WO2017032825A1 - Alliages de vanadium résistants à l'oxydation et destinés à des éléments structuraux exposés à des températures élevées - Google Patents

Alliages de vanadium résistants à l'oxydation et destinés à des éléments structuraux exposés à des températures élevées Download PDF

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Publication number
WO2017032825A1
WO2017032825A1 PCT/EP2016/070070 EP2016070070W WO2017032825A1 WO 2017032825 A1 WO2017032825 A1 WO 2017032825A1 EP 2016070070 W EP2016070070 W EP 2016070070W WO 2017032825 A1 WO2017032825 A1 WO 2017032825A1
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Prior art keywords
vanadium
alloy according
boron
silicon
intermetallic
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PCT/EP2016/070070
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German (de)
English (en)
Inventor
Manja Krüger
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Otto-Von-Guericke-Universität Magdeburg
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Publication of WO2017032825A1 publication Critical patent/WO2017032825A1/fr

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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
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0078—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only silicides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the present invention relates to a vanadium alloy, which has excellent oxidation resistance even at high temperatures and is particularly suitable for the production of high temperature stressed components with simultaneous mechanical stress.
  • Vanadium has a low neutron capture cross-section, making it a promising candidate as a structural material for fusion reactors and for energy conversion applications such as gas turbines.
  • vanadium and vanadium alloys rapidly form oxides at high temperatures, as occur, for example, in fusion reactors and in the presence of oxygen.
  • the oxides can flake off or become liquid or gaseous at correspondingly higher temperatures and thus lead to an uncontrollable loss of material and shape of the component.
  • vanadium for the manufacture of components that are exposed to atmospheric conditions or other oxygenated environments at high temperatures.
  • Vanadium and vanadium alloys are therefore limited to applications carried out either under protective gas or in low-oxygen media or at low temperatures.
  • vanadium alloys with, for example, Ti, Zr, Ta, Nb and Cr as alloying elements as reactor materials at temperatures up to about 950 K in an oxygen-free or oxygen-poor environment such as an inert gas atmosphere (for example helium) or in water.
  • V-4Ti-4Cr alloys showed the formation of a significant oxide layer when treated in dry air at 700 ° C (973 K). Significantly thicker oxide layers were observed when minor additions of Si, Al and Y were added to the base alloy (Fujiwara et al., "Oxidation and Hardness Profiles of V-Ti-Cr-Si-Al-Y Alloys", Journal of Nuclear Materials 283 -287 (2000) 131 1 -1315).
  • vanadium alloys which have improved oxidation resistance even at relatively high temperatures and can therefore also be used at higher temperatures in an oxygen-containing atmosphere. Furthermore, the vanadium alloy should have the best possible mechanical strength even at higher temperatures.
  • a vanadium alloy having 2 to 35 at.% Silicon (Si), 3 to 50 at.% Boron (B) and the remainder vanadium (V), wherein the vanadium alloy comprises at least one intermetallic phase of at least vanadium, silicon and boron having.
  • Preferred content ranges are 5 to 18 at.% For silicon and 22 to 35 at.% For boron.
  • the alloy contains 5 to 18 at.% Silicon and 22 to 35 at.% Boron.
  • the vanadium alloy according to the invention has a microstructure in which one or more intermetallic phases with the constituents vanadium, silicon and boron are distributed in a matrix of vanadium.
  • the intermetallic phases of vanadium according to the invention with silicon and boron are collectively referred to below as "intermetallic V-Si-B phase (s)."
  • intermetallic Phases having a different composition such as phases of V with Si such as V3S1, V5S13, etc., as well as intermetallic phases, which may contain other alloying elements.
  • the vanadium alloys according to the invention are resistant to oxidation even at relatively high temperatures.
  • the intermetallic V-Si-B phases which are distributed in the vanadium matrix, form a thin protective layer on the surface at high temperatures under oxygen-containing atmosphere.
  • this protective layer By means of this protective layer, the vanadium material is protected against further oxidation and the dimensional stability of components which have been produced from the vanadium material according to the invention is made possible.
  • the protective effect or oxidation resistance is all the better the higher the volume fraction of inventive intermetallic V-Si-B phase in the vanadium alloy.
  • the intermetallic V-Si-B phase is comparatively brittle, as the intermetallic phase in the vanadium alloy increases, the susceptibility to cracking and breakage of the material increases, that is, the mechanical strength in terms of fracture toughness decreases.
  • the vanadium alloys with increasing volume fraction of the intermetallic phases under compressive stress have increasing strengths.
  • the volume fraction of the intermetallic V-Si-B phase (s) in the vanadium alloy should preferably be at least 35 vol.%, In particular at least 50 vol.%, And 75 vol. do not exceed. These values are values optimized with regard to oxidation resistance and mechanical resistance, which can be exceeded or exceeded depending on the application and requirements. From the point of view of mechanical resistance, in particular fracture toughness, it is particularly advantageous if the intermetallic phases do not interrupt the vanadium matrix.
  • the V-Si-B intermetallic phases improve the oxidation resistance of the alloy and the more ductile and fracture-resistant vanadium matrix ensures good mechanical properties. From the viewpoint of oxidation resistance, therefore, a material of 100% intermetallic V-Si-B phase is advantageous, but such a perfectly intermetallic material is very brittle, so that for use in the production of mechanically stressed components also sufficient mechanical resistance should be respected.
  • the vanadium alloy according to the invention also has its own contribution
  • Temperatures up to 1 .000 ° C also at pressures of 1 to 2 GPa an excellent strength on.
  • the values found are significantly higher than those of materials such as steels, nickel-base alloys or titanium alloys.
  • the vanadium alloys according to the invention thus have a
  • FIG. 1 shows a diagrammatic sectional view of an embodiment of a vanadium alloy according to the invention with intermetallic V-Si-B phase
  • FIG. 2 shows a diagram of the oxidation curves at 600 ° C. of examples of inventive V alloys in comparison with prior art V alloys;
  • Figure 3 is a graph of oxidation curves of examples of inventive V alloys at 600 ° C and 700 ° C after pre-oxidation
  • FIG. 4 shows a diagram with the results of a compressive stress measurement of examples of inventive V alloys.
  • FIG. 1 shows the microstructure of a vanadium alloy according to the invention with the composition V-9Si-15B according to exemplary embodiment 1, an intermetallic phase having the composition V5S1B2 being homogeneously distributed in the vanadium matrix.
  • the volume fraction of phase V5S1B2 on the alloy is about 50% in this example.
  • the macroscopic phase areas formed can have a multiform shape and are idealized only in a sectional view as a hexagon. Shown in FIG. 1 is an optimized alloy with regard to the balance between oxidation resistance and mechanical properties.
  • the vanadium alloy according to the invention may contain a V-Si-B intermetallic phase as is the case in FIG. There may also be two or more V-Si-B intermetallic phases.
  • phase V5S1B2 is phase V5S1B2, as illustrated in FIG. 1 in an idealized manner.
  • intermetallic V-Si-B phase in addition to the intermetallic V-Si-B phase according to the invention, one or more further phases having different compositions may also be present in the vanadium alloy according to the invention, for example intermetallic phases formed from V and Si. In addition, there may be intermetallic phases comprising one or more of the additional alloying elements mentioned below.
  • the alloy of the present invention may contain one or more additional alloying elements selected from the group consisting of Ti, Fe, Zr, Mg, Hf, Li, Pb, Bi, Cr, Mn, Co, Ni, Cu, Zn, Ge, Ga, Y , Nb, Mo, Ru, Rh, Pd, Ag, Au, Cd, Ca, La, Ta, W, Re, Os, Ir, Pt and Au.
  • These additional alloying elements may typically each be added at a level of from 0.01 at.% To 15 at.%, And preferably to at least 10 at.%.
  • additional alloying elements may also be added in the form of their oxides, nitrides and / or carbides in concentrations of up to 15% by volume of the alloy.
  • a powder of supersaturated mixed crystals of the alloy components is produced in a first step.
  • powder metallurgical processes are used for the production of the mixed crystal powder for the alloy according to the invention, such as gas atomization with rapid cooling (rapid solidification) or mechanical alloying. These methods are known per se.
  • the resulting pre-alloyed powder is compacted.
  • the compaction is carried out in such a way that in the end result compact structural materials are obtained which have the desired microstructure after the last compaction step.
  • Conventional compaction processes such as cold pressing, sintering, hot pressing or other compaction processes such as Field Assisted Sintering Technology (FAST), Spark Plasma Sintering (SPS), Sintering or Equal Channel Angular Pressing (ECAP) can be used for compaction.
  • FAST Field Assisted Sintering Technology
  • SPS Spark Plasma Sintering
  • ECAP Equal Channel Angular Pressing
  • the mentioned compaction methods are known per se.
  • the precipitation of the intermetallic V-Si-B phase or phases according to the invention and the residual porosity of the material can be controlled via the temperature and holding time. Typical temperatures are between 1000 ° C and 1 .700 ° C.
  • the heating to the desired temperature can be done in one step or in several steps. Subsequently is cooled rapidly to room temperature, suitable heating or cooling rates are in a range between 50 and 150 K / min.
  • suitable holding times are between 15 minutes and several hours, the holding time depending on the method used, the nature and chemical composition of the powder particles and the temperature.
  • the sintering activity of smaller powder particles is higher than the larger particles, so that the required holding time decreases with decreasing particle size.
  • particles of irregular shape require a longer hold time and / or higher temperature than regularly shaped particles.
  • the higher the Si and B content the longer the compaction process should take at high temperature in order to achieve the highest possible density in the compact material.
  • the compaction by means of FAST method can be carried out as follows:
  • the production method (production of the supersaturated mixed-crystal powder and compaction) is preferably carried out in an oxygen-free atmosphere as possible, for example under an inert gas such as argon, a reducing atmosphere, for example hydrogen or a hydrogen-containing mixture, or vacuum.
  • an inert gas such as argon
  • a reducing atmosphere for example hydrogen or a hydrogen-containing mixture, or vacuum.
  • starting materials pure V, Si and boron powders were mechanically alloyed in the stated quantitative ratio (9 at.% Si, 15 at.% B and the remainder vanadium) in order to obtain a supersaturated mixed-crystal powder.
  • the starting materials were ground in a planetary ball mill for 20 hours at 200 U / min.
  • the resulting supersaturated powder was compacted using the Field Assisted Sintering method.
  • the compaction was carried out by first heating to 1 .100 ° C and held for 15 minutes. Thereafter, it was further heated to 1 .500 ° C and held again for 15 minutes. Subsequently, it was cooled down to room temperature.
  • a vanadium alloy was obtained whose idealized sectional view is shown in FIG.
  • the vanadium alloy obtained contained the intermetallic phase V5S1B2, which was homogeneously distributed in the vanadium matrix, and had no discontinuity of the vanadium matrix.
  • the alloying components were processed in the amounts mentioned (12.5 at.% Si, 25 at.% B, remainder vanadium) as under 1, with the exception that during the compaction in the second stage the mixture was heated to 1 600 ° C and the temperature was kept for 30 minutes. As a result, a V alloy containing about 90 vol% intermetallic phase V 5 SiB 2 was obtained .
  • sample material with about 50% intermetallic phases (Example 1) and about 90% intermetallic phase (Example 2) was heated to 600 ° C, wherein after 2, 5, 10, 20, 50 and 100 hours cooled to room temperature and the mass was determined.
  • the alloys of the present invention have higher oxidation resistance.
  • Example 1 For further investigation of oxidation resistance, the vanadium alloys of Example 1 and Example 2 were subjected to pre-oxidation at 1, 000 ° C for one hour under air. This pre-oxidation served to form an oxide protective layer on the surface, which in turn protects against further oxidation.
  • the compressive strength of the vanadium alloys according to Examples 1 and 2 was measured at temperatures between 600 ° C and 1, 000 ° C.
  • the compressive stress-strain curves which show the strength and deformation potential of the alloys as a function of the temperature and the content of intermetallic phases, is shown in FIG.
  • the measurement was carried out with a testing machine from Zwick type Z100, wherein the measurement according to DIN 50106: 1978-12 "testing of metallic materials; Pressure test "was performed.
  • the pressure range limit of the testing machine was reached in the alloys according to Example 1 at 600 ° C and after Example 2 at 1, 000 ° C. It follows that the material is significantly stronger at these temperatures than can be measured with the testing machine used.
  • the vanadium alloy Due to the higher concentration of intermetallic phases, the vanadium alloy is about 90% stronger than the vanadium alloy according to example 1 with about 50% intermetallic phase.
  • the high oxidation resistance in conjunction with the high compressive strength make the vanadium alloys according to the invention an excellent material for the production of components which are exposed to high temperatures with simultaneous mechanical stress.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un alliage de vanadium comprenant de 2 à 35 en% atomique de silicium et de 3 à 50 en% atomique de bore, ledit alliage étant résistant à l'oxydation même à des températures élevées et étant approprié notamment à la fabrication d'éléments structuraux exposés à des températures élevées.
PCT/EP2016/070070 2015-08-25 2016-08-25 Alliages de vanadium résistants à l'oxydation et destinés à des éléments structuraux exposés à des températures élevées WO2017032825A1 (fr)

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DE102015114092.6 2015-08-25
DE102015114092.6A DE102015114092B4 (de) 2015-08-25 2015-08-25 Oxidationsbeständige Vanadiumlegierungen für hochtemperaturbeanspruchte Bauteile

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
WO2019234016A1 (fr) * 2018-06-05 2019-12-12 Otto-Von-Guericke-Universität Magdeburg Alliage de molybdène à densité optimisée
DE102019121936A1 (de) * 2019-08-14 2021-02-18 Technische Universitaet Dresden Hochtemperaturaktivlote

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019234016A1 (fr) * 2018-06-05 2019-12-12 Otto-Von-Guericke-Universität Magdeburg Alliage de molybdène à densité optimisée
CN112218964A (zh) * 2018-06-05 2021-01-12 奥托·冯·格里克马格德堡大学 密度优化的钼合金
US11492683B2 (en) 2018-06-05 2022-11-08 Otto-Von-Guericke-Universitat Magdeburg Density-optimized molybdenum alloy
CN112218964B (zh) * 2018-06-05 2023-03-10 奥托·冯·格里克马格德堡大学 密度优化的钼合金
DE102019121936A1 (de) * 2019-08-14 2021-02-18 Technische Universitaet Dresden Hochtemperaturaktivlote

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