EP0488450A1 - X-Ray tube anode with oxide layer - Google Patents

X-Ray tube anode with oxide layer Download PDF

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Publication number
EP0488450A1
EP0488450A1 EP91203023A EP91203023A EP0488450A1 EP 0488450 A1 EP0488450 A1 EP 0488450A1 EP 91203023 A EP91203023 A EP 91203023A EP 91203023 A EP91203023 A EP 91203023A EP 0488450 A1 EP0488450 A1 EP 0488450A1
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layer
anode
ray
intermediate layer
oxidic
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German (de)
French (fr)
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EP0488450B1 (en
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Wolfgang Hohenauer
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Plansee SE
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Plansee SE
Metallwerk Plansee GmbH
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00X-ray tubes
    • H01J35/02Details
    • H01J35/04Electrodes ; Mutual position thereof; Constructional adaptations therefor
    • H01J35/08Anodes; Anti cathodes
    • H01J35/10Rotary anodes; Arrangements for rotating anodes; Cooling rotary anodes
    • H01J35/105Cooling of rotating anodes, e.g. heat emitting layers or structures

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  • the invention relates to an X-ray anode, in particular a rotating anode, with high heat emissivity, with a carbon-containing base body made of a high-melting material and a focal spot or focal path region made of a high-melting metal or its alloys, which has an oxidic cover layer on at least parts of the surface outside the focal path has homogeneous melted phase.
  • EP-A2 0 172 491 describes an X-ray anode made from a molybdenum alloy, such as TZM, with an oxide coating from a mixture of 40-70% titanium oxide, the rest being stabilized oxides from the group ZrO2, HfO, MgO, CeO2, La2O3 and SrO.
  • melting the oxide coating improves the thermal emission coefficient and improves the adhesion of the oxide layer to the base body.
  • the disadvantage of such an X-ray anode is that the carbon contained in the base body of the rotating anode causes the oxidic cover layer to age rapidly, which leads to a premature deterioration in the thermal heat emission coefficient.
  • the AT-PS 376 064 describes an X-ray tube anode with a base, made of a carbon-containing molybdenum alloy, for. B. TZM, which is provided outside the focal path with a coating of one or more oxides or a mixture of one or more metals with one or more oxides to improve the heat emissivity.
  • a 10-200 ⁇ m thick intermediate layer made of molybdenum and / or tungsten between the base body and the oxidic coating in order to prevent the rapid aging of the rotating anode and thus the premature reduction of the thermal emission coefficient.
  • a disadvantage of such a rotating anode is that melted oxide cover layers are practically impossible to produce. It has been found that, depending on the type of application of the molybdenum and / or tungsten intermediate layer, the oxidic top layer cannot be melted at all or runs off from the surface to be coated during melting.
  • the object of the present invention is therefore to provide an X-ray tube anode consisting of a carbon-containing base body and a melted oxide cover layer to increase the to create thermal emission coefficients, which has a noticeably improved aging resistance with respect to the thermal emission coefficient compared to the prior art and in which the melting of the oxide cover layer into a homogeneous phase is possible without problems.
  • a two-layer intermediate layer is arranged with a layer of molybdenum and / or tungsten and a layer of Al2O3 with 1 - 30 wt.
  • the X-ray anodes according to the invention have an oxidic covering layer which adheres well to the base body and has good melting properties.
  • the thermal emission coefficient is more than 80% for suitable oxidic cover layers and deteriorates only insignificantly in the long-term operation of the X-ray anode.
  • oxide cover layers can now be melted without problems and do not run off the surface during melting, cannot be explained ad hoc from the theoretical background .
  • thermal coating processes such as. B. plasma spraying, for use.
  • PVD and CVD processes in particular plasma CVD processes and sputtering processes, have also proven themselves.
  • the oxide layer of the intermediate layer consists of Al2O3 with 5 - 20 wt.% TiO2 and the total layer thickness of the intermediate layer is between 10 and 100 ⁇ m.
  • the molybdenum alloy TZM with typical 0.5% Ti, 0.7% Zr and 0 - 0.05% C has proven to be the material for the base body.
  • An X-ray rotary anode consisting of the molybdenum alloy TZM, has an approx. 2 mm thick W-Re layer in the focal path area.
  • the anode surface is first provided with an intermediate layer according to the invention and then with an oxidic cover layer.
  • 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, immediately provided with a 20 ⁇ m thick molybdenum layer using plasma spraying. After this coating, annealing takes place under a hydrogen atmosphere at approx. 1350 o C for about 2 hours.
  • the oxide powder has the following composition: 68% by weight of ZrO2, 7.5% by weight of CaO, 19% by weight of TiO2 and 5.5% by weight of SiO2
  • the anode coated in this way must be subjected to an annealing treatment in order to make it useful 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 subsequently 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).
  • annealing takes place at 1620 o 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.
  • gaseous oxides evaporate from the layer surface during the annealing process, these are struck not as a disruptive layer 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 a TZM base body and a 2 mm thick W-Re layer in the focal path area is produced like the rotating anode according to Example 1, with the exception that the oxidic cover layer has the following changed composition: 68% by weight ZrO2, 7.5% by weight CaO, 19% by weight TiO2 and 5.5% by weight Al2O3
  • rotating anodes according to Examples 1 and 2 with rotating anodes which have the same oxidic cover layer but no intermediate layer according to the invention, are used with regard to their thermal emission factor as a function of temperature and time compared with each other.
  • curve 1 shows the course of the thermal emission factor ⁇ of a rotating anode produced according to Example 1 as a function of the temperature.
  • Curve 2 shows the corresponding course of a rotary anode produced in accordance with Example 1, but without an intermediate layer according to the invention. It can be seen that the course of these two curves is approximately the same.
  • Curve 3 shows the course of the thermal emission factor ⁇ of a rotating anode produced according to Example 1 after thermal aging of the rotating anode. The aging takes place by annealing the rotating anode for ten hours at a temperature which is higher than the maximum temperature that later occurs during operation.
  • Curve 4 shows the corresponding course of a thermally aged rotating anode produced in accordance with Example 1, but without an intermediate layer according to the invention. It is clear to see that the thermal emission coefficient shows only a slight deterioration even under long-term exposure due to the intermediate layer according to the invention, while the thermal emission coefficient of the rotating anode without the intermediate layer according to the invention drops significantly.
  • FIG. 2 shows, analogously to FIG. 1, the corresponding curves of a rotating anode produced according to Example 2 with and without an intermediate layer before and after ten hours of aging, curve 1 of the rotating anode with an intermediate layer before aging, curve 2 of the rotating anode without Intermediate layer before aging, curve 3 of the rotating anode with intermediate layer after aging and curve 4 of the rotating anode without intermediate layer after aging.
  • the intermediate layer according to the invention achieves a substantially improved aging resistance of the thermal emission factor.

Abstract

In an X-ray anode, in particular a rotary anode having a parent body consisting of a refractory material containing carbon, the anode is provided with an oxidic top coating containing a homogeneously fused phase outside the focal spot or the focal track to improve the heat radiation. Situated between the parent body and the oxidic top layer is a two-layer interlayer containing a layer of molybdenum and/or tungsten and a layer of Al2O3 containing 1 - 30 % by weight of TiO2. It is only this interlayer which makes it possible to fuse the oxidic top layer satisfactorily to form a homogeneous phase. In addition, the ageing resistance of the thermal emission coefficient is substantially improved.

Description

Die Erfindung betrifft eine Röntgenanode, insbesondere Drehanode, hoher Wärmeemissivität, mit einem Kohlenstoff enthaltenden Grundkörper aus einem hochschmelzenden Material sowie einem Brennfleck- bzw. Brennbahnbereich aus einem hochschmelzenden Metall oder dessen Legierungen, die zumindest auf Teilen der Oberfläche außerhalb der Brennbahn eine oxidische Deckschicht mit einer homogenen aufgeschmolzenen Phase aufweist.The invention relates to an X-ray anode, in particular a rotating anode, with high heat emissivity, with a carbon-containing base body made of a high-melting material and a focal spot or focal path region made of a high-melting metal or its alloys, which has an oxidic cover layer on at least parts of the surface outside the focal path has homogeneous melted phase.

Bei Röntgenröhrenanoden wird die zugeführte elektrische Energie nur zu einem Bruchteil in Röntgenstrahlungs-Energie umgesetzt. Der Großteil der Energie wird in unerwünschte Wärme umgesetzt, was zu einer starken Temperatur-Belastung der Anoden führt. Es hat daher in der Vergangenheit nicht an Versuchen gefehlt, die in Röntgenanoden erzeugte Wärmeenergie so rasch wie möglich, vorwiegend durch Vergrößerung der oberflächlichen Wärmeemissivität, abzuführen. Eine bekannte Maßnahme, die Wärmeemissivität der Röntgenanoden zu vergrößern, ist die Aufbringung oxidischer überzüge, die einen bestimmten Anteil an Titandioxid erhalten, wodurch sich ein Schwärzungseffekt ergibt. Diese oxidischen Deckschichten werden nach dem Schichtauftrag vielfach noch durch eine thermische Behandlung aufgeschmolzen, wodurch der Wärmeemissionsfaktor noch weiter verbessert wird und eine verbesserte Haftung der überzugsschicht am Substratmaterial erreicht wird.In the case of X-ray tube anodes, only a fraction of the electrical energy supplied is converted into X-ray radiation energy. Most of the energy is converted into unwanted heat, which leads to a high temperature load on the anodes. There has therefore been no lack of attempts in the past to dissipate the thermal energy generated in X-ray anodes as quickly as possible, predominantly by increasing the superficial heat emissivity. A known measure to increase the heat emissivity of the X-ray anodes is the application of oxidic coatings which contain a certain proportion of titanium dioxide, which results in a blackening effect. These oxide cover layers are often melted after the layer application by a thermal treatment, whereby the heat emission factor is further improved and improved adhesion of the coating layer to the substrate material is achieved.

Die EP-A2 0 172 491 beschreibt eine Röntgenanode aus einer Molybdänlegierung, wie TZM, mit einem Oxidüberzug aus einer Mischung von 40 - 70 % Titanoxid, der Rest stabilisierte Oxide aus der Gruppe ZrO₂, HfO, MgO, CeO₂, La₂O₃ und SrO. In dieser Vorveröffentlichung wird beschrieben, daß durch eine Aufschmelzung des oxidischen überzuges eine Verbesserung des thermischen Emissionskoeffizienten und eine verbesserte Haftung der Oxidschicht am Grundkörper erreicht wird. Der Nachteil einer derartigen Röntgenanode besteht darin, daß der im Grundkörper der Drehanode enthaltene Kohlenstoff eine starke Alterung der oxidischen Deckschicht bewirkt, was zu einer vorzeitigen Verschlechterung des thermischen Wärmeemissions-Koeffizienten führt.EP-A2 0 172 491 describes an X-ray anode made from a molybdenum alloy, such as TZM, with an oxide coating from a mixture of 40-70% titanium oxide, the rest being stabilized oxides from the group ZrO₂, HfO, MgO, CeO₂, La₂O₃ and SrO. In this prior publication it is described that melting the oxide coating improves the thermal emission coefficient and improves the adhesion of the oxide layer to the base body. The disadvantage of such an X-ray anode is that the carbon contained in the base body of the rotating anode causes the oxidic cover layer to age rapidly, which leads to a premature deterioration in the thermal heat emission coefficient.

Die AT-PS 376 064 beschreibt eine Röntgenröhren-Drehanode mit einem Grundkörper, aus einer Kohlenstoff enthaltenden Molybdänlegierung, z. B. TZM, die außerhalb der Brennbahn mit einem Überzug aus einem oder mehreren Oxiden oder aus einem Gemisch aus einem oder mehreren Metallen mit einem oder mehreren Oxiden zur Verbesserung der Wärmeemissivität versehen ist. Entsprechend dieser Vorveröffentlichung wird vorgeschlagen, zwischen Grundkörper und oxidischen Überzug eine 10 - 200 µm dicke Zwischenschicht aus Molybdän und/oder Wolfram anzuordnen, um auf diese Art und Weise die rasche Alterung der Drehanode und damit die vorzeitige Verminderung des thermischen Emissionskoeffizienten zu verhindern. Nachteilig bei einer derartigen Drehanode ist, daß aufgeschmolzene oxidische Deckschichten praktisch nicht herstellbar sind. Es ist festgestellt worden, daß je nach Art der Aufbringung der Molybdän- und/oder Wolfram-Zwischenschicht die oxidische Deckschicht überhaupt nicht zum Aufschmelzen gebracht werden kann oder beim Aufschmelzen von der zu beschichtenden Oberfläche abläuft.The AT-PS 376 064 describes an X-ray tube anode with a base, made of a carbon-containing molybdenum alloy, for. B. TZM, which is provided outside the focal path with a coating of one or more oxides or a mixture of one or more metals with one or more oxides to improve the heat emissivity. According to this prior publication, it is proposed to arrange a 10-200 μm thick intermediate layer made of molybdenum and / or tungsten between the base body and the oxidic coating in order to prevent the rapid aging of the rotating anode and thus the premature reduction of the thermal emission coefficient. A disadvantage of such a rotating anode is that melted oxide cover layers are practically impossible to produce. It has been found that, depending on the type of application of the molybdenum and / or tungsten intermediate layer, the oxidic top layer cannot be melted at all or runs off from the surface to be coated during melting.

Die Aufgabe der vorliegenden Erfindung ist es daher, eine Röntgenröhrenanode, bestehend aus einem kohlenstoffhältigen Grundkörper sowie einer aufgeschmolzenen oxidischen Deckschicht zur Erhöhung des thermischen Emissionskoeffizienten zu schaffen, die gegenüber dem Stand der Technik eine merklich verbesserte Alterungsbeständigkeit im Hinblick auf den thermischen Emissionskoeffizienten aufweist und bei der die Aufschmelzung der oxidischen Deckschicht zu einer homogenen Phase ohne Probleme möglich ist.The object of the present invention is therefore to provide an X-ray tube anode consisting of a carbon-containing base body and a melted oxide cover layer to increase the to create thermal emission coefficients, which has a noticeably improved aging resistance with respect to the thermal emission coefficient compared to the prior art and in which the melting of the oxide cover layer into a homogeneous phase is possible without problems.

Erfindungsgemäß wird dies dadurch erreicht, daß zwischen Grundkörper und oxidischer Deckschicht eine zweilagige Zwischenschicht mit ausgehend vom Grundkörper einer Lage Molybdän und/oder Wolfram und einer Lage Al₂O₃ mit 1 - 30 Gew.%-Anteilen TiO₂ angeordnet ist.According to the invention this is achieved in that a two-layer intermediate layer is arranged with a layer of molybdenum and / or tungsten and a layer of Al₂O₃ with 1 - 30 wt.

Die erfindungsgemäßen Röntgenanoden weisen durch die spezielle Zwischenschicht eine ausgezeichnet auf dem Grundkörper haftende, gute aufschmelzbare oxidische Deckschicht auf. Der thermische Emissionskoeffizient liegt für geeignete oxidische Deckschichten über 80 % und verschlechtert sich im Langzeitbetrieb der Röntgenanode nur unwesentlich.Due to the special intermediate layer, the X-ray anodes according to the invention have an oxidic covering layer which adheres well to the base body and has good melting properties. The thermal emission coefficient is more than 80% for suitable oxidic cover layers and deteriorates only insignificantly in the long-term operation of the X-ray anode.

Der Effekt, daß sich durch Ergänzen der bekannten Zwischenschicht aus Molybdän und/oder Wolfram durch eine weitere oxidische Lage ganz spezieller Zusammensetzung oxidische Deckschichten nunmehr problemlos aufschmelzen lassen und bei der Aufschmelzung nicht von der Oberfläche ablaufen, ist von den theoretischen Hintergründen her nicht ad hoc erklärbar.The effect that by supplementing the known intermediate layer of molybdenum and / or tungsten with a further oxidic layer of a very special composition, oxide cover layers can now be melted without problems and do not run off the surface during melting, cannot be explained ad hoc from the theoretical background .

Als Abscheideverfahren für die Zwischenschicht und die oxidische Deckschicht kommen vorzugsweise thermische Beschichtungsverfahren, wie z. B. Plasmaspritzen, zur Anwendung. Andere Abscheideverfahren, wie PVD- und CVD-Verfahren, insbesondere Plasma-CVD-Verfahren und Sputterverfahren, haben sich jedoch ebenso bewährt.As a deposition process for the intermediate layer and the oxidic top layer preferably thermal coating processes such as. B. plasma spraying, for use. However, other deposition processes, such as PVD and CVD processes, in particular plasma CVD processes and sputtering processes, have also proven themselves.

Die besten Ergebnisse hinsichtlich Aufschmelzeigenschaften und Alterungsbeständigkeit werden erzielt, wenn die oxidsche Lage der Zwischenschicht aus Al₂O₃ mit 5 - 20 Gew.%-Anteilen TiO₂ besteht und die Gesamtschichtstarke der Zwischenschicht zwischen 10 und 100 µm beträgt.The best results with regard to melting properties and aging resistance are achieved if the oxide layer of the intermediate layer consists of Al₂O₃ with 5 - 20 wt.% TiO₂ and the total layer thickness of the intermediate layer is between 10 and 100 µm.

Als aufgeschmolzene oxidische Deckschichten haben sich insbesondere Mischungen aus ZrO₂, TiO₂ und Al₂O₃ sowie Mischungen aus TiO₂, ZrO₂, Al₂O₃ und/oder SiO₂ jeweils mit oder ohne stabilisierende Oxide wie CaO und/oder Y₂O₃ bewährt.Mixtures of ZrO₂, TiO₂ and Al₂O₃ and mixtures of TiO₂, ZrO₂, Al₂O₃ and / or SiO₂, each with or without stabilizing oxides such as CaO and / or Y₂O₃, have proven particularly useful as melted oxide cover layers.

Als Material für den Grundkörper hat sich insbesondere die Molybdänlegierung TZM mit typisch 0,5 % Ti, 0,7 % Zr und 0 - 0,05 % C bewährt.In particular, the molybdenum alloy TZM with typical 0.5% Ti, 0.7% Zr and 0 - 0.05% C has proven to be the material for the base body.

Im folgenden wird die Erfindung anhand von Beispielen näher erläutert.The invention is explained in more detail below with the aid of examples.

Beispiel 1example 1

Eine Röntgendrehanode, bestehend aus der Molybdänlegierung TZM, weist im Brennbahnbereich eine ca. 2 mm dicke W-Re-Schicht auf. Zur Erhöhung der Warmeabstrahlfähigkeit wird die Anodenoberfläche zuerst mit einer erfindungsgemäßen Zwischenschicht und dann mit einer oxidischen Deckschicht versehen. Dazu wird eine fertig gesinterte und mechanisch umgeformte Röntgenanode auf der zu beschichtenden Anoden-Rückseite mittels Sandstrahlen gereinigt und aufgerauht und möglichst gleich anschließend unter den üblichen Verfahrensbedingungen mittels Plasmaspritzens mit einer 20 µm starken Molybdänschicht versehen. Nach dieser Beschichtung erfolgt eine Glühung unter Wasserstoffatmosphäre bei ca. 1350oC während etwa 2 Stunden. Dann erfolgt abermals durch Plasmaspritzen die Aufbringung einer oxidischen Schicht mit 13 Gew.% TiO₂, Rest Al₂O₃ in einer Schichtstärke von 20 µm.
Unmittelbar darauf erfolgt die Aufbringung der oxidischen Deckschicht in einer Schichtstärke von 20 µm ebenfalls durch Plasmaspritzen unter den üblichen Verfahrensbedingungen.
Das Oxidpulver weist folgende Zusammensetzung auf:
68 Gew.% ZrO₂, 7,5 Gew.% CaO, 19 Gew.% TiO₂ sowie 5,5 Gew.% SiO₂ Die so beschichtete Drehanode muß einer Glühbehandlung unterworfen werden, um sie für den Einsatz in Röntgenröhren brauchbar zu machen. Durch die Glühung wird die Drehanode, und zwar sowohl das Grundmaterial als auch das Schichtmaterial von Gaseinschlüssen sowie von bei höheren Temperaturen flüchtigen Verunreinigungen weitgehend befreit, um beim späteren Einsatz der Drehanode in der Hochvakuum-Röntgenröhre elektrische Überschläge als Folge der Freisetzung von Gaseinschlüssen auszuschalten. Die Entgasungsglühung erfolgt, abgestimmt auf das Anoden-Grundmaterial, innerhalb eines engen Temperatur- und Zeitbereiches, um unerwünschte Strukturänderungen des Grundmaterials zu vermeiden. Andererseits muß die aufgetragene Schicht in Abhängigkeit von deren Zusammensetzung ebenfalls innerhalb eines sehr spezifischen Temperatur- und Zeitbereiches behandelt werden, um ein Aufschmelzen in der gewünschten homogenen Phase und mit einer leicht genoppten Oberflächenstruktur (Orangenhautschicht) zu erzielen.
Die Glühung erfolgt im vorliegenden Fall bei 1620oC während 65 Minuten. Die aufgeschmolzene Schicht weist den gewünschten Schwärzungsgrad sowie die angestrebte Oberflächenstruktur (Orangenhaut) auf. Es kommt zu keinem unkontrollierten Fließen der aufschmelzenden Oxidschicht, insbesondere nicht im Übergangsbereich zwischen beschichteten und unbeschichteten Teilen der Drehanodenoberfläche. Soweit während des Glühvorganges gasförmige Oxide von der Schichtoberflache abdampfen, schlagen sich diese nicht als störender Schichtbelag im ursprünglich nicht beschichteten Brennbahnbereich der Drehanode nieder.
Die Drehanode wurde anschließend in einer Röntgenröhren-Versuchsanordnung unter praxisnahen Bedingungen erprobt. Sie lief dort über mehrere Tage störungsfrei innerhalb der geforderten Grenzbelastung.
An X-ray rotary anode, consisting of the molybdenum alloy TZM, has an approx. 2 mm thick W-Re layer in the focal path area. To increase the heat radiation capability, the anode surface is first provided with an intermediate layer according to the invention and then with an oxidic cover layer. For this purpose, 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, immediately provided with a 20 µm thick molybdenum layer using plasma spraying. After this coating, annealing takes place under a hydrogen atmosphere at approx. 1350 o C for about 2 hours. Then done again Plasma spraying the application of an oxide layer with 13 wt.% TiO₂, the rest Al₂O₃ in a layer thickness of 20 µm.
Immediately afterwards, the oxide cover layer is applied in a layer thickness of 20 μm, likewise by plasma spraying under the usual process conditions.
The oxide powder has the following composition:
68% by weight of ZrO₂, 7.5% by weight of CaO, 19% by weight of TiO₂ and 5.5% by weight of SiO₂ The anode coated in this way must be subjected to an annealing treatment in order to make it useful for use in X-ray tubes. As a result of the annealing, 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 subsequently 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. On the other hand, depending on its composition, 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).
In the present case, annealing takes place at 1620 o 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 are struck not as a disruptive layer 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.

Beispiel 2Example 2

Eine Röntgendrehanode aus einem TZM-Grundkörper und einer 2 mm dicken W-Re-Schicht im Brennbahnbereich wird wie die Drehanode entsprechend Beispiel 1 hergestellt, mit der Ausnahme, daß die oxidische Deckschicht folgende geänderte Zusammensetzung aufweist:
68 Gew.% ZrO₂, 7,5 Gew.% CaO, 19 Gew.% TiO₂ sowie 5,5 Gew.% Al₂O₃
An X-ray rotating anode consisting of a TZM base body and a 2 mm thick W-Re layer in the focal path area is produced like the rotating anode according to Example 1, with the exception that the oxidic cover layer has the following changed composition:
68% by weight ZrO₂, 7.5% by weight CaO, 19% by weight TiO₂ and 5.5% by weight Al₂O₃

Zum Nachweis, daß die erfindungsgemäße Zwischenschicht die Alterungsbeständigkeit des thermischen Emissionskoeffizienten gegenüber Drehanoden ohne Zwischenschicht deutlich verbessert, werden Drehanoden entsprechend den Beispielen 1 und 2 mit Drehanoden, die dieselbe oxidische Deckschicht jedoch keine erfindungsgemäße Zwischenschicht aufweisen, hinsichtlich ihres thermischen Emissionsfaktors in Abhängigkeit von Temperaturen und Zeit miteinander verglichen.To demonstrate that the intermediate layer according to the invention significantly improves the aging resistance of the thermal emission coefficient compared to rotating anodes without an intermediate layer, rotating anodes according to Examples 1 and 2 with rotating anodes, which have the same oxidic cover layer but no intermediate layer according to the invention, are used with regard to their thermal emission factor as a function of temperature and time compared with each other.

Die Erfindung wird dabei anhand von Figuren näher erläutert.The invention is explained in more detail with reference to figures.

Es zeigen

Figur 1
ein Diagramm, das die Temperaturabhängigkeit des thermischen Emissionsfaktors ε der nach Beispiel 1 hergestellten Drehanode sowie einer entsprechenden Drehanode ohne Zwischenschicht jeweils mit und ohne thermischer Alterung wiedergibt
Figur 2
ein Diagramm, das die Temperaturabhängigkeit des thermischen Emissionsfaktors ε der nach Beispiel 2 hergestellten Drehanode sowie einer entsprechenden Drehanode ohne Zwischenschicht jeweils mit und ohne thermischer Alterung wiedergibt.
Show it
Figure 1
a diagram showing the temperature dependence of the thermal emission factor ε of the rotating anode produced according to Example 1 and a corresponding rotating anode without an intermediate layer, in each case with and without thermal aging
Figure 2
a diagram showing the temperature dependence of the thermal emission factor ε of the rotating anode produced according to Example 2 and a corresponding rotating anode without an intermediate layer, each with and without thermal aging.

In Figur 1 zeigt die Kurve 1 den Verlauf des thermischen Emissionsfaktors ε einer nach Beispiel 1 hergestellten Drehanode in Abhängigkeit von der Temperatur.
Kurve 2 zeigt den entsprechenden Verlauf einer entsprechend Beispiel 1, jedoch ohne erfindungsgemäße Zwischenschicht, hergestellten Drehanode. Es ist zu sehen, daß der Verlauf dieser beiden Kurven etwa gleich ist. Kurve 3 zeigt den Verlauf des thermischen Emissionsfaktors ε einer nach Beispiel 1 hergestellten Drehanode nach einer thermischen Alterung der Drehanode. Die Alterung erfolgt durch eine zehnstündige Glühung der Drehanode bei einer Temperatur, die über der späteren im Betrieb auftretenden maximalen Temperatur liegt.
Kurve 4 zeigt den entsprechenden Verlauf einer entsprechend Beispiel 1, jedoch ohne erfindungsgemäße Zwischenschicht, hergestellten, thermisch gealterten Drehanode.
Es ist klar zu sehen, daß durch die erfindungsgemäße Zwischenschicht der thermische Emissionskoeffizient auch bei Langzeitbelastung eine nur geringfügige Verschlechterung zeigt, während der thermische Emissionskoeffizient der Drehanode ohne erfindungsgemäße Zwischenschicht signifikant absinkt.
In FIG. 1, curve 1 shows the course of the thermal emission factor ε of a rotating anode produced according to Example 1 as a function of the temperature.
Curve 2 shows the corresponding course of a rotary anode produced in accordance with Example 1, but without an intermediate layer according to the invention. It can be seen that the course of these two curves is approximately the same. Curve 3 shows the course of the thermal emission factor ε of a rotating anode produced according to Example 1 after thermal aging of the rotating anode. The aging takes place by annealing the rotating anode for ten hours at a temperature which is higher than the maximum temperature that later occurs during operation.
Curve 4 shows the corresponding course of a thermally aged rotating anode produced in accordance with Example 1, but without an intermediate layer according to the invention.
It is clear to see that the thermal emission coefficient shows only a slight deterioration even under long-term exposure due to the intermediate layer according to the invention, while the thermal emission coefficient of the rotating anode without the intermediate layer according to the invention drops significantly.

Figur 2 Zeigt analog wie Figur 1 die entsprechenden Kurven einer nach Beispiel 2 hergestellten Drehanode mit und ohne Zwischenschicht vor und nach zehnstündiger Alterung, wobei Kurve 1 der Drehanode mit Zwischenschicht vor der Alterung, Kurve 2 der Drehanode ohne Zwischenschicht vor der Alterung, Kurve 3 der Drehanode mit Zwischenschicht nach der Alterung und Kurve 4 der Drehanode ohne Zwischenschicht nach der Alterung entsprechen. Auch hier ist zu sehen, daß durch die erfindungsgemäße Zwischenschicht eine wesentlich verbesserte Alterungsbeständigkeit des thermischen Emissionsfaktors erreicht wird.FIG. 2 shows, analogously to FIG. 1, the corresponding curves of a rotating anode produced according to Example 2 with and without an intermediate layer before and after ten hours of aging, curve 1 of the rotating anode with an intermediate layer before aging, curve 2 of the rotating anode without Intermediate layer before aging, curve 3 of the rotating anode with intermediate layer after aging and curve 4 of the rotating anode without intermediate layer after aging. It can also be seen here that the intermediate layer according to the invention achieves a substantially improved aging resistance of the thermal emission factor.

Claims (6)

Röntgenanode, insbesondere Drehanode, hoher Wärmeemissivität mit einem Kohlenstoff enthaltenden Grundkörper aus einem hochschmelzenden Material sowie einem Brennfleck- bzw. Brennbahnbereich aus einem hochschmelzenden Metall oder dessen Legierungen, die zumindest auf Teilen der Oberfläche außerhalb der Brennbahn eine oxidische Deckschicht mit einer homogenen aufgeschmolzenen Phase aufweist,
dadurch gekennzeichnet,
daß zwischen Grundkörper und oxidischer Deckschicht eine zweilagige Zwischenschicht mit ausgehend vom Grundkörper einer Lage Molybdän und/oder Wolfram und einer Lage Al₂O₃ mit 1 - 30 Gew.%-Anteilen TiO₂ angeordnet ist.
X-ray anode, in particular a rotating anode, with high heat emissivity with a carbon-containing base body made of a high-melting material and a focal spot or focal path region made of a high-melting metal or its alloys, which has an oxidic cover layer with a homogeneous melted phase at least on parts of the surface outside the focal path,
characterized by
that between the base body and the oxide cover layer, a two-layer intermediate layer is arranged with a layer of molybdenum and / or tungsten and a layer of Al₂O₃ with 1 - 30 wt.
Röntgenanode, insbesondere Drehanode, nach Anspruch 1, dadurch gekennzeichnet, daß die oxidische Lage der Zwischenschicht aus Al₂O₃ mit 5 - 20 Gew.%-Anteilen TiO₂ besteht.X-ray anode, in particular a rotating anode, according to claim 1, characterized in that the oxidic layer of the intermediate layer consists of Al₂O₃ with 5-20% by weight of TiO₂. Röntgenanode, insbesondere Drehanode, nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Gesamtschichtstärke der Zwischenschicht zwischen 10 und 100 µm beträgt.X-ray anode, in particular rotary anode, according to claim 1 or 2, characterized in that the total layer thickness of the intermediate layer is between 10 and 100 µm. Röntgenanode, insbesondere Drehanode, nach einem der Ansprüche 1 - 3, dadurch gekennzeichnet, daß die oxidische Deckschicht aus einer Mischung aus ZrO₂, TiO₂ und Al₂O₃, gegebenenfalls mit stabilisierenden Oxiden, wie CaO und/oder Y₂O₃ besteht.X-ray anode, in particular rotary anode, according to one of claims 1-3, characterized in that the oxide cover layer consists of a mixture of ZrO₂, TiO₂ and Al₂O₃, optionally with stabilizing oxides such as CaO and / or Y₂O₃. Röntgenanode, insbesondere Drehanode, nach einem der Ansprüche 1 - 3, dadurch gekennzeichnet, daß die oxidische Deckschicht aus einer Mischung aus TiO₂, ZrO₂ und SiO₂, gegebenenfalls mit stabilisierenden Oxiden, wie Cao und/oder Y₂O₃ besteht.X-ray anode, in particular rotating anode, according to one of claims 1-3, characterized in that the oxide cover layer consists of a mixture of TiO₂, ZrO₂ and SiO₂, optionally with stabilizing oxides such as Cao and / or Y₂O₃. Röntgenanode, insbesondere Drehanode, nach einem der Ansprüche 1 - 5, dadurch gekennzeichnet, daß der Grundkörper aus TZM besteht.X-ray anode, in particular a rotating anode, according to one of claims 1-5, characterized in that the base body consists of TZM.
EP91203023A 1990-11-30 1991-11-20 X-Ray tube anode with oxide layer Expired - Lifetime EP0488450B1 (en)

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AT0242190A AT394642B (en) 1990-11-30 1990-11-30 X-RAY TUBE ANODE WITH OXIDE COATING
AT2421/90 1990-11-30

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EP0488450B1 (en) 1995-03-08
DE59104875D1 (en) 1995-04-13
AT394642B (en) 1992-05-25
US5157706A (en) 1992-10-20
ATA242190A (en) 1991-10-15
JPH04269436A (en) 1992-09-25

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