EP0299027B1 - Alliage de metaux refractaires resistant au fluage et son procede de production - Google Patents

Alliage de metaux refractaires resistant au fluage et son procede de production Download PDF

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Publication number
EP0299027B1
EP0299027B1 EP88901002A EP88901002A EP0299027B1 EP 0299027 B1 EP0299027 B1 EP 0299027B1 EP 88901002 A EP88901002 A EP 88901002A EP 88901002 A EP88901002 A EP 88901002A EP 0299027 B1 EP0299027 B1 EP 0299027B1
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EP
European Patent Office
Prior art keywords
alloy
creep
metals
sintered
refractory metals
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Expired - Lifetime
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EP88901002A
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German (de)
English (en)
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EP0299027A1 (fr
Inventor
Ralf Eck
Gerhard Leichtfried
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Metallwerk Plansee GmbH
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Metallwerk Plansee GmbH
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Classifications

    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • 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
    • C22C32/001—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 only oxides
    • C22C32/0015—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 only oxides with only single oxides as main non-metallic constituents
    • C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
    • 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
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon

Definitions

  • the invention relates to a sintered alloy of one or more of the high-melting metals Mo, W, Nb, Ta, V, Cr with a stacked structure, which has excellent heat resistance combined with excellent creep resistance at high temperatures, and a process for its production.
  • refractory metals are often used for molded parts that are designed to withstand high temperatures.
  • TZM molybdenum alloy which typically contains approximately 0.5% by weight of titanium, 0.08% by weight of zirconium and 0.05% by weight of carbon.
  • the US-PS 3982970 also describes a high-melting alloy of this type, where the base material is strengthened to dispersion by heat treatment in a special atmosphere.
  • a suitable atmosphere is one which contains particles of thorium oxide or aluminum oxide with a grain size of ⁇ 1 ⁇ m.
  • Known alloys of high-melting metals of this type are, for example, tungsten and molybdenum alloys, which are usually doped with small amounts of aluminum and / or silicon and potassium. It is essential with these alloys made of high-melting metals that at least potassium must always be present in the alloy so that a stacked wire structure is formed.
  • the additional doping elements such as aluminum and / or silicon ensure that the potassium does not completely diffuse out of the material during the sintering, while practically completely escaping even during the sintering.
  • the doping elements aluminum, silicon and potassium can in principle be introduced in liquid form, in the form of their solutions, and dry in the form of the solid powders.
  • both methods of introduction are not without problems in the production of these alloys from refractory metals on an industrial scale.
  • the introduction of the potassium can only be sensibly solved in the form of the potassium silicates.
  • the potassium silicates have the disadvantage that they are hygroscopic and are therefore very difficult to distribute uniformly in the powder mixture.
  • the wet introduction of the doping elements in the form of solutions is also not without disadvantages with regard to reproducible production, since the slight volatility of the solutions, again in particular in the case of potassium, sintering with high sintering densities, which would be very advantageous for the subsequent mechanical shaping , difficult.
  • the introduction of the doping elements with a very specific grain size was not considered to be of major importance.
  • the object of the present invention is to create an alloy with a stack structure of one or more high-melting metals, in which the use of potassium as a doping element is dispensed with, as a result of which good reproducible production of the alloy and in particular high densities during sintering are achieved.
  • the alloy is said to have improved room temperature, warm and creep strength properties compared to the known alloys of high-melting metals with a stacked structure.
  • the alloy 0.005-10% by weight of one or more compounds and / or one or more mixed phases of the compounds from the group of oxides, nitrides, carbides, borides, silicates or aluminates with a grain size elf 1.5 ⁇ m, the additions being limited to compounds and / or mixed phases whose melting point is above 1500 ° C.
  • the present invention is based on the completely surprising finding, based on the known prior art, that the element potassium can be dispensed with when using very specific compounds as doping materials for producing high-strength and creep-resistant, sintered alloys from high-melting metals with a stacked structure.
  • the alloy of high-melting metal according to the invention has high strength and creep resistance at high temperatures, which exceed those of the known alloys of high-melting metals with a stacked structure.
  • the strength values at room temperature also correspond, at least approximately, to those of the known alloys made of refractory metals, but may even exceed them in some cases.
  • a particularly advantageous alloy made of high-melting metal with a stacked structure according to the present invention contains 1-5% by weight of the oxides and / or mixed oxides with a respective grain size ⁇ 0.5 ⁇ m of one or more elements from the group La, Ce, Y, Th, Mg, Ca, Sr, Hf, Zr, Er, Ba, Pr, Cr.
  • Another particularly advantageous alloy made of refractory metal with a stacked structure according to the present invention contains 1-5% by weight of at least one of the borides and / or the nitride with a respective grain size ⁇ 0.5 ⁇ m, of Hf.
  • the oxides La2O3, CeO2, Y2O3, ThO2, MgO, CaO, the mixed oxides Sr (Hf, Zr) O3, ZrO2; Er2O3, SrZrO3, Sr4Zr3O10, BaZrO3 and La 0.84 Sr 0.16 CrO3 and the borides HfB, HfB2 and HfN have proven to be particularly suitable doping materials within an alloy content of 1-5% by weight. With additions of at least 1% by weight of the doping materials, considerable improvements in tensile strength and creep strength can still be achieved with certain compounds, in particular in the case of yttrium, compared to smaller amounts of alloys. On the other hand, alloy proportions that exceed 5% by weight do not bring any significant improvements in the properties mentioned in most cases, so that the preferred range can be limited to a maximum of 5% by weight due to the generally very expensive doping materials.
  • Molybdenum, tungsten, chromium and their alloys are particularly suitable as high-melting metals for the production of the alloy according to the invention.
  • the alloy of high-melting metal according to the invention can only be produced by powder metallurgy.
  • the alloy according to the invention is produced from high-melting metal in a particularly advantageous manner by adding 0.005-10% by weight of one or more compounds and / or one or more mixed phases of the compounds from the group of hydroxides, oxides, to the powdery high-melting metal or metals.
  • Nitrides, carbides, borides, silicates or aluminates with a grain size ⁇ 1.5 ⁇ m and a melting point above 1500 ° C are mixed in powder form and that the powder mixture is pressed and sintered in a known manner and the sintered body obtained with a degree of deformation of at least 85 % is mechanically formed while observing the necessary heat treatments and is then subjected to a recrystallization annealing.
  • the doping materials according to the invention can be introduced dry in the form of solid powders in the high-melting metal powder. It is only important that the doping materials are introduced in a correspondingly fine manner with the specified grain size as a discrete, that is to say non-agglomerated and non-aggregated powder. Such a powder can be obtained, for example, by spray drying finely precipitated compounds. The most uniform possible distribution is achieved by forced mixing.
  • Another method to achieve the required fine grain of the doping materials in the finished alloy is the introduction of the doping materials in the form of compounds that can be decomposed at low temperatures, for example in the case of lanthanum as lanthanum hydroxide La (OH) 3, lanthanum carbonate La2 ( CO3) 3 ⁇ 8H2O, lanthanum heptahydrate LaCl3 ⁇ 7H2O or lanthanum molybdate La2 (MoO4) 3.
  • lanthanum as lanthanum hydroxide La (OH) 3, lanthanum carbonate La2 ( CO3) 3 ⁇ 8H2O, lanthanum heptahydrate LaCl3 ⁇ 7H2O or lanthanum molybdate La2 (MoO4) 3.
  • the insertion can be achieved with the necessary fine grain.
  • the doping materials have melting points that are well above 1500 ° C., the amount of doping materials introduced into the powder mixture remains almost completely in the finished sintered alloy.
  • the doping materials have melting points that are close to the specified lower limit of 1500 ° C., some of the doping materials introduced into the powder mixture escape due to the high vapor pressure during sintering in gas form and entrains inevitable impurities in the alloy, so that a positive cleaning effect occurs.
  • the powder batches can be pressed on die presses or isostatic presses.
  • the compacts are usually sintered under normal pressure and under an H2 atmosphere.
  • the sintering temperature is selected depending on the alloy composition, but must as a rule be at least 200 ° below the melting point of the lowest melting component.
  • the achievable sintered densities of the alloy according to the invention are then over 95% of the theoretical density.
  • the alloy is mechanically deformed by at least 85%, e.g. by rolling or drawing.
  • the mechanical reshaping takes place in individual stages, each reshaping stage advantageously resulting in a reshaping by approximately 10%.
  • Heat treatments are inserted between the individual forming operations. It is essential that both the forming temperature and the temperature of the heat treatment are below the respective recrystallization temperature.
  • the material is subjected to a recrystallization annealing, whereby the stack structure is formed.
  • Table 1 shows the comparison of the creep strengths of known alloys made of high-melting metals according to the prior art and alloys according to the invention made of high-melting metals.
  • Table 2 shows the improved strengths and hardness values of alloys according to the invention made from refractory metals compared to alloys made from refractory metals according to the prior art and to unalloyed refractory metals.
  • Alloy 4 was produced in the same way as in Example 1. Instead of La (OH) 3 1 wt.% MgO was mixed with a grain size of 0.45 microns and wire of 0.5 mm in diameter was produced.
  • Alloy 5 was produced by the same procedure as in Example 1. Instead of La (OH) 3 1 wt.% Al2O3 with a grain size of 1.2 microns was mixed and wire of 0.5 mm in diameter was produced.
  • Molybdenum metal powder with a grain size of 5 microns was mixed with 2 wt.% La (OH) 3 powder with a grain size of 0.4 microns and pressed on dies with 3 MN to plates with the dimensions 17 cm ⁇ 40 cm ⁇ 5 cm.
  • the plates were then rolled to form sheet metal with a final sheet thickness of 1 mm, starting with grading temperatures of approximately 1400 ° C., in steps of approximately 10% each. After a final recrystallization annealing at approx. 1900 ° C, the sheets had a stacked structure.
  • a tungsten alloy according to the invention was produced as follows:

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Un alliage fritté, résistant au fluage, ayant une disposition structurelle empilée d'un ou plusieurs métaux réfractaires Mo, W, Nb, Ta, V, Cr contenant certains agents de dopage, ainsi qu'un procédé permettant sa production. Les agents spéciaux de dopage sont des compositions et/ou des phases mélangées de ces compositions prises dans le groupe des oxides, des nitrures, des carbures, des borures, des silicates ou des aluminates ayant un point de fusion supérieur à 1500°C. La taille de leurs grains est 1,5 mum, leur proportion dans l'alliage est comprise entre 0,005 et 10 % du poids. A la différence des règles de l'art connues en ce qui concerne cet alliage, l'utilisation de potassium en tant qu'agent de dopage est evitée. Une bonne consolidation reproductible, et en particulier des densités élevées pendant le frittage, peuvent ainsi être obtenues. En outre, cet alliage a de meilleures propriétés de résistance à la température ambiante, à la chaleur et au fluage que les alliages de métaux réfractaires connus ayant une dispositions structurelle empilée.

Claims (7)

1. Alliage fritté, résistant au fluage, à structure de texture en grappes, composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr, caractérisé en ce que il comporte 0,005 à 10% en poids d'une ou plusieurs combinaisons et/ou d'une ou plusieurs phases mixtes des combinaisons du groupe des oxydes, nitrures, carbures, borures, silicates ou aluminates d'une grosseur de grain ≦ 1,5 µm, les additifs étant limités à des combinaisons et/ou des phases mixtes dont le point de fusion est supérieur à 1500°C.
2. Alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb Ta, V, Cr selon la revendication 1, caractérisé en ce qu'il contient 1 à 5% en poids des oxydes et/ou des oxydes mixtes d'une grosseur de grain respective ≦ 0,5 µm d'un ou plusieurs des éléments du groupe La, Ce, Y, Th, Mg, Ca, Sr, Hf, Zr, Er, Ba, Pr, Cr.
3. Alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr selon la revendication1, caractérisé en ce qu'il contient 1 à 5% en poids des borures et/ou du nitrure d'hafnium respectivement d'une grosseur de grain ≦ 0,05 µm.
4. Alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr selon l'une des revendications 1 à 3, caractérisé en ce que le ou les métaux à haut point de fusion sont du molybdène ou un alliage de molybdène.
5. Alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr selon l'une des revendications 1 à 3, caractérisé en ce que le ou les métaux à haut point de fusion sont du tungstène ou un alliage de tungstène.
6. Alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr selon l'une des revendications 1 à 3, caractérisé en ce que le ou les métaux à haut point de fusion sont du chrome ou un alliage de chrome.
7. Procédé de fabrication d'un alliage fritté, résistant au fluage, à structure à texture en grappes composé d'un ou plusieurs des métaux à haut point de fusion Mo, W, Nb, Ta, V, Cr selon l'une des revendications 1, 4, 5 ou 6, caractérisé en ce qu'il est ajouté par mélange, métal à haut point de fusion ou aux métaux à haut point de fusion sous forme de poudre, 0,05 à 10% en poids d'une ou plusieurs des combinaisons et/ou d'une ou plusieurs phases mixtes des combinaisons du groupe des hydroxides, oxydes, nitrures, carbures, borures, silicates ou aluminates d'une grosseur de grain inférieure ou égale à 1,5 µm et à point de fusion supérieur à 1500°C sous forme de poudre et en ce que le mélange des poudres est comprimé et fritté de façon connue et que le corps fritté obtenu est transformé mécaniquement selon un taux de déformation d'au moins 85% en effectuant les traitements thermiques nécessaires et est finalement soumis à un circuit de recristallisation.
EP88901002A 1987-01-28 1988-01-26 Alliage de metaux refractaires resistant au fluage et son procede de production Expired - Lifetime EP0299027B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT158/87 1987-01-28
AT0015887A AT386612B (de) 1987-01-28 1987-01-28 Kriechfeste legierung aus hochschmelzendem metall und verfahren zu ihrer herstellung

Publications (2)

Publication Number Publication Date
EP0299027A1 EP0299027A1 (fr) 1989-01-18
EP0299027B1 true EP0299027B1 (fr) 1991-10-02

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EP88901002A Expired - Lifetime EP0299027B1 (fr) 1987-01-28 1988-01-26 Alliage de metaux refractaires resistant au fluage et son procede de production

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Country Link
US (1) US4950327A (fr)
EP (1) EP0299027B1 (fr)
JP (1) JP2609212B2 (fr)
AT (1) AT386612B (fr)
DE (1) DE3865259D1 (fr)
WO (1) WO1988005830A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0570072A2 (fr) * 1992-05-14 1993-11-18 PLANSEE Aktiengesellschaft Procédé d'obtention d'un alliage à base de chrome
EP0570072B1 (fr) * 1992-05-14 1996-07-31 PLANSEE Aktiengesellschaft Procédé d'obtention d'un alliage à base de chrome

Also Published As

Publication number Publication date
DE3865259D1 (de) 1991-11-07
WO1988005830A1 (fr) 1988-08-11
EP0299027A1 (fr) 1989-01-18
ATA15887A (de) 1988-02-15
US4950327A (en) 1990-08-21
AT386612B (de) 1988-09-26
JP2609212B2 (ja) 1997-05-14
JPH01502680A (ja) 1989-09-14

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