EP3109889A1 - Anode rotative de tube a rayons x - Google Patents

Anode rotative de tube a rayons x Download PDF

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Publication number
EP3109889A1
EP3109889A1 EP16001702.6A EP16001702A EP3109889A1 EP 3109889 A1 EP3109889 A1 EP 3109889A1 EP 16001702 A EP16001702 A EP 16001702A EP 3109889 A1 EP3109889 A1 EP 3109889A1
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EP
European Patent Office
Prior art keywords
focal
carrier body
rotary anode
grain boundary
ray rotary
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EP16001702.6A
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German (de)
English (en)
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EP3109889B1 (fr
Inventor
Johann Eiter
Jürgen SCHATTE
Wolfgang Glatz
Gerhard Leichtfried
Wolfram Knabl
Stefan SCHÖNAUER
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Plansee SE
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Plansee SE
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    • 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
    • H01J35/108—Substrates for and bonding of emissive target, e.g. composite structures
    • 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
    • H01J35/101—Arrangements for rotating anodes, e.g. supporting means, means for greasing, means for sealing the axle or means for shielding or protecting the driving
    • 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
    • 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
    • H01J2235/085—Target treatment, e.g. ageing, heating

Definitions

  • the present invention relates to an X-ray rotary anode which has a carrier body and a focal path formed on the carrier body, wherein the carrier body and the focal path are produced by powder metallurgy in the composite, the carrier body is formed from molybdenum or a molybdenum-based alloy, and the focal track made of tungsten or a tungsten-based alloy is formed.
  • the surface of the focal track is as smooth as possible.
  • the achievable life of the focal point should be as stable as possible against a roughening of the focal point surface and the formation of wide and / or deep cracks in the same. Due to the high temperatures and temperature gradients as well as the high rotational speeds, relatively high thermal and mechanical stresses occur on the carrier body. Despite these stresses, the carrier body should be as stable as possible against macroscopic deformations. So far, the prevailing view has been that this stability can be obtained both in the focal lane and in the carrier body in that both the focal lane and the carrier body are present in a completely recrystallized structure. It was assumed that in this way the structure of the focal track as well as the structure of the support body are largely stable even with the high, occurring use temperatures against subsequent microstructural changes (eg compared to a recrystallization, etc.).
  • the object of the present invention is to provide a powder metallurgically produced in the composite X-ray rotary anode, which allows a high dose yield over long periods of use and has a long service life.
  • an X-ray rotary anode comprising a support body and a focal path formed on the support body.
  • the carrier body and the focal path are produced by powder metallurgy in a composite, the carrier body is formed from molybdenum or a molybdenum-based alloy, and the focal lane is formed from tungsten or a tungsten-based alloy.
  • the focal lane is formed from tungsten or a tungsten-based alloy.
  • this section does not show grain nucleation (in the case of a non-recrystallized structure) or significantly less than 100% grain remodeling resulting crystal grains (partially recrystallized structure) on.
  • the remaining portion of this section is present in a forming structure, which is obtained in the powder metallurgy production by the forming step, in particular by the forging process.
  • a very fine-grained structure both large-angle grain boundary and wide-angle grain boundary portions and small-angle grain boundaries
  • This structure has a very smooth surface, which is advantageous in terms of dose yield. It was found that this structure recrystallized locally under the influence of an electron beam (For example, when "conditioning” or “retraction” with the electron beam, and / or during use). The region in which recrystallization takes place is limited to the immediate vicinity of the path of the electron beam on the focal path and, depending on the thickness of the focal path, can extend down into the carrier body (and possibly into it). The refractory path then has in the recrystallized region an increased ductility, which is advantageous with regard to the prevention of cracking, and an increased thermal conductivity, which is advantageous with regard to an effective heat dissipation to the carrier body. The surrounding areas of the focal track remain largely unchanged.
  • the locally recrystallized structure of the focal track (in use) remains considerably finer grained than is the case in the recrystallization processes in the context of conventional production processes, in particular the conventional powder metallurgical production processes.
  • the focal track surface is also smooth in the areas with the recrystallized structure over long periods of use and has a uniform, finely distributed crack pattern. Accordingly, with the X-ray rotary anode according to the invention over long periods of use a high dose yield can be achieved.
  • a higher starting hardness (and a higher starting strength) can be obtained with increasing degree of deformation (which is set in the step of forming, in particular forging). From this starting hardness (and starting strength), the hardness (and strength) decreases with the degree of recrystallization of the structure. As the degree of recrystallization increases, ductility also increases.
  • a partially recrystallized structure (with respect to the focal path and with respect to the carrier body) is understood to mean a structure in which grain grains formed by grain remodeling are surrounded by a forming structure and in which a cross-sectional area through the part Recrystallized structure these crystal grains form an area ratio in the range of 5-90%.
  • the area fraction of the crystal grains formed by grain regeneration is in the range below 5% or if there are no crystal grains formed in the structure by grain nucleation, an unrecrystallized structure is assumed in the present context. If the area fraction exceeds 90%, then in the present context a completely recrystallized structure is assumed.
  • a possible measuring method suitable for determining the area fraction is described below in connection with the description of FIG Figs. 4A-4D specified.
  • the X-ray rotary anode according to the invention is, in particular, a high-performance X-ray rotary anode which is designed for high radiation power (or dose rate) and a high rotational speed.
  • Such high-power X-ray rotary anodes are used in particular in the medical field, such as in computed tomography (CT) and in cardiovascular applications (CV).
  • CT computed tomography
  • CV cardiovascular applications
  • further layers, add-on parts, etc. such as a graphite block, etc., may also be provided on the carrier body, in particular on the side remote from the focal point.
  • additional heat removal from the carrier body is generally required.
  • the inventive X-ray rotary anode is designed for active cooling.
  • a flowing fluid out which serves for heat dissipation from the carrier body.
  • a graphite body eg by soldering, diffusion bonding, etc.
  • the X-ray rotary anode can also be designed for lower radiation powers. In this case, it may be possible to dispense with an active cooling and the attachment of a graphite block.
  • a molybdenum-based alloy is particularly referred to an alloy containing molybdenum as the main constituent, i. to a higher proportion (measured in weight percent) than any other containing element.
  • special alloys with high strength and hardness can also be used as the carrier body material and / or atomic impurities or particles can be added to the respective carrier body material to increase the strength.
  • the molybdenum-based alloy has a proportion of at least 80 (wt.%: Weight percent) molybdenum, in particular of at least 98 wt.% Molybdenum.
  • a tungsten-based alloy is particularly referred to an alloy having tungsten as the main component.
  • the focal track is formed from a tungsten-rhenium alloy having a rhenium content of up to 26 wt.%.
  • the rhenium content is in a range of 5-10 wt.%. Good properties can be achieved with regard to hardness, temperature resistance and heat conduction in the case of these stated compositions of the focal track and of the carrier body and especially in the narrower regions specified in each case.
  • a "finally heat-treated x-ray rotary anode” is understood to have passed through all the heat treatment (s) carried out during the powder metallurgical production.
  • the claimed features relate in particular to the end product (not yet used), as it is present after completion of the heat treatment (s) carried out as part of the powder metallurgical production ,
  • the powder metallurgy production of the carrier body and the fuel track in the composite can be seen on the end product, inter alia, at the pronounced diffusion zone between the carrier body and the focal track.
  • the diffusion zone is typically formed smaller or almost nonexistent.
  • the "section" of the focal path is referred to a macroscopic contiguous section (ie, including a plurality of grain boundaries and / or grain boundary sections) of the focal path. It can also be several, such sections with the claimed properties.
  • the portion of the focal path over which (in use) the path of the electron beam passes has the claimed properties.
  • non-recrystallized and / or partially recrystallized structure refers to a structure which can not be exclusively recrystallized, which can be exclusively partially recrystallized, or which can not be partially recrystallized in sections and partially recrystallized in sections.
  • the ⁇ 111> direction and the ⁇ 001> direction are aligned more along the normal of the focal plane than along the directions parallel to the focal plane.
  • the "focal plane" is determined by the main extension surface of the focal track. If the focal plane is curved (which is the case, for example, in the case of a frustum-shaped focal path), reference is made to the main extension surface present in the respective measuring or reference point of the focal track.
  • the preferential texturing of the ⁇ 111> direction and the ⁇ 001> direction perpendicular to the focal plane is set by the forging process and decreases with increasing degree of recrystallization of the focal path.
  • the degree of recrystallization in turn increases with increasing temperature and with increasing duration of the heat treatment (at and / or after forging).
  • the stated texture coefficients are also a measure of the degree of recrystallization of the focal track. In particular, the higher the texture coefficients of these directions, the lower the degree of recrystallization of the focal track.
  • the section of the focal track is present in a non-recrystallized structure or in a partially recrystallized structure with a relatively low degree of recrystallization. It was found that within these ranges, the above-explained, advantageous properties (high hardness, fine graininess) of the focal path can be achieved, with these advantageous properties occur even more at even higher texture coefficients.
  • the section of the focal track perpendicular to the focal plane has a texture coefficient TC (222) of ⁇ 5 and / or a texture coefficient TC (200) of ⁇ 6.
  • the degree of deformation is lower (for example only in the range of 20% -30% (total) degree of deformation of the x-ray rotary anode), then the preferred texturisations given above are also less pronounced.
  • the section of the focal track perpendicular to the focal plane has a texture coefficient TC (222) of ⁇ 3.3 and / or a texture coefficient TC (200) of ⁇ 4, the range of these lower limit values in particular at comparatively low degrees of deformation is approximated.
  • the peak that can be evaluated as part of the XRD measurement at the network level (222) is also weighted by the equivalent network levels (eg, (111), etc.). Accordingly, the intensity of the peak determined by XRD measurement (222) and in particular the thereof texture coefficient TC (222) determined a measure of the preferential texturing of the ⁇ 111> direction (perpendicular to the focal plane). Similarly, the intensity of the peak (200) determined by XRD measurement, and in particular the texture coefficient TC (200) determined therefrom, is a measure of the preferential texturing of the ⁇ 001> direction.
  • I (hkl) denotes the intensity, determined by XRD measurement, of the relevant peak (hkl) at which the texture coefficient TC (hkl) is to be determined.
  • the "specific intensity" of a peak (hkl) is the maximum of the relevant peak (hkl), as recorded in the XRD measurement.
  • the texture-free intensities for the respective peaks can be taken from databases, with the data in each case being used for the main constituent of the relevant material. Accordingly, in the present case, the powder diffraction file for tungsten (JCPDS No. 00-004-0806) was used for the focal line.
  • the texture-free intensity 100 for the peak (200) the texture-free intensity 15, for the peak (211) the texture-free intensity 23, for the peak (220) the texture-free intensity 8, for the peak ( 310) uses the texture-free intensity 11, for the peak (222) the texture-free intensity 4 and for the peak (321) the texture-free intensity 18.
  • the track is ground so that the area of the forging zone (upper portion of the track which was in direct contact with the forging tool or in close proximity to the forging tool during the forging process) is removed, if not already complete in the finished X-ray rotary anode was removed.
  • the focal track with a ground plane parallel to the focal plane is ground to a residual thickness of 0.1-0.5 mm (depending on the output thickness of the focal track).
  • the obtained ground surface is electropolished several times, at least twice (to remove the deformation structure due to the grinding process).
  • Molybdenum and molybdenum based alloys also have a cubic internal centered crystal structure. Accordingly, the notations discussed above with respect to the focal path, the texture coefficient determination formula, the sample preparation, and the measurement method are respectively applicable.
  • the X-ray rotary anode is ground down to the carrier body material, the ground surface extending parallel to the focal plane.
  • the Powder Diffraction File for molybdenum JCPDS No. 00-042-1120
  • the texture-free Intensity 100 for the peak (200) the texture-free intensity 16, for the peak (211) the texture-free intensity 31, for the peak (220) the texture-free intensity 9, for the peak (310) the texture-free intensity 14, for the peak (222) the texture-free intensity 3 and for the peak (321) the texture-free intensity 24 is used.
  • the section of the focal track is completely in a partially recrystallized structure.
  • the entire focal track is completely in a partially recrystallized structure.
  • crystal grains formed in the partially recrystallized structure by grain regeneration are surrounded by a forming structure and these crystal grains have an area fraction in the range of 10% to 80%, in particular in a range of 10%, based on a cross-sectional area through the partially recrystallized structure 20% to 60%. Within these areas, and in particular within the narrower range, it was possible to achieve good properties of the focal track with respect to its surface quality and dose yield, even over long periods of use.
  • the method for determining the area ratio which can be used for the specified range of values is explained with reference to the figures (see in particular the description of the figures relating to FIGS FIGS. 4A-4D ).
  • the area fraction (the crystal grains produced by grain regeneration) is ⁇ 80%, in particular ⁇ 60%.
  • Such a fine-grained structure which has an average small-angle grain boundary distance of ⁇ 10 ⁇ m, is particularly advantageous with regard to avoiding roughening of the focal point surface.
  • This fine granularity of the structure also depends on the degree of deformation. Accordingly, especially at a high degree of deformation of the X-ray rotary anode, a low, medium small angle grain boundary distance can be achieved.
  • the average small-angle grain boundary distance according to a development ⁇ 5 microns. At a low degree of deformation of the X-ray rotary anode, the small angle grain boundary distance is slightly higher. In particular, according to a further development, it is ⁇ 15 ⁇ m, whereby even this higher limit value is even lower than the corresponding value in conventional X-ray rotary anodes produced by powder metallurgy in a composite.
  • the preferential texturing of the ⁇ 110> direction (or ⁇ 101> direction) in directions parallel to the focal plane is less pronounced, in particular less than half as pronounced as the preference Textures of the ⁇ 111> direction and the ⁇ 001> direction perpendicular to the focal plane (this was confirmed by further samples).
  • the focal track has a thickness (measured perpendicular to the focal plane) in the range of 0.5 mm to 1.5 mm. In use, in particular, a thickness in the range of about 1 mm has been proven.
  • the focal length and / or the carrier body has a relative density of ⁇ 96%, in particular of ⁇ 98%, (relative to the theoretical density), which is particularly advantageous with regard to the material properties and the heat conduction.
  • the density measurement is carried out in particular according to DIN ISO 3369.
  • the carrier body specified characteristics in at least a portion of the same.
  • section of the carrier body reference is in particular made to a macroscopic coherent section (ie comprising a plurality of grain boundaries and / or grain boundary sections) of the carrier body. It can also be several, such sections with the claimed properties.
  • the carrier body has over its entire area the respective claimed properties.
  • the carrier body material is formed by a molybdenum alloy designated as TZM, which is specified in the standard ASTM B387-90 for powder metallurgy production.
  • the TZM alloy has a Ti content (Ti: titanium) of 0.40-0.55 wt%, a Zr content of 0.06-0.12 wt% (Zr: zirconium), a C Content of 0.010-0.040 wt% (C: carbon), an O content of less than 0.03 wt% (O: oxygen), and the remaining content (other than impurities) Mo (Mo: molybdenum)
  • the carrier body material is formed by a molybdenum alloy which has an Hf content of 1.0 to 1.3% by weight (Hf: hafnium), a C content of 0.05-0.12% by weight.
  • the section of the carrier body perpendicular to the focal plane has a preferred texturing of the ⁇ 111> direction and the ⁇ 001> direction.
  • the section of the carrier body in directions parallel to the focal plane has a preferred texturing of the ⁇ 101> direction.
  • the specified preferred texturing will be adjusted accordingly in the forging process, as explained above with respect to the focal path. They are reduced again with increasing degree of recrystallization. From these dependencies results in turn for a person skilled in the art (in accordance with what has been explained above with respect to the focal path) how he has to select the parameters of the powder metallurgy production in the respective composition of the carrier body by the specified preferential texturing in at least one section of the carrier body to obtain.
  • the section of the carrier body at room temperature has an elongation at break of ⁇ 2.5%.
  • the section of the carrier body at room temperature has an elongation at break of ⁇ 5%.
  • elongation at break it must again be taken into consideration that with increasing degree of recrystallization of the carrier body, its ductility and thus its elongation at break at room temperature increases. Because of this dependency, the person skilled in the art can accordingly select the parameters of powder metallurgy production (in particular the duration and temperature of the heat treatment (s)), so that the respective value ranges of the elongation at break are achieved.
  • the measurement method associated with the elongation at break is to be carried out in accordance with DIN EN ISO 6892-1, wherein in each case a sample extending radially in the carrier body is used as the measuring sample.
  • method B which is based on the voltage velocity and described in DIN EN ISO 6892-1, should be used.
  • the heat treatment takes place at temperatures below the recrystallization temperature of the focal path, in particular at temperatures in the region of the recrystallization threshold of the focal path.
  • the heat treatment takes place at temperatures below the recrystallization temperature of the carrier body, in particular at temperatures in the region of the recrystallization threshold of the carrier body.
  • the recrystallization temperature depends inter alia on the particular (material) composition and on the degree of deformation of the respective material. The higher the degree of deformation, the lower the recrystallization temperature.
  • the Heat treatment at temperatures ⁇ 1,500 ° C in particular carried out at temperatures in a range of 1300-1500 ° C. These temperatures are particularly suitable for a carrier body made of TZM or from the above specified, concrete composition of Mo, Hf, C and O, in order to achieve the desired properties both in the focal path and in the carrier body.
  • the duration of a heat treatment carried out after the forging process is in particular a few hours, for example in the range of 1-5 hours.
  • FIGS. 1A-1C and 2 identifies criteria by which a non-recrystallized structure, a partially recrystallized structure, and a (complete) recrystallized structure can be distinguished from each other. Furthermore, with reference to these figures, parameters are explained by means of which the degree of recrystallization can be stated. These explanations apply both in relation to the focal track and in relation to the carrier body.
  • Figures 1A-1C In this case, schematically (greatly enlarged) structures are shown, as can be represented for example in an electron micrograph of a suitably prepared ground surface, in particular in the context of an EBSD analysis (EBSD: Electron Backscatter Diffraction).
  • FIG. 2 is, starting from an initial hardness -AH-, which is obtained in the context of powder metallurgy production after the forging process (initial hardness -AH- the forming structure), schematically the dependence of the hardness of the temperature -T- a subsequent heat treatment (stress relief annealing), which is performed over a predetermined period of time -t-, such as over a period of one hour. If the heat treatment is carried out over a longer, predetermined period of time, the shifts in Fig. 2 1 to the left (ie, toward lower temperatures), while it shifts to the right (ie, toward higher temperatures) for a shorter period of time.
  • initial hardness -AH- which is obtained in the context of powder metallurgy production after the forging process
  • stress relief annealing stress relief annealing
  • Fig. 1A is a pure forming structure, as obtained for example after a forging process (which is carried out in the context of powder metallurgical production) is shown.
  • a forging process which is carried out in the context of powder metallurgical production
  • a reforming structure does not have clear grain boundaries around corresponding crystal grains. Rather, only grain boundary sections -2- can be seen, each having an open beginning and / or an open end. In some cases (depending on the degree of deformation during the forging process), sections of the grain boundaries of the original grains of the sintered product can also be identified.
  • form by the forming (forging) Transfers -4- which in the Fig. 1A and 1B represented by the symbol " ⁇ " and new grain boundary sections -2-.
  • the forming structure has a substructure that can be made visible in the context of an EBSD analysis of the respective ground surface when setting a smaller minimum rotation angle.
  • This substructure of the forming structure will be explained below with reference to FIG Fig. 1B explained.
  • the original grain boundaries the grains of the sintered product
  • the intensity and frequency of these typical features of the forming structure depends, inter alia, on the (material) composition and the degree of deformation.
  • small angle grain boundary sections increasingly occur and also the frequency of large angle grain boundary sections increases.
  • a determination of the average grain size, which regularly takes place in the case of uniform structures according to the standard ASTM E 112-96, is not possible because (at least at a minimum angle of rotation of 15 °) only grain boundary sections are recognizable.
  • Recovery processes usually take place in the forming structure, which increase with increasing temperature. For such recovery processes, which can be seen, for example, in the disappearance and / or ordering of dislocations, no activation energy is required. These recovery processes lead to a decrease in hardness. In this area -EH- the recovery operations (range up to T 1 in Fig. 2 ) the hardness decreases continuously with increasing temperature, the slope in this range -EH- being relatively flat (cf. Fig. 2 ). Above a certain temperature -T 1 - the activation energy required for grain regeneration during the recrystallization can be applied. This temperature -T 1 - depends inter alia on the composition and the degree of deformation of the forming structure and on the duration of the heat treatment carried out in each case.
  • the recrystallization region because recrystallization processes occur to a considerable extent within it.
  • the graph goes into an area -EB-, in which it no longer or only very flat drops. Grain growth still occurs in this region, but there is no recrystallization or only a very small amount of recrystallization (in particular of the remaining one percent of the structure).
  • Fig. 1C is an idealized, fully recrystallized structure shown.
  • the grain boundaries of the crystal grains formed by grain remodeling directly adjoin one another.
  • the original forming structure has completely disappeared.
  • Fig. 1C the "ideal case" of a fully recrystallized structure shown, since the grain boundaries each adjacent to each other along their entire extension direction.
  • Fig. 3 is schematically shown the structure of a Röntgenformatanode -10-, which is rotationally symmetrical to a rotational axis of symmetry -12- is formed.
  • the X-ray rotary anode -10- has a plate-shaped carrier body -14- which can be mounted on a corresponding shaft.
  • the focal track 16 covers at least one region of the carrier body 14 which, in use, is traversed by an electron beam. As a rule, the focal track covers a larger area of the carrier body than that of the path of the electron beam.
  • the outer shape and the structure of the X-ray rotary anode -10- can, as is known in the art, deviate from the illustrated X-ray rotary anode.
  • the (macroscopic) portion of the non-recrystallized and / or partially-recrystallized structure can be generally determined by a radial (ie through the axis of rotation symmetry -12- extending ) and is examined perpendicular to the focal plane plane cross-sectional area then, which areas are present in a non-recrystallized and / or in a partially-recrystallized structure.
  • FIGS. 4A to 4D a with a scanning electron microscope feasible EBSD analysis (EBSD: Electron Backscatter Diffraction; German: electron diffraction) explained.
  • EBSD Electron Backscatter Diffraction
  • German electron diffraction
  • a characterization of the respective structure can be carried out on a microscopic level.
  • the fine granularity of the respective structure can be determined, the appearance and extent of substructures can be determined, the proportion of grain grains formed by grain remodeling in a partially recrystallized structure, and preferred texture textures occurring in the structure.
  • a cross-sectional area which extends radially and perpendicular to the focal plane (corresponds to, in FIG Fig. 3 Cross-sectional area shown) produced by the X-ray rotary anode.
  • the preparation of a corresponding ground surface is effected in particular by embedding, grinding, polishing and etching at least a portion of the obtained cross-sectional area of the X-ray rotary anode, the surface subsequently being further ion-polished (for removal of the deformation structure on the surface resulting from the grinding process).
  • the ground surface to be examined can in particular be chosen such that it has a section of the focal path and a section of the carrier body of the X-ray rotary anode, so that both sections can be examined.
  • the measuring arrangement is such that the electron beam impinges on the prepared ground surface at an angle of 20 °.
  • the distance between the electron source (here: field emission cathode) and the sample 16 is 16 mm.
  • the details given in parentheses relate to the types of equipment used by the applicant, and in principle also other types of equipment, which allow the described functions, are used in a corresponding manner.
  • the acceleration voltage is 20 kV
  • a 50-fold magnification is set
  • the pitch of the individual pixels on the sample, which are scanned in succession is 4 ⁇ m.
  • the individual pixels 17 are arranged in equilateral triangles with each other, the side length of a triangle in each case corresponding to the grid spacing -18- of 4 ⁇ m (cf. Fig. 4A ).
  • the information for a single pixel -17- come from a volume of the respective sample, which has a surface with a diameter of 50 nm (nanometers) and a depth of 50 nm.
  • the representation of the information of a pixel is then in the form of a hexagon -19- (in Fig. 4A dashed lines) whose sides each form the mid-perpendicular between the respective pixel -17- and the respective nearest (six) pixels -17-.
  • the examined sample area -21- is in particular 1,700 ⁇ m by 1,700 ⁇ m.
  • Fig. 4B In the present case, in an upper half it comprises a focal section -22- (in cross-section) of approximately 850 by 1,700 ⁇ m 2 and in the lower half a support body section -24- (in cross section) of approximately 850 by 1,700 ⁇ m 2 .
  • the interface -26- (between the focal track and the carrier body) runs parallel to the focal plane and centrally through the examined sample surface -21- (in each case parallel to their sides). Furthermore, it runs parallel to the radial direction -RD- (cf., for example, direction -RD- in FIG Fig. 3, 4B ).
  • the examined sample surface -21- is scanned with a grid of 4 microns.
  • grain boundaries and grain boundary sections with a grain boundary angle greater than or equal to a minimum rotation angle are visualized within the examined sample surface -21- within the scope of the EBSD analysis.
  • a minimum angle of rotation of 15 ° in the scanning electron microscope is set to determine the mean grain boundary distance.
  • the investigated section of the X-ray rotary anode has a (total) degree of deformation of 60%. It should be noted that due to the high hardness of the focal point of the (local) degree of deformation of the focal path is lower per se, while the (local) degree of deformation of the carrier body is at least partially higher.
  • the degree of deformation of the carrier body away from the focal path increases in a direction perpendicular to the focal plane in the downward direction. Accordingly, the result of the investigation depends on the (total) degree of deformation of the examined section as well as on the position of the investigated sample surface -21-. Because of the explained position of the examined sample surface -21- in the region of the interface -26-, both the investigated focal-web section -22- and the investigated carrier body section -24- are less than 1-mm from the interface -26- (this is particularly relevant with respect to the carrier body in which, depending on the height, ie in a direction parallel to the rotational axis of symmetry, different degrees of deformation occur).
  • -21-grain boundaries or grain boundary sections are always determined and displayed between two grid points -17 by the scanning electron microscope if an orientation difference of the respective grid of ⁇ 15 ° is determined between the two grid points -17- (becomes another Minimum rotation angle set, the latter is decisive).
  • the orientation difference used is in each case the smallest angle which is required in order to convert the respective crystal lattices which are present at the respective grid points 17 to be compared into one another. This process is performed at each grid point -17- with respect to all grid points surrounding it (ie, each with respect to six surrounding grid points).
  • Fig. 4A For example, a grain boundary portion -20 is shown.
  • the determination of the average grain boundary distance of the focal-web material parallel to the focal plane is explained.
  • the mean grain boundary distance along the direction -RD- ie along a plane parallel to the focal plane (or to the interface -26- in Fig. 4B ) and substantially radially extending direction.
  • the length of the section becomes Line end evaluated to the first intersection with a line of the grain boundary pattern -32-as a half crystal grain.
  • the frequency of the different distances determined within the focal section -22- (approximately 850 x 1.700 ⁇ m 2 ) is evaluated and then an average of the distances is formed (corresponds to the sum of the detected distances divided by the number of measured distances) ,
  • the method described for determining the mean grain boundary distance is also referred to as "intercept length".
  • a family of -36- (again 98) lines are placed in the grain boundary pattern -32-.
  • the technicallynschar -36- runs parallel to the surface being examined (or cross-sectional area) and the individual lines are each parallel to the direction -ND-.
  • Fig. 4D this is again shown schematically for the section -28-.
  • the evaluation of the distances is carried out accordingly, as explained above. In this way, a measure of the fine grain of the structure formed of (large-angle) grain boundaries and (large-angle) grain boundary portions can be given.
  • the mean grain boundary distance parallel to the focal plane is generally greater than the mean grain boundary distance perpendicular to the focal plane. This effect is due to the force applied perpendicular to the focal plane during the forging process.
  • the determination of the mean (small angle) grain boundary distance of the section of the focal track can be performed in parallel as well as perpendicular to the focal plane by specifying a minimum rotation angle of 5 ° become. From this, in turn, the average small-angle grain boundary distance can be determined according to the formula given above. By specifying a minimum rotation angle of 5 °, the small angle grain boundaries of the substructure (which is present in the deformation structure) are additionally taken into account. In this way, a measure of the fine graininess of the structure formed of (large angle) grain boundaries, (large angle) grain boundary portions and small angle grain boundaries can be given.
  • the degree of recrystallization can be determined on the microscopic level by specifying in a micrograph such as, for example, US Pat Fig. 1A-1C is shown schematically, the area ratio of the, formed by Kornneu Struktur crystal grains (relative to the total area of the examined section) is determined. This determination can in turn be made with a scanning electron microscope in the context of an EBSD analysis.
  • a scanning electron microscope in the context of an EBSD analysis.
  • an angle of ⁇ 15 ° is specified as the minimum rotation angle, so that the course of the large-angle grain boundaries can be seen.
  • the same range can also be examined by specifying a minimum rotation angle of ⁇ 5 ° (or another small value for the minimum rotation angle) to check whether the individual crystal grains are crystal grains formed by grain remodeling act (they have no substructure). Subsequently, the ratio of the area of the crystal grains formed by grain remodeling relative to the entire area under investigation is determined.
  • the degree of recrystallization can also be estimated from the hardness. This can be done, for example, by subjecting a plurality of identically produced samples each time after the forging process to heat treatments at a different time for a predetermined period of time (if appropriate, the duration of the heat treatment may additionally or alternatively be varied). A hardness measurement is then carried out on the samples at the same position (within the sample). Thus, in essence, the course of, in Fig. 2 Traced curve shown and it can be determined in which area of the curve the respective sample is located.
  • the recrystallization threshold -RKS- is preferably used within the range-TB- (the range -TB-in Fig. 2 schematically represented by the dashed circle around the recrystallization threshold -RKS-).
  • Fig. 2 there is a qualitative difference as shown in Fig. 2 is shown schematically by the dashed line.
  • this effect is additionally superimposed by the formation of particles, which can also have an effect on the concrete curve course.
  • the curve is always essentially as it is in Fig. 2 is shown.
  • the starting powders for the carrier body are mixed and the starting powders for the focal path are mixed.
  • the starting powders for the carrier body are chosen such that for the carrier body (apart from impurities) a composition of 0.5 wt.% Ti, 0.08 wt.% Zirconium, 0.01-0.04 wt.% Carbon, less is obtained as 0.03% by weight of oxygen and the remaining portion of molybdenum (after completion of all the heat treatments carried out in the powder metallurgical production) (ie TZM).
  • the starting powders are chosen such that a composition of 10% by weight of rhenium and 90% by weight of tungsten is obtained for the fuel track (apart from impurities).
  • the starting powders are pressed together with 400 tons (equivalent to 4 * 10 5 kg) per X-ray rotary anode.
  • the obtained body is added Temperatures in the range of 2,000 ° C - 2,300 ° C sintered for 2 to 24 hours.
  • the starting body (sintering) obtained after sintering has a relative density of 94%.
  • the starting body obtained after sintering is forged at temperatures in the range of 1300 ° C to 1500 ° C (preferably 1300 ° C), the body after the forging step having a degree of deformation in the range of 20-60% (preferably of 60%).
  • a heat treatment of the body is carried out at temperatures in the range of 1300 ° C to 1500 ° C (preferably 1400 ° C) for 2 to 10 hours.
  • good results can be achieved in each case for different combinations within the respective area.
  • the specified parameters in the pressing step and in the sintering step are less critical for the inventive properties of the focal track (and essentially also for the described advantageous properties of the carrier body), the temperatures in particular during the forging step and in the subsequent heat treatment on the properties of the focal track (in particular on their degree of recrystallization). In particular, particularly good results are obtained at the preferred temperature values at the forging step and at the subsequent heat treatment step (at the 60% preferred degree of deformation).
  • a hardness of 450 HV 30 and, in the case of the carrier body, a hardness of 315 HV 10 could be achieved in the case of the focal track.
  • the hardness measurements are to be carried out at one, extending through the axis of rotation symmetry cross-sectional area.
  • a 0.2% proof stress R p 0.2 of 650 MPa (Mega Pascal) and an elongation at break A of 5% could be obtained at room temperature.
  • a sample extending radially in the carrier body is to be used as a measurement sample.
  • the measuring method to be used is method B, which is based on the voltage velocity and described in DIN EN ISO 6892-1.
  • conventional powders produced by powder metallurgy typically achieve hardnesses of at most 220 HV 10 and also lower yield strengths.
  • the achieved ductilization can be recognized in particular on the basis of the values obtained for the elongation at break A at room temperature.
  • the elongation at break of the (pressed, sintered and forged) carrier body material is typically ⁇ 1%.
  • the focal point was examined at the end of its service life. It was found that cracks are deflected along the grain boundaries of the fine-grained structure and thus change the direction of propagation several times. Due to this crack deflection along the fine-grained structure, crack propagation deep into the focal track is avoided. It was also possible to observe a uniformly distributed crack pattern with uniformly formed cracks on the surface of the focal point at the end of its service life. In contrast, at comparative X-ray rotary anodes, in which the focal track was produced by vacuum plasma spraying, the crystals of the track are stalk-shaped and aligned perpendicular to the focal plane. As a result, a crack spreads along the grain boundaries deep into the focal path (and eventually down to the support body).
  • an X-ray rotary anode was used, as described above with reference to FIGS FIGS. 4A to 4D is prepared as prepared sample to be examined.
  • the X-ray rotary anode was designed according to the invention.
  • the hearth had (apart from impurities) a composition of 90 wt% tungsten and 10 wt% rhenium, while the support body (apart from impurities) had a composition of 0.5 wt% Ti, 0.08 wt% zirconium , 0.01-0.04 wt% carbon, less than 0.03 wt% oxygen and the remaining portion of molybdenum.
  • the measuring arrangement corresponds to the arrangement explained above.
  • the above with reference to the FIGS. 4A to 4D used settings, provided that they are applicable or to determine the texture.
  • the inverse pole figures obtained as part of the EBSD analysis of the focal track are in the Figs. 5A-5C shown.
  • the focal track with respect to the focal track, the macroscopic, mutually perpendicular directions -ND-, which is perpendicular to the focal plane in the respective investigated area, -RD-, which runs substantially radially and parallel to the focal plane and TD-, which is tangent and parallel to the focal plane, defined (these directions are for illustration in FIG Fig. 3 shown).
  • Fig. 5A is the inverse pole figure of the focal path in the direction -ND-
  • Fig. 5B is the inverse pole figure towards -RD-
  • Fig. 5C the inverse pole figure is shown in the direction -TD-.
  • the pronounced preferential texturing of the ⁇ 111> direction and the ⁇ 001> direction along the direction -ND- can be recognized.
  • the Figures 5B and 5C to recognize the (less strong) pronounced preferential texturing of the ⁇ 101> direction along the directions -RD and -TD-.

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  • Powder Metallurgy (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
EP16001702.6A 2011-01-19 2012-01-17 Anode rotative de tube a rayons x Active EP3109889B1 (fr)

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ATGM34/2011U AT12494U9 (de) 2011-01-19 2011-01-19 Röntgendrehanode
EP12709493.6A EP2666180B1 (fr) 2011-01-19 2012-01-17 Anode tournante pour tube à rayons x

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JP (1) JP5984846B2 (fr)
KR (1) KR101788907B1 (fr)
CN (1) CN103329239B (fr)
AT (1) AT12494U9 (fr)
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DE102013219123A1 (de) 2013-09-24 2015-03-26 Siemens Aktiengesellschaft Drehanodenanordnung
US9992917B2 (en) 2014-03-10 2018-06-05 Vulcan GMS 3-D printing method for producing tungsten-based shielding parts
CN104062311B (zh) * 2014-05-23 2017-01-18 武汉钢铁(集团)公司 采用倾斜并旋转试样测量反极图的方法
DE102014210216A1 (de) 2014-05-28 2015-12-03 Siemens Aktiengesellschaft Verfahren zum Herstellen eines Bauteils
CN106531599B (zh) * 2016-10-28 2018-04-17 安泰天龙钨钼科技有限公司 一种x射线管用钨铼‑钼合金旋转阳极靶材及其制备方法
KR101902010B1 (ko) * 2016-12-09 2018-10-18 경북대학교 산학협력단 엑스선관 타겟, 이를 구비한 엑스선관, 및 상기 엑스선관 타겟의 제조 방법
EP3766613B1 (fr) * 2018-03-16 2024-06-26 Sumitomo Electric Hardmetal Corp. Outil de coupe à surface revêtue
EP3629361B1 (fr) * 2018-09-26 2020-10-28 Siemens Healthcare GmbH Émetteur de rayons x, emploi d'un émetteur de rayons x et procédé de fabrication d'un émetteur de rayons x
KR102236293B1 (ko) * 2019-03-27 2021-04-05 주식회사 동남케이티씨 엑스선관용 회전양극타겟 제작방법 및 회전양극타겟
CN110293223B (zh) * 2019-07-23 2022-03-22 金堆城钼业股份有限公司 一种蝶形钼钨双金属复合旋转靶的制备方法
US11043352B1 (en) 2019-12-20 2021-06-22 Varex Imaging Corporation Aligned grain structure targets, systems, and methods of forming
CN115917025A (zh) * 2021-04-06 2023-04-04 联合材料公司 钨材料
EP4386807A1 (fr) 2022-12-13 2024-06-19 Plansee SE Anode tournante pour rayons x comportant deux structures de grains différentes dans le revêtement de la bande de combustion

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US4109058A (en) * 1976-05-03 1978-08-22 General Electric Company X-ray tube anode with alloyed surface and method of making the same
US6487275B1 (en) 1994-03-28 2002-11-26 Hitachi, Ltd. Anode target for X-ray tube and X-ray tube therewith
US20050135959A1 (en) 2003-12-22 2005-06-23 General Electric Company Nano particle-reinforced Mo alloys for x-ray targets and method to make
WO2009022292A2 (fr) * 2007-08-16 2009-02-19 Philips Intellectual Property & Standards Gmbh Agencement hybride d'une structure de disque d'anode pour des configurations de tube à rayons x à puissance élevée du type anode rotative

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JP5984846B2 (ja) 2016-09-06
WO2012097393A1 (fr) 2012-07-26
AT12494U9 (de) 2012-09-15
JP2014506711A (ja) 2014-03-17
EP3109889B1 (fr) 2018-05-16
AT12494U1 (de) 2012-06-15
CN103329239B (zh) 2016-10-12
KR20140020850A (ko) 2014-02-19
KR101788907B1 (ko) 2017-10-20
US20160254115A1 (en) 2016-09-01
US9368318B2 (en) 2016-06-14
US20130308758A1 (en) 2013-11-21
US9767983B2 (en) 2017-09-19
ES2613816T3 (es) 2017-05-26
EP2666180A1 (fr) 2013-11-27
CN103329239A (zh) 2013-09-25
EP2666180B1 (fr) 2016-11-30

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