EP0421521B1 - Anode pour tube à rayons X avec couche d'oxide - Google Patents

Anode pour tube à rayons X avec couche d'oxide Download PDF

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Publication number
EP0421521B1
EP0421521B1 EP90202558A EP90202558A EP0421521B1 EP 0421521 B1 EP0421521 B1 EP 0421521B1 EP 90202558 A EP90202558 A EP 90202558A EP 90202558 A EP90202558 A EP 90202558A EP 0421521 B1 EP0421521 B1 EP 0421521B1
Authority
EP
European Patent Office
Prior art keywords
oxide
weight
coating
ray anode
ray
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
EP90202558A
Other languages
German (de)
English (en)
Other versions
EP0421521A2 (fr
EP0421521A3 (en
Inventor
Wolfgang Hohenauer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Metallwerk Plansee GmbH
Original Assignee
Metallwerk Plansee GmbH
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 Metallwerk Plansee GmbH filed Critical Metallwerk Plansee GmbH
Publication of EP0421521A2 publication Critical patent/EP0421521A2/fr
Publication of EP0421521A3 publication Critical patent/EP0421521A3/de
Application granted granted Critical
Publication of EP0421521B1 publication Critical patent/EP0421521B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00—X-ray tubes
    • H01J35/02—Details
    • H01J35/04—Electrodes ; Mutual position thereof; Constructional adaptations therefor
    • H01J35/08—Anodes; Anti cathodes
    • H01J35/10—Rotary anodes; Arrangements for rotating anodes; Cooling rotary anodes
    • H01J35/105—Cooling of rotating anodes, e.g. heat emitting layers or structures

Definitions

  • the invention relates to an X-ray anode, in particular a rotating anode, with high heat emissivity, with a base body made of refractory metal or its alloys and a focal spot or focal path region made of refractory metal which may differ from the base body, the X-ray anode at least on parts of the surface outside the focal path essentially has the metals titanium, zirconium and optionally aluminum-containing oxidic coating.
  • X-ray tube anodes only emit a fraction of the radiated energy in the form of X-rays. The rest is transferred to heat and has to leave the anode in the form of heat radiation. It has therefore been known for many years to improve the heat emissivity of X-ray anodes from refractory metals by means of an oxidic coating (AT-A-337 314, DE-A-22 01 979, DE-A-24 43 354). These prior publications claim to increase the adhesion of the oxide layer on the surface of the base metal compared to the prior art by means of different oxide materials and production processes and to increase the thermal emissivity of the anode surface. It has been shown that the performance of layers produced in this way is limited in view of the continuously increasing requirements for X-ray anodes with regard to layer aging, heat radiation capability and the resistance to degassing (avoidance of electrical flashovers).
  • EP-A-0 172 491 describes in a further development an X-ray anode made of a molybdenum alloy with an oxide coating from a mixture of 40% - 70% titanium oxide, the rest of the stabilizing oxides from the group ZrO2, HfO, MgO, CeO2, La2O3 and SrO.
  • this prior publication has in particular the task of melting the oxides into smooth, shiny, shimmering layers by means of economical processes.
  • EP-A-0 244 776 relates essentially to the same subject matter of the invention.
  • the invention relates to the pretreatment of the oxidic material before application to the X-ray anode by means of conventional spraying techniques.
  • a mixture of 77% - 85% titanium dioxide with 15 - 23% by weight calcium oxide is processed in a first process step to a powder with a homogeneous phase and then optionally mixed with other oxide powders by known spraying methods.
  • Plasma spraying, sputtering processes, chemical and physical deposition processes from the gas phase or also the electron beam process are mentioned as coating processes for the oxide coating on the X-ray anodes made of refractory metals.
  • An X-ray anode made of refractory metal is usually subjected to a degassing annealing at the end of the manufacturing process.
  • the degassing annealing of the anode serves to avoid gas leaks and consequently highly undesirable flashovers between the electrodes when they are used in an X-ray tube in a high vacuum.
  • the inventive teaching of this prior publication includes an advantageous coordination of the material composition of the oxide layer with regard to the annealing treatment after the coating of the X-ray anodes.
  • These degassing anneals simultaneously serve for the final formation and melting of the oxide phase, ie the conversion into a state which cannot be achieved by an oxide application process such as the plasma spraying process alone.
  • the layer composition according to the prior publication and the processes for their production do not meet the requirements sufficiently. Rather, when annealing the oxide layers according to this prior publication, there is the risk that at an annealing temperature at which the oxides melt into smooth, well-adhering layers, they are already so thin that the contour between coated and uncoated parts of the X-ray anode surface is undesirable in Area of the focal track disappears to an intolerable extent. In addition, such oxide layers have an annoying gas phase formation at the required annealing temperatures.
  • the object of the present invention is therefore to give the oxide surface layer such a composition that, when it is produced by customary application processes, including annealing treatment, on the one hand, the good adhesion properties between the oxide layer and the substrate which have been achieved to date, and the good thermal emissivity properties of the layer, are at least maintained if not be surpassed.
  • the structural structure and the composition of the oxide layer should allow easier technical handling in the production of the layer, in particular with regard to smooth melting without annoying evaporation and undesirable flow of the oxide during the annealing treatment of the X-ray anode.
  • the object is achieved in that the oxidic coating on the X-ray anode contains 1 to 20% by weight of silicon oxide and is a homogeneously melted phase.
  • the oxide layer according to the invention applied to an X-ray anode made of high-melting metals has excellent adhesion, smooth surfaces and a high thermal heat coefficient ⁇ ⁇ 0.80.
  • the oxidic layer has the decisive advantage over the prior art that it is less liquid under otherwise comparable conditions during the required annealing treatment of the anode. ie the melt toughness is higher in comparison with similar oxide layers without the addition of silicon oxide when melting during the annealing treatment.
  • the contours between surface parts with and without oxide coating do not melt. There is only a comparatively small amount of evaporation and undesirable precipitation of oxide components on uncoated surface parts during the annealing process.
  • layers with a desired surface roughness of approx. 20 ⁇ m (R T ) and the appearance of an orange peel can be achieved.
  • X-ray rotary anodes are currently usually made from the refractory metals tungsten, molybdenum or molybdenum alloys, in particular the carbon-containing alloy TZM.
  • the oxidic coating has the previously preferred oxide components zirconium oxide, calcium oxide and / or titanium oxide, for example in a ratio of 70: 10: 20.
  • the calcium oxide can be partially or completely replaced by other stabilizing oxides known for such applications and can also be supplemented by small proportions of other, thermally stable compounds, such as borides and / or nitrides.
  • the aforementioned oxide mixture can contain up to 10% by weight of aluminum oxide, primarily for reducing or controlling the melting temperature.
  • the remainder of the composition of the oxidic coating is, according to the invention, silicon oxide with a weight fraction of 1-20%, preferably 4-7%.
  • the thickness of the oxide layer can vary between a few and a few thousand micrometers depending on the deposition process.
  • PVD and CVD processes in particular plasma CVD processes and sputtering processes, as well as flame spraying, plasma spraying and electron beam processes have proven themselves as deposition processes.
  • a homogeneous phase is to be understood as a finely divided oxide mixture in the oxidic coating.
  • the desired oxide layer structure and surface roughness can be achieved with good adhesion between the layer and the base material by means of annealing at temperatures between 1550 ° C and 1680 ° C and a glow time between 30 minutes and 1.5 hours achieve advantageous.
  • the evaporation of oxide components begins to become noticeable at temperatures above approx. 1550 ° C. In the worst cases, it is therefore advisable to cover the focal path area during the glow treatment or to carry out a final cleaning, for example also grinding treatment of the focal path after the glow treatment.
  • the molybdenum alloy TZM with low carbon content tends to release carbon at temperatures above 1550 ° C.
  • the released carbon forms volatile CO or CO2 with the oxygen components of the oxide in the oxide layer and results in premature aging of the layer.
  • An X-ray rotating anode consisting of the alloy Mo 5% by weight W has an approx. 2 mm thick W-Re layer in the focal path area.
  • this anode surface is provided with an oxide layer according to the invention.
  • a completely sintered and mechanically shaped X-ray anode on the back of the anode to be coated is cleaned and roughened by means of sandblasting and, if possible, subsequently coated under the usual process conditions by means of plasma spraying of oxide powder.
  • the applied oxide powder has the following composition: 89% by weight of an oxide mixture of 72% by weight ZrO2, 8% by weight CaO, 20% by weight TiO2, further 5% by weight Al2O3 and 6% by weight Si-O2.
  • the rotating anode coated in this way must be subjected to an annealing treatment in order to make it usable for use in X-ray tubes.
  • the rotating anode both the base material and the layer material, is largely freed of gas inclusions and of contaminants which are volatile at higher temperatures, in order to prevent electrical flashovers as a result of the release of gas inclusions when the rotating anode is later used in the high-vacuum X-ray tube.
  • the degassing annealing takes place within a narrow temperature and time range, matched to the anode base material, in order to avoid undesired structural changes in the base material.
  • the applied layer must also be treated within a very specific temperature and time range in order to achieve melting in the desired homogeneous phase and with a slightly nubbed surface structure (orange peel layer).
  • the annealing is carried out at 1620 ° C. for 65 minutes.
  • the melted layer has the desired degree of blackening and the desired surface structure (orange peel).
  • There is no uncontrolled flow of the melting oxide layer especially not in the transition area between coated and uncoated parts of the rotating anode surface. Insofar as gaseous oxides evaporate from the layer surface during the annealing process, these do not form a disturbing layer coating in the originally uncoated focal path area of the rotating anode.
  • the rotating anode was then tested in an X-ray tube arrangement under practical conditions. It ran there for several days without any problems within the required limit load.
  • An X-ray rotating anode consisting of the alloy TZM, has an approx. 2 mm thick W / Re layer in the focal path area. To increase the heat radiation capability, this anode surface is provided with an oxide layer according to the invention.
  • a completely sintered and mechanically shaped X-ray anode is cleaned and roughened by means of sandblasting and, if possible, coated immediately afterwards under the usual process conditions by means of plasma spraying outside the focal path area.
  • a molybdenum layer acting as a carbon barrier is applied and subjected to a reduction annealing in hydrogen at 1350 ° C. for 2 hours.
  • a first oxide coating based on aluminum oxide-titanium oxide It is only this oxide layer that enables the blackening oxidic coating to be melted in the required quality.
  • the final oxidic coating has the composition: 94% by weight of an oxide mixture of 72% zirconium oxide, 8% calcium oxide, 20% titanium oxide, and also 6% silicon oxide.
  • the rotating anode coated in this way must be subjected to an annealing treatment in accordance with Example 1.
  • Example 1 The rotating anode was then tested according to Example 1 in an X-ray tube test arrangement under practical conditions. There it ran trouble-free within the required limit load.

Landscapes

  • Coating By Spraying Or Casting (AREA)

Claims (6)

  1. Anode de tube à rayons X, en particulier anode tournante, à haute émittance thermique, comprenant un corps de base en métal à haut point de fusion ou en alliages de ceux-ci, ainsi qu'une zone de foyer de gaine ou de bande de gaine en un métal à haut point de fusion, éventuellement différent du corps de base, qui possède, au moins sur des parties situées en dehors de la bande de gaine, un revêtement formé par voie d'oxydation présentant les métaux: Ti, Zr et à volonté Al,
       caractérisé en ce que
       le revêtement contient des proportions de 1 à 20% en poids d'oxyde de silicium et une phase homogène fondue.
  2. Anode de tube à rayons X selon la revendication 1, caractérisée en ce que le revêtement formé par oxydation contient des additifs d'oxydes stabilisants.
  3. Anode de tube à rayons X selon la revendication 2, caractérisée en ce que l'additif stabilisant est de la CaO.
  4. Anode de tube à rayons X selon l'une des revendications 1 à 3, caractérisée en ce que une couche intermédiaire en deux strates, d'une épaisseur comprise entre 10 et 1000 µm, est disposée entre le corps de base en un alliage de Mo et le revêtement formé par oxydation, la première strate se composant de Mo et la deuxième strate d'un oxyde TiO₂ et/ou Al₂o₃.
  5. Anode de tube à rayons X selon l'une des revendications 1 à 4, caractérisée en ce que la composition du revêtement d'oxyde est la suivante:
       89% en poids d'un mélange d'oxydes comprenant 72% en poids de ZrO₂, 8% en poids de CaO et 20% en poids de TiO₂; ainsi que 5% en poids de Al₂O₃ et 6% en poids de SiO₂.
  6. Procédé de fabrication d'une anode pour tube à rayons X selon l'une des revendications 1 à 5, caractérisé en ce que le revêtement formé par oxydation est réalisé par pulvérisation en plasma de poudres d'oxyde et est fondu de façon simultanée avec le dégazage et le nettoyage du substrat dans un processus de recuit ultérieur à des températures comprises entre 1550 et 1680°C pendant un temps de recuit compris entre 0,5 et 1,5 heures, pour former une phase homogène à surface structurée.
EP90202558A 1989-10-02 1990-09-27 Anode pour tube à rayons X avec couche d'oxide Expired - Lifetime EP0421521B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0227689A AT394643B (de) 1989-10-02 1989-10-02 Roentgenroehrenanode mit oxidbeschichtung
AT2276/89 1989-10-02

Publications (3)

Publication Number Publication Date
EP0421521A2 EP0421521A2 (fr) 1991-04-10
EP0421521A3 EP0421521A3 (en) 1991-07-24
EP0421521B1 true EP0421521B1 (fr) 1994-11-09

Family

ID=3531351

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90202558A Expired - Lifetime EP0421521B1 (fr) 1989-10-02 1990-09-27 Anode pour tube à rayons X avec couche d'oxide

Country Status (5)

Country Link
US (1) US5157705A (fr)
EP (1) EP0421521B1 (fr)
JP (1) JPH03127439A (fr)
AT (1) AT394643B (fr)
DE (1) DE59007689D1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6132812A (en) * 1997-04-22 2000-10-17 Schwarzkopf Technologies Corp. Process for making an anode for X-ray tubes

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0487144A1 (fr) * 1990-11-22 1992-05-27 PLANSEE Aktiengesellschaft Anode pour tube à rayons X munie d'une couche d'oxyde
US6804497B2 (en) * 2001-01-12 2004-10-12 Silicon Laboratories, Inc. Partitioned radio-frequency apparatus and associated methods
US6749337B1 (en) 2000-01-26 2004-06-15 Varian Medical Systems, Inc. X-ray tube and method of manufacture
US6456692B1 (en) * 2000-09-28 2002-09-24 Varian Medical Systems, Inc. High emissive coatings on x-ray tube components
AU2001296611A1 (en) * 2000-10-23 2002-05-06 Varian Medical Systems, Inc. X-ray tube and method of manufacture
US20080039056A1 (en) * 2006-06-28 2008-02-14 Motorola, Inc. System and method for interaction of a mobile station with an interactive voice response system
US11450331B2 (en) 2006-07-08 2022-09-20 Staton Techiya, Llc Personal audio assistant device and method
JP2014216290A (ja) * 2013-04-30 2014-11-17 株式会社東芝 Ｘ線管及び陽極ターゲット

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT13732B (fr) * 1901-07-01 1903-10-26 Thomas Joseph Moriarty
AT38919B (de) * 1907-09-09 1909-09-25 Emil Kemper Befestigungsvorrichtung für in Eisenbahngüterwagen einsetzbare Türen, Wiehgitter und ähnliche Sperrwände.
DE2201979C3 (de) * 1972-01-17 1979-05-03 Siemens Ag, 1000 Berlin Und 8000 Muenchen Verfahren zur Herstellung einer geschwärzten Schicht auf Drehanoden von Röntgenröhren
NL7312945A (nl) * 1973-09-20 1975-03-24 Philips Nv Draaianode voor een roentgenbuis en werkwijze voor de vervaardiging van een dergelijke anode.
US4132916A (en) * 1977-02-16 1979-01-02 General Electric Company High thermal emittance coating for X-ray targets
JPS57158937A (en) * 1981-03-26 1982-09-30 Tokyo Tungsten Co Ltd Rotary anode target for x-ray tube
NL8101697A (nl) * 1981-04-07 1982-11-01 Philips Nv Werkwijze voor het vervaardigen van een anode en zo verkregen anode.
AT376064B (de) * 1982-02-18 1984-10-10 Plansee Metallwerk Roentgenroehren-drehanode
US4600659A (en) * 1984-08-24 1986-07-15 General Electric Company Emissive coating on alloy x-ray tube target
NL8402828A (nl) * 1984-09-14 1986-04-01 Philips Nv Werkwijze voor de vervaardiging van een roentgendraaianode en roentgendraaianode vervaardigd volgens de werkwijze.
US4840850A (en) * 1986-05-09 1989-06-20 General Electric Company Emissive coating for X-ray target
US4870672A (en) * 1987-08-26 1989-09-26 General Electric Company Thermal emittance coating for x-ray tube target

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6132812A (en) * 1997-04-22 2000-10-17 Schwarzkopf Technologies Corp. Process for making an anode for X-ray tubes

Also Published As

Publication number Publication date
EP0421521A2 (fr) 1991-04-10
DE59007689D1 (de) 1994-12-15
US5157705A (en) 1992-10-20
EP0421521A3 (en) 1991-07-24
ATA227689A (de) 1991-10-15
JPH03127439A (ja) 1991-05-30
AT394643B (de) 1992-05-25

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