WO2011070475A1 - Alliage comprenant deux métaux réfractaires, en particulier w et ta, et anode à rayons x comprenant un tel alliage et procédé de production correspondant - Google Patents

Alliage comprenant deux métaux réfractaires, en particulier w et ta, et anode à rayons x comprenant un tel alliage et procédé de production correspondant Download PDF

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Publication number
WO2011070475A1
WO2011070475A1 PCT/IB2010/055489 IB2010055489W WO2011070475A1 WO 2011070475 A1 WO2011070475 A1 WO 2011070475A1 IB 2010055489 W IB2010055489 W IB 2010055489W WO 2011070475 A1 WO2011070475 A1 WO 2011070475A1
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WO
WIPO (PCT)
Prior art keywords
alloy
refractory metals
refractory
refractory metal
tantalum
Prior art date
Application number
PCT/IB2010/055489
Other languages
English (en)
Inventor
Paul Xu
Kevin C. Kraft
Min He
Gerald J. Carlson
Original Assignee
Koninklijke Philips Electronics N.V.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Koninklijke Philips Electronics N.V. filed Critical Koninklijke Philips Electronics N.V.
Priority to JP2012541613A priority Critical patent/JP2013513026A/ja
Priority to US13/512,977 priority patent/US20120236997A1/en
Priority to EP10798623.4A priority patent/EP2510130B1/fr
Priority to CN2010800552933A priority patent/CN102639730A/zh
Publication of WO2011070475A1 publication Critical patent/WO2011070475A1/fr

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Classifications

    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/088—Fluid nozzles, e.g. angle, distance
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2235/00—X-ray tubes
    • H01J2235/08—Targets (anodes) and X-ray converters
    • H01J2235/081—Target material

Definitions

  • the present invention relates to an alloy comprising at least two refractory metals and to an X-ray anode comprising such alloy. Furthermore, the present invention relates to a method of preparing such alloy and to a method of preparing such X-ray anode.
  • Rotating anodes in X-ray devices are subjected to large mechanical stresses, as well as thermal-mechanical stresses induced from an X-ray generation process.
  • X-Rays are generated by electron bombardment of the anode's focal track. A vast majority of energy applied to the focal spot and subsequent anode surface is transformed into heat, which must be managed.
  • the localized heating of the focal spot may be a function of the target angle, focal track diameter, focal spot size (length x width), rotating frequency, power applied, and material properties such as thermal conductivity, density, and specific heat.
  • Focal spot temperatures and thermal-mechanical stresses are usually managed by adequately controlling and selecting the above mentioned variables.
  • X-ray tube protocols may be limited due to a limited ability to modify these variables because of material property limitations.
  • a conventional rotating anode X-ray tube is often limited by the mechanical properties of the anode's substrate material, as well as the ability of the material to remove the heat from a localized volume.
  • X-ray anodes are manufactured with a Tungsten-Rhenium alloy by various means.
  • the current methods may be either mechanically mixing Tungsten and Rhenium powder or use of solvents containing Rhenium to mix with Tungsten powder. Both current practices then rely on Rhenium diffusion during a sinter fire process to create the Tungsten-Rhenium alloy. Rhenium is added to the Tungsten focal track to create an alloy with improved ductility.
  • the current alloy manufacturing processes may have a potential of creating a poor distribution of elements affecting the material properties.
  • an alloy comprising at least two refractory metals wherein the alloy has improved material properties. Furthermore, there may be a need for a method of forming such alloy. In addition, there may be a need for an X-ray anode in which at least a focal track region comprises such alloy and for a method of preparing such X-ray anode.
  • a method for forming an alloy comprising at least two refractory metals comprises the following steps preferably in the indicated order: (a) providing the two refractory metals in a common crucible; (b) melting both refractory metals by application of an electron beam; (c) mixing the molten refractory metals; and (d) solidifying the melt.
  • a method for preparing an X-ray anode comprising preparing an alloy using the method according to the above first aspect of the present invention and applying the alloy at least to portions of an X-ray anode substrate which portions form a focal track region of the X-ray anode.
  • an alloy comprising at least two refractory metals.
  • a first refractory metal forming a minor portion of the alloy is completely dissolved in a second refractory metal forming a major portion of the alloy.
  • an X-ray anode is proposed wherein at least a portion of the X-ray anode forming a focal track region comprises the alloy according to the above third aspect of the present invention.
  • a gist of the present invention may be seen as based on the following findings and ideas: It has been observed that in present refractory metal alloys material properties are frequently non-optimum. Such deficiency in material properties may be attributed to a poor distribution of the elements forming the alloy, i.e. the particles from which the alloy is composed.
  • the alloy-forming refractory metals are provided in the form of a powder wherein the mixture of powders of the pure metal is compacted, heated using for example electric current and further fabricated by e.g. cold working with annealing steps. Using such conventional fabrication methods, refractory metal alloys may be worked into wires, ingots, rebars, sheets or foils.
  • the alloy components in the form of a powder comprising macroscopic particles the atoms of the at least two refractory metals are usually not homogeneously distributed throughout a final alloy.
  • An idea is now to provide the at least two refractory metals in a common crucible and to melt both refractory metals such that the molten refractory metals can easily and preferably completely mix.
  • an advantageous way of melting refractory metals typically having very elevated melting point temperatures may be electron beam heating, i.e. directing an electron beam comprising high energy electrons onto the refractory metal material comprised in the crucible.
  • very high temperatures well above the melting point of refractory metals may be achieved.
  • the melt may be cooled down thereby resolidifying the melt.
  • the solidified melt then forms an alloy in which the two refractory metals are completely dissolved into each other.
  • Such homogeneous mixture of alloy components may result in advantageous material properties of the prepared alloy such as high temperature resistance, high mechanical strength, good thermal conductivity, high thermal capacity, etc.
  • Refractory metals are a class of metals that are extraordinarily resistant to heat and wear.
  • a definition which elements belong to this group may, in a wider interpretation, comprise 10 elements of the group 4, group 5 group 6 excluding the transuranium element but including the group 7 element rhenium.
  • the group of refractory metals at least comprises the five metals tungsten, molybdenum, niobium, tantalum and rhenium.
  • the two refractory metals comprised in the prepared alloy are tungsten (W) and tantalum (Ta).
  • tantalum may be provided in a weight percentage of between 5% and 15%, preferably between 8% and 12%, for example approximately 10% referred to the entire alloy weight.
  • the remainder of the alloy may be tungsten or may be tungsten further comprising other elements, particularly other refractory metal elements.
  • conventional refractory metal alloys used for example for X-ray anodes are generally composed from tungsten (W) and rhenium (Re) in order to obtain sufficient thermal and mechanical strength, it has been observed that particularly rhenium may be extremely expensive resulting in a high price of the alloy and devices fabricated therewith.
  • the rhenium comprised in the alloy may be responsible for some focal track erosion problems frequently occurring during X-ray anode operation. Such focal track erosion problems are also known as "mudflatting".
  • Tantalum is much cheaper than rhenium and surpasses most other refractory metals in ductility. Tantalum is dark, dense, ductile, very hard, easily fabricated and highly conductive of heat and electricity. Furthermore, the metal is renowned for its resistance to corrosion.
  • Tungsten and tantalum may have a significantly lower sputter rate of about 340 and 380 A/min , respectively. Accordingly, by replacing rhenium by tantalum in an alloy together with tungsten, the overall sputter rate of the alloy may be significantly reduced thereby possibly alleviating the focal track erosion problem (mudflatting).
  • At least one of the refractory metals comprised in the alloy is provided as a powder.
  • both refractory metal components are provided in the form of a powder.
  • the powder may comprise particles having for example a size in the range of 2 ⁇ to 100 ⁇ .
  • a complete mixing of the alloy components resulting in a complete dissolution of the two refractory metal components into each other may be achieved the faster the more the alloy fomiing components are already pre- mixed before the melting process. Accordingly, providing the refractory metal components in the form of small particles forming a powder may significantly accelerate the mixing process of the molten refractory metals and may therefore significantly shorten the overall duration needed for perfomiing the proposed method.
  • the molten refractory metals are quenched for solidification.
  • quenching may mean that the melt including the two molten refractory metals is cooled-down very rapidly.
  • cooling rates in a range of 200 Ks 1 to 2000 Ks 1 , e.g. between 800 Ks 1 and 1200 Ks 1 may be applied.
  • the melt may be rapidly cooled-down by bringing it into contact with a very cool liquid such as liquid nitrogen.
  • One possible way of rapidly cooling the melt comprising the molten refractory metals may be a pulverization process by gas atomization thereby solidifying the melt.
  • the liquid melt is formed to a powder for a fine particle distribution.
  • a gas atomization process is carried out by pouring melted metal through a refractory orifice, a high pressure inert gas, typically argon, breaks up the melted metal into liquid droplets, which are solidified.
  • a quenching process i.e. a rapid cool-down, for solidifying the melt comprising the two refractory metals may advantageously result in fomiing a so-called "infinite solid solution”.
  • a solid solution may be a solid-state solution of one or more solutes in a solvent.
  • a solute may be interpreted as the component fomiing a minor part of the final product, i.e. the final alloy, whereas the solvent may be interpreted to be formed by the major component of the final product.
  • the solute may be e.g. tantalum, whereas the solvent may be tungsten.
  • a mixture comprising a solute and a solvent is considered a solution rather than a compound when a crystal structure of the solvent remains unchanged by addition of the solutes and when a mixture remains in a single homogeneous phase. This often happens when the two components, i.e. in the present case the two refractory metals, involved are close together on the periodic table.
  • the solute may
  • infinite solid solution may be interpreted in that the two metals can form a solid solution at any percentage and may still maintain a single phase, i.e. the percentage of solute can be from 0 to 100 % without generating a second phase.
  • FIG. 1 shows a flow-chart indicating steps of a method for forming an alloy according to an embodiment of the present invention.
  • Fig. 2 illustrates an arrangement for melting refractory metals using an electron beam in accordance with an embodiment of the present invention.
  • Fig. 3 shows an X-ray anode comprising an alloy according to an embodiment of the present invention.
  • a first step two refractory metals such as tungsten (W) and tantalum (Ta) are provided in a form of small particles forming a powder.
  • the powder 1 comprising the two refractory metal components is filled into a crucible 3 enclosed within a vacuum container 5.
  • a vacuum of a pressure of for example 10 ⁇ 5 torr may be generated within the vacuum container 5 using a vacuum pump 7.
  • a high energy electron beam 9 is directed onto the pulverized mixture of refractory metals comprised in the crucible 3.
  • the electron beam 9 is emitted by a cathode 11 and is accelerated and controlled by an anode 13, the cathode 11 and the anode 13 being connected to a control 15.
  • the electrons emitted by the cathode 11 are accelerated using the anode 13 to very high energies in the range of between 20 keV and 50 keV.
  • the anode 13 may be controlled such as to focus the electron beam 9 onto the refractory metals comprised in the crucible 3 such that the electron beam 9 may be scanned along a surface of the refractory metal powder 1 in order to homogeneously heat the powder within the crucible 3.
  • the refractory metal powder 1 Upon impact of the high energy electrons of the electron beam 9, the refractory metal powder 1 is heated to such high temperatures of for example above 3410°C being the melting point of tungsten such that a melt comprising both refractory metals in a molten liquid state is formed.
  • the two refractory metals may mix (step S3) due to diffusion and/or convection processes. Thereby, a mixture in which the tantalum is completely dissolved within the tungsten may be generated.
  • step S4 the melt comprised in the crucible 3 is rapidly cooled ("quenched") thereby solidifying the melt.
  • Such cool-down process may be realized by gas atomization of the liquid melt.
  • the molten refractory metal mixture may be forced through an orifice and gas may be introduced into the metal stream just before it leaves a nozzle, serving to create turbulence as the entrained gas expands due to heating and exits into a large collection volume exterior to the orifice.
  • the collection volume is filled with gas to promote further turbulence of the molten metal jet.
  • the generated powder stream may be segregated using gravity.
  • a typical gas atomization nozzle 31 is shown. Such nozzle 31 may be connected to the crucible 3 but has not been shown in figure 2 for clarity reasons.
  • a liquid melt 33 coming from a tundish or crucible may flow to a nozzle orifice 35 where it may be ejected.
  • a gas jet 37 coming from a gas inlet 39 is directed onto the ejected metal stream in order to create a turbulence to thereby atomize the metal stream into metal droplets 41 which may be rapidly cooled.
  • Fig. 4 shows a cross-section of an X-ray anode 21 according to an embodiment of the present invention.
  • the X-ray anode 21 comprises a disk-shaped substrate 23 attached to a shaft 25 around which the anode may be rotated during operation.
  • a focal track region 29 is provided on a slanted surface 27, a focal track region 29 is provided.
  • This focal track region 29 comprises the tungsten-tantalum- alloy the preparation of which has been described above.
  • tungsten alloy powder is first put in a mould. It is distributed at the position of focal track. Then, TZM being a Molybdenum alloy with 0.5 wt.
  • the X- ray anode 21 may have superior characteristics such as an improved thermal resistance, improved mechanical strength, etc. Furthermore, such X-ray anode 21 may be produced at reduced costs as the expensive rhenium conventionally comprised in the focal track material of prior art X-ray anodes has been replaced by comparatively cheap tantalum.
  • the proposed targets may be used in rotating anode X-ray tubes as for example envisioned as high performance products that could be used in car dio -vascular or CT medical imaging equipment. X-ray tubes used for inspection and security could also benefit therefrom.

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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)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention porte sur un alliage comprenant au moins deux métaux réfractaires et sur un procédé permettant de former un tel alliage. Dans l'alliage, un premier métal réfractaire tel que le tantale constituant une partie minoritaire de l'alliage est complètement dissous dans un second métal réfractaire tel que le tungstène qui constitue une partie majoritaire de l'alliage. L'alliage peut être formé par introduction des deux métaux réfractaires dans un creuset commun (étape S1), fusion des deux métaux réfractaires par application d'un faisceau d'électrons (étape S2), mélange des métaux réfractaires fondus (étape S3) et solidification de la masse fondue (étape S4). Du fait du mélange complet possible des composants métalliques réfractaires à l'état fondu, des propriétés de matériau améliorées de l'alliage solidifié peuvent être obtenues. En outre, du fait de l'utilisation de tantale au lieu de rhénium conjointement avec du tungstène, un alliage de métaux réfractaires bon marché et résistant peut être produit, lequel alliage peut être utilisé, par exemple, pour former une région de piste focale d'une anode à rayons X.
PCT/IB2010/055489 2009-12-07 2010-11-30 Alliage comprenant deux métaux réfractaires, en particulier w et ta, et anode à rayons x comprenant un tel alliage et procédé de production correspondant WO2011070475A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2012541613A JP2013513026A (ja) 2009-12-07 2010-11-30 ２つの耐熱金属、特にタングステン及びタンタルを有する合金、及び上記合金を有するｘ線の陽極、並びに上記合金及びｘ線の陽極を製作するための方法
US13/512,977 US20120236997A1 (en) 2009-12-07 2010-11-30 Alloy comprising two refractory metals, particularly w and ta and x-ray anode comprising such alloy and method for producing same
EP10798623.4A EP2510130B1 (fr) 2009-12-07 2010-11-30 Procéde de fabrication d'un alliage contenant deux metaux réfractaires, en particuliere w et ta et une anode a rayons x contenant cet alliage, et son procédé de fabrication
CN2010800552933A CN102639730A (zh) 2009-12-07 2010-11-30 包含两种难熔金属特别是W和Ta的合金和包含此类合金的X射线阳极及其生产方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US26717809P 2009-12-07 2009-12-07
US61/267,178 2009-12-07

Publications (1)

Publication Number Publication Date
WO2011070475A1 true WO2011070475A1 (fr) 2011-06-16

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PCT/IB2010/055489 WO2011070475A1 (fr) 2009-12-07 2010-11-30 Alliage comprenant deux métaux réfractaires, en particulier w et ta, et anode à rayons x comprenant un tel alliage et procédé de production correspondant

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US (1) US20120236997A1 (fr)
EP (1) EP2510130B1 (fr)
JP (1) JP2013513026A (fr)
CN (1) CN102639730A (fr)
WO (1) WO2011070475A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018175567A1 (fr) * 2017-03-21 2018-09-27 Apollo Energy Systems, Inc. Procédé de fabrication d'un catalyseur de nickel spongieux et catalyseur de nickel spongieux ainsi fabriqué
CN109680173A (zh) * 2019-01-11 2019-04-26 重庆文理学院 一种钨钽铼难熔合金的制备方法
WO2021094560A1 (fr) 2019-11-15 2021-05-20 Taniobis Gmbh Poudre sphérique pour la fabrication d'objets en 3d

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CN105895474A (zh) * 2014-05-06 2016-08-24 苏州艾默特材料技术有限公司 一种x射线管阳极靶的制备方法
CN108070804B (zh) * 2017-12-13 2019-09-10 西北有色金属研究院 一种低密度铌合金的第二相弥散析出热处理方法
CN112616233B (zh) * 2020-12-16 2023-03-21 中国科学院合肥物质科学研究院 一种适用于加速器的稳态高束流密度长寿命锂离子源
CN112795828B (zh) * 2020-12-27 2022-08-12 西北工业大学 一种用于3d打印的钽钨合金及制备钽钨合金薄壁板的方法
CN113215462B (zh) * 2021-05-13 2021-12-17 中南大学 一种基于悬浮感应熔炼制备W-Ta单相固溶体材料

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WO2018175567A1 (fr) * 2017-03-21 2018-09-27 Apollo Energy Systems, Inc. Procédé de fabrication d'un catalyseur de nickel spongieux et catalyseur de nickel spongieux ainsi fabriqué
CN109680173A (zh) * 2019-01-11 2019-04-26 重庆文理学院 一种钨钽铼难熔合金的制备方法
CN109680173B (zh) * 2019-01-11 2020-02-07 重庆文理学院 一种钨钽铼难熔合金的制备方法
WO2021094560A1 (fr) 2019-11-15 2021-05-20 Taniobis Gmbh Poudre sphérique pour la fabrication d'objets en 3d

Also Published As

Publication number Publication date
EP2510130A1 (fr) 2012-10-17
EP2510130B1 (fr) 2014-10-15
US20120236997A1 (en) 2012-09-20
CN102639730A (zh) 2012-08-15
JP2013513026A (ja) 2013-04-18

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