouvant comprendre 9 % d'hafnium.
  3. Composition d'alliage selon la revendication 1 ou 2, la composition comprenant entre 0,15 % et 0,25 % de carbone, et pouvant comprendre entre 0,19 % et 0,21 % de carbone, et pouvant comprendre 0,2 % de carbone.
  4. Composition d'alliage selon l'une quelconque des revendications précédentes, la composition comprenant entre 5 et 6 % de niobium, et pouvant comprendre entre 5,5 et 5,9 % de niobium, et pouvant comprendre 5,7 % de niobium.
  5. Composition d'alliage selon l'une quelconque des revendications précédentes, la composition comprenant 1 % de Ti.
  6. Composition d'alliage selon l'une quelconque des revendications précédentes, la composition comprenant entre 0,8 et 1,9 % de zirconium, pouvant comprendre entre 0,8 % et 1,0 % de zirconium, et pouvant comprendre 0,9 % de zirconium.
  7. Composition d'alliage selon l'une quelconque des revendications précédentes, la composition comprenant entre 0,3 % et 0,7 % de tungstène, et pouvant comprendre 0,5 % de tungstène.
  8. Alliage selon l'une quelconque des revendications précédentes ayant une résistance à la traction maximale comprise entre 680 MPa et 760 MPa à une température de 1 000 °C.
  9. Composition d'alliage selon l'une quelconque des revendications précédentes constituée, en pourcentage en poids, de 8,9 % à 9,1 % d'hafnium, de 5,5 % à 5,9 % de niobium, de 0,9 % à 1,1 % de titane, de 0,8 % à 1 % de zirconium, de 0,3 % à 0,7 % de tungstène et de 0,19 à 0,21 % de carbone, le reste comprenant du molybdène et des impuretés accidentelles.
EP14161255.6A 2013-04-26 2014-03-24 Composition d'alliage Active EP2796580B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GBGB1307533.8A GB201307533D0 (en) 2013-04-26 2013-04-26 Alloy composition

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EP2796580A1 EP2796580A1 (fr) 2014-10-29
EP2796580B1 true EP2796580B1 (fr) 2019-09-11

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US (1) US20160369379A1 (fr)
EP (1) EP2796580B1 (fr)
GB (1) GB201307533D0 (fr)

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2678269A (en) * 1951-10-06 1954-05-11 Climax Molybdenum Co Molybdenum-titanium alloys
US3177076A (en) * 1961-06-12 1965-04-06 American Metal Climax Inc Forgeable high temperature cast alloys
GB1011781A (en) * 1963-01-04 1965-12-01 Imp Metal Ind Kynoch Ltd Niobium-base alloys
GB1022486A (en) * 1963-07-11 1966-03-16 Imp Metal Ind Kynoch Ltd Tantalum alloys
US5693156A (en) * 1993-12-21 1997-12-02 United Technologies Corporation Oxidation resistant molybdenum alloy
RU2320750C1 (ru) * 2006-05-15 2008-03-27 Юлия Алексеевна Щепочкина Сплав на основе ниобия

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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GB201307533D0 (en) 2013-06-12
US20160369379A1 (en) 2016-12-22

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