JP2017139238A - Transmission type target, method of manufacturing transmission type target, radiation generating tube, radiation generating device with radiation generating tube, and radiographic device with the radiation generating device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a transmission type target that suppresses composition variation accompanying an operation history of the transmission type target and suppresses radiation output variation over a long period of time in a transmission type target with diamond base material as transmission type base material.SOLUTION: A transmission type target includes: a target layer containing metal carbide in which X ray occurs by irradiation of an electron; and diamond base material that supports the target layer.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a radiation generation apparatus that emits X-rays belonging to a wavelength range of 1 pm to 10 nm that can be applied to medical devices, non-destructive inspection apparatuses, and the like. In particular, the present invention relates to a transmission target including a target layer and a diamond base material that supports the target layer. Furthermore, the present invention relates to a radiation generating tube including the transmission target, further to a radiation generating device including the radiation generating tube, and further to a radiation imaging apparatus including the radiation generating device.

  Due to changes in social conditions such as the improvement of home medical care systems and the expansion of emergency medical treatment, there is an increasing need for portable, compact and lightweight medical modalities. In recent years, various medical modalities have been developed to meet such needs, coupled with the development of analytical and diagnostic techniques in the medical field. Conventionally, a radiographic apparatus equipped with a radiation generation apparatus has been mainly installed in a hospital, a medical examination institution, or the like because of the scale of the apparatus. Conventionally, a medical modality that is fixedly installed is configured to regularly set and use an operation period and a rest period including maintenance.

  Even in a radiography apparatus equipped with such a radiation generator, it is possible to improve the operating rate of the apparatus by improving durability and reducing maintenance, and can be applied to home medical care or emergency medical care such as disasters and accidents. There is a need for a possible medical modality.

  One of the main factors that determine the durability of a radiation generator is the durability of a target that is a source of radiation such as X-rays. The target generally has a laminated structure, but it has been known that securing “adhesion” between layers of the target for a long period of time is important for improving the durability of the target.

  In a radiation generation apparatus that generates radiation by irradiating a target with an electron beam, the “radiation generation efficiency” of the target is less than 1%, so that most of the energy input to the target is converted into heat. If the heat generated by the target is not sufficiently "radiated" to the outside of the target, there will be problems of "adhesion" such as modification of the material that constitutes the target and film peeling due to stress generated between the layer structures. There was a case.

  As a method for improving the "radiation generation efficiency", the target is a transmission target composed of a target layer in the form of a thin film containing heavy metal and a base material that transmits radiation and supports the target layer. This is well known. Patent Document 1 discloses a rotating anode transmission type target in which the “radiation generation efficiency” is increased by 1.5 times or more compared to a conventional rotating anode reflection type target.

  As a method for promoting “heat dissipation” from the target to the outside, it is known to apply diamond to a base material that supports a target layer of a transmission target. Patent Document 2 discloses that diamond is used as a base material for supporting a target layer made of tungsten, thereby improving heat dissipation and realizing a fine focus. Diamond has a high heat resistance, a high thermal conductivity, and a high radiation transmittance, and therefore is a suitable material for the support substrate of the transmission target. The transmission target of the present invention also employs a configuration in which diamond is applied as a base material that supports the target layer.

JP-T 2009-545840 Special table 2003-505845 gazette US Pat. No. 7,359,487

“Carbon self-diffusion in tungsten carbide”, Buhsmer, C .; P. Crayton, P .; H. J. et al. Mater. Sci. 1971 vol. 6 page. 981-988

  Patent Document 2 discloses that a non-disclosure adhesion promoting layer is disposed between a target layer and a diamond base material to improve the adhesion between the target layer and the diamond base material. However, in the radiation generating apparatus to which the transmission type target provided with the adhesion promoting layer as disclosed in Patent Document 2 is applied, the radiation emission characteristics may vary depending on the driving history. As a result of intensive studies by the present inventors, it has been found that the radiation output fluctuation of such a radiation generating device is derived from a change in the composition of the target layer of the transmission target. More specifically, the fact that the carbon derived from the diamond base material that supports the target layer diffuses into the target layer and causes a change in the composition of the target layer is a cause of the radiation output fluctuation. The present inventors have found out.

  Next, the present inventors will explain the analysis results obtained by analyzing the composition change of the target layer using a diffusion equation as a carbon transport problem.

  First, the calculation model will be described. The calculation model was a laminated target 90 in which a target layer 52 made of pure metal tungsten was formed on a diamond substrate 51. This schematic cross-sectional view is shown in FIG. FIG. 8C is a partially enlarged view in which a range 54 from the interface 57 between the diamond substrate 51 and the target layer 52 to the upper surface 58 of the target layer 52 in FIG. 8B is cut out. The arrival position 56 of carbon derived from the material 51 and the carbon diffusion distance Ld (t) are shown. In the calculation, the drive condition is a pulse drive with an average duty ratio of 1/1000 that is exposed for 0.1 second every 100 seconds, and the average operation of a typical target is controlled by controlling the current density of incident electrons. The temperature was set to 800 ° C. and 1000 ° C.

  FIG. 8A shows the driving time dependence of the carbon diffusion distance Ld in the target layer 52 of the transmission target 90 obtained as a result. The vertical axis of the graph of FIG. 8A indicates the diffusion distance Ld of carbon diffused in the target layer 52 with reference to the interface between the target layer 52 and the diamond substrate 51. In addition, the horizontal axis of the graph of FIG. 8A shows the drive time (hour) and the cumulative drive count (count) as the first horizontal axis and the second horizontal axis, respectively.

  The two plots in FIG. 8A correspond to temperature conditions of 800 ° C. (dashed line) and 1000 ° C. (dotted line) in order from the bottom. Both plots increase by 0.5 power with respect to the driving time t, and it can be seen that carbon diffuses from the interface 57 toward the upper surface 58 of the target layer 52 as the driving time elapses.

In the trial calculation of the diffusion distance Ld of carbon, the Arrhenius rule D (T) = D0 × exp (−Qx / RT) of the diffusion coefficient and the steady solution Ld (t) = 2 × (D (T) × t of the diffusion distance It was obtained by substituting the diffusion constant D0 (m ² / sec) described in Non-Patent Document 1 and the activation energy Qx (kJ / mol) of the diffusion coefficient for ^0.5 . Where T is a thermodynamic temperature (K), t is a driving time (sec), and R is a gas constant (kJ / K / mol).

Non-Patent Document 1 describes the diffusion constant D0 (m ² / sec) and the activation energy Qx (kJ / mol) of the diffusion coefficient obtained based on the measured data of the diffusion phenomenon of carbon in tungsten carbide. Each is specifically disclosed. According to the algebraic description of each of D (T) and Ld (t), the carbon diffusion distance Ld at an operating temperature of 800 ° C. or higher and 1000 ° C. or lower is located between the two plots in FIG. Is clear.

  Next, the layer thickness of the target layer included in the stacked target will be described. In general, the thickness of the target layer of the reflective target is selected in the range of 1 μm to 1 mm. The lower limit of the target layer thickness of the reflective target is determined in consideration of the electron penetration depth Dp defined by the tube voltage and the layer density of the target layer. Further, the upper limit of the layer thickness of the target layer of the reflective target is determined in consideration of heat transfer in the layer thickness direction and the layer surface direction.

  On the other hand, the layer thickness of the transmission target can be selected in the range of 1 μm or more and 15 μm or less. In general, the lower limit of the layer thickness of the transmissive target in the range of 1 μm to 9 μm is determined for the same reason as that of the reflective target. On the other hand, the upper limit of the layer thickness of the transmission target is determined in consideration of the radiation attenuation rate of the target layer in addition to the heat transfer property, and is limited to a range lower than the layer thickness of the target layer of the reflection target. .

  From the graph of FIG. 8A, the carbon diffusion distance Ld is 7.9 μm to 10.8 μm when the exposure driving is performed 104 times in total at an operating temperature of 800 ° C. to 1000 ° C. Can be read.

  In the reflection type target, for example, by providing the target layer 52 having a thickness of 100 μm, as shown in FIG. 8D, carbon reaches the range of 89.2 μm to 92.1 μm from the electron incident surface 58 side. It is possible to ensure the distance Lr not to be performed on the radiation emitting surface side (= electron incident surface 58 side) of the target layer 52. This distance Lr of 89.2 μm to 92.1 μm is sufficiently larger than the thickness of 6 μm to 7 μm, which is the electron penetration depth Dp of 100 keV incident electrons with respect to tungsten. Since it is clear that the “radiation emission depth” in the target layer 52 that contributes to the generation of radiation is a distance more limited than the “electron penetration depth Dp”, in the reflective target, the diffusion of carbon A “radiation emission depth” that is not affected can be secured in the target layer 52.

  On the other hand, in the transmissive target, even if the transmissive target includes the target layer 52 having a thickness of 8 μm, as shown in FIG. 8E, the “electron penetration depth Dp” from the electron incident surface 58 side. Carbon reaches the range of. More specifically, when the target layer 52 has a thickness lower than 14 μm, carbon reaches the range of the “electron penetration depth Dp” from the electron incident surface 58 side. This means that the composition of the target layer 52 is changed by driving the radiation generator.

  Furthermore, in the transmission type target, since the radiation emitted from the support base 51 side of the target layer 52 is used, the available radiation forward (that is, the side surface direction opposite to the support surface of the target layer 52) A region having a high transmission probability corresponds to the deep side of the electron penetration depth Dp. Also in this respect, it can be said that the transmission type target is more susceptible to the influence of carbon diffusion in the radiation output operation than the reflection type target.

  As described above, there is a problem inherent to the transmission type in which the carbon diffusion derived from the diamond that is the support base material and the radiation attenuation rate of the target layer itself conflict in determining the layer thickness of the target layer. .

  In addition, although the laminated structure in which the carbon supply source is a diamond base material has been described as a calculation model, the same problem occurs even when a metal carbide is sandwiched between the diamond base material and the target layer.

  Therefore, the present invention maintains a merit that “radiation generation efficiency” and “heat dissipation” are good in a transmission type target including a diamond base material as a transmission base material, and further, in the drive history of the target layer. An object of the present invention is to provide a highly reliable transmission target in which the accompanying composition fluctuation is suppressed. Furthermore, an object of the present invention is to provide a highly reliable radiation generating apparatus and a radiation imaging apparatus in which fluctuations associated with a driving time history of radiation output are suppressed.

  A first aspect of the present invention includes a transmission type target comprising: a target layer containing a metal carbide that generates X-rays upon electron irradiation; and a diamond base material that supports the target layer.

  The second aspect of the present invention is an X-ray generation target comprising a target layer containing a metal carbide that generates X-rays upon electron irradiation, and a diamond substrate that supports the target layer, The metal carbide includes a transmission target characterized by being located in a region where X-rays are generated.

Furthermore, the third of the present invention is a method for manufacturing a transmission target comprising a metal carbide layer as a target layer, the step of preparing a diamond substrate,
A film forming step of forming a metal layer made of a metal selected from at least one of molybdenum, tantalum, and tungsten on one surface of the diamond substrate;
A step of heating a diamond base material provided with the metal layer, diffusing carbon from the diamond base material to the metal layer, and forming a metal carbide layer containing the metal carbide to form a target layer; and The manufacturing method of the transmission type target characterized by providing is included.

Furthermore, a fourth aspect of the present invention is a method for manufacturing a transmission target comprising a metal carbide layer as a target layer, the step of preparing a diamond substrate,
Forming a metal carbide layer made of at least one selected from molybdenum, tantalum, and tungsten and carbon and forming a target layer on one surface of the diamond base material. And a manufacturing method of the transmission type target.

  The transmission type target of the present invention suppresses the diffusion of carbon derived from the diamond base material into the target layer even when it receives an operation history at a high temperature, thereby suppressing the composition variation of the target layer. As a result, it is possible to suppress variations in the output or radiation quality of the radiation emitted from the target layer. Furthermore, the reliability relating to the durability can be improved by using the radiation generating tube including the transmission target of the present invention, the radiation generating device including the radiation generating tube, and the radiation imaging apparatus. It becomes.

Schematic sectional view showing a basic configuration example (a) and an operating state (b) of a transmission type target of the present invention Schematic sectional view showing a configuration example of a radiation generating tube provided with a transmission type target of the present invention Configuration diagram of radiation generating apparatus and radiation imaging apparatus including the radiation generating tube of the present invention Examples (a) to (c) of a method for producing a transmission type target of the present invention Explanatory drawing which shows embodiment provided with the modification of the layer structure of the transmission type target of this invention X-ray diffraction chart (upper plot) shown by the target layer of the transmission target described in Example 1, and X-ray diffraction chart (lower plot) shown by the metal layer of the reference example Explanatory drawing of the stability evaluation system of the radiation output of the radiation generator of Example 1 and 2 (A) Dependence of drive time on diffusion distance of carbon in tungsten, (b) Calculation model of (a), (c) Partial enlarged view of (b), (d) Influence of carbon diffusion distance of reflective target Explanatory drawing showing, (e) Explanatory drawing showing the influence of transmission type target and carbon diffusion distance

  Exemplary embodiments of a target structure of the present invention, a radiation generation apparatus including the target structure, and a radiation imaging apparatus will be described below in detail with reference to the drawings. However, the materials, dimensions, shapes, relative arrangements, and the like of the configurations described in the following embodiments are not intended to limit the scope of the present invention unless otherwise specified.

  First, a basic configuration example of a radiation generating tube to which the transmission target of the present invention can be applied will be described with reference to FIG.

  In the present embodiment, the radiation generating tube 1 includes a transmission type target 9 including a target layer 42 and a diamond base material 41, and an electron emission source 3 having an electron emission unit 2 so as to be separated from and opposed to the target layer 42. And the envelope 6 whose internal space 13 is decompressed. At least the electron emission part 2 and the target layer 42 are accommodated in the internal space 13 or are disposed on the inner surface of the envelope 6 so as to face the internal space 13 and are opposed to each other. .

  The electron emission source 3 is electrically connected to a drive circuit (not shown) disposed outside the envelope 6. The electron emission source 3 can be configured to include a current introduction terminal 4 for electrical connection with such a drive circuit.

  The electron emission source 3 is connected to a cathode member made of a conductive material (not shown). A structure composed of the electron emission source 3 and the cathode member is a cathode of the radiation generating tube 1 in the present embodiment. The cathode is regulated to the cathode potential. The cathode member may be disposed inside the envelope 6 or may be a structural member that constitutes a portion of the envelope 6.

  The electron emission source 3 only needs to be capable of electrically controlling the amount of electron emission by a drive circuit (not shown), and any type of electron emission element can be provided as the electron emission unit 2. As the electron emission part 2, a cold cathode type electron emission element such as Spindt type, SCE type, MIM type, CNT type, or a hot cathode type electron emission element of filament type or impregnation type may be applied. Is possible. The electron emission source 3 can include a focusing grid (not shown).

  The transmission type target 9 is electrically connected to an anode potential defining means (not shown) disposed outside the envelope 6. In the present embodiment, the structure composed of the transmission target 9 and the anode member is the anode of the radiation generating tube 1.

  Further, the anode member may be disposed inside the envelope 6 in the same manner as the cathode member, or may be a structural member constituting a portion of the envelope 6.

  The envelope 6 constitutes the radiation generating tube 1 using the internal space 13 as a vacuum container whose vacuum is reduced. The envelope 6 is composed of a member having an atmospheric pressure strength for withstanding a differential pressure between the outside and the inside of the vacuum vessel and maintaining a structure, and an airtightness for maintaining a predetermined degree of vacuum. It is preferable.

The degree of vacuum of the internal space 13 can be appropriately selected according to the type of the electron emission source 3, but the range of 1 × 10 ⁻⁴ Pa to 1 × 10 ⁻⁸ Pa is high in the electron emission source 3. It is preferable from the viewpoint of lifetime. Depending on the type of the electron emission source 3 or the required degree of vacuum, a getter (not shown) can be arranged in the envelope 6 or in a space communicating with the internal space.

  The envelope 6 is an embodiment in which the electron emission source 3 and the transmission target 9 are connected to the envelope 6 for the purpose of defining the distance between the electron emission portion 2 and the target layer 42. It is also possible. In the present embodiment, the envelope 6 desirably includes a tubular member having electrical insulation for insulating a high voltage applied between the electron emission unit 2 and the target layer 42. Such a tubular member can be made of an insulating material such as an inorganic oxide such as ceramic or glass, an inorganic nitride, or an inorganic boride.

  The cathode member and the anode member are made of a conductive material for the potential regulating function, and a metal material can be applied. In addition, it is preferable to select a metal material for the cathode member and the anode member from the viewpoint of heat resistance in view of the operating temperature of the radiation generating tube 1 or matching of the linear expansion coefficient with the insulating tubular member described above. For example, Kovar (KOVAR, CRS HOLDINGS, INC. US trademark, Ni-Co-Fe alloy), Monel (Special Metals Corporation, HUNTINGTON ALLOYS CORPORATION, Ni-Cu-Fe alloy), stainless steel, etc. Metal materials can be used.

  Further, as shown in FIG. 2, the radiation generating tube 1 is configured to include a shield 7 that limits the emission direction of the radiation generated from the transmission target 9, that is, the shield 7 in the vicinity of the radiation generation source. It is possible to provide a light radiation generating device by adopting a form in which they are arranged in an integrated manner. The shield 7 includes a rear shield 40 disposed on the electron emission source 3 side with respect to the transmission target 9, and a front shield 46 positioned on the opposite side to the electron emission source 3 side with respect to the transmission target 9. Can be configured.

  Next, the radiation generator provided with the transmission type target of the present invention will be described with reference to FIG.

  As shown in FIG. 3, the radiation generation apparatus 20 includes a drive circuit 15 electrically connected to the radiation generation tube 1 and the radiation generation tube 1. In the present embodiment, the drive circuit 15 determines the amount of electrons emitted from the electron beam 5 emitted from the electron emission source 3 and the anode potential regulating means and cathode potential regulating means for regulating the anode and cathode of the radiation generating tube 1. An electron gun drive circuit to be controlled. Furthermore, the radiation generation apparatus 20 can be configured to include a storage container 16 that stores the radiation generation tube 1 and the drive circuit 15 in the internal space 43 thereof.

  The storage container 16 can have a form in which the internal space 43 is filled with an insulating liquid 14 (not shown) such as silicone oil or perfluoro oil. By adopting such a form, the radiation generator can be formed. Thus, it is possible to improve the heat dissipation performance and the pressure resistance.

  Further, the storage container 16 is provided with a transmission window 17 on the side facing the transmission target 9, so that the radiation can be efficiently emitted to the outside of the radiation generator 20.

  As the anode potential regulating means, a voltage source that outputs a positive acceleration voltage Va of about several tens of kV to 200 kV with respect to the cathode can be applied.

  The anode-side output potential of the anode potential regulating means can be selected according to the presence or absence of contact between the subject and the anode member, the distance, and the like. Specifically, the ground potential (anode ground), + 1/2 × Va (middle point grounding), + Va (cathode grounding), or the like can be used.

  Next, a radiographic apparatus equipped with the radiation generating apparatus of the present invention will be described with reference to FIG.

  As shown in FIG. 3, the radiation imaging apparatus 60 of the present invention includes a radiation detector 47 that detects radiation emitted from the radiation generation apparatus 20 and transmitted through the subject 25. The radiation imaging apparatus 60 may be configured to further include a control unit 50 that controls the drive circuit 15 included in the radiation generation apparatus 20 and receives a radiation image from the radiation detector 47.

  The control unit 50 further has a function of controlling the radiation detector 47, a function of displaying a radiographic image to the operator, a function of receiving an operation input from the operator, and a function of stopping the radiation generator based on an emergency stop command. It is also possible to adopt a form including at least one of the above.

  Next, the structure of the transmission target, which is a feature of the present invention, will be described with reference to FIGS. 1 (a) and 1 (b).

  The transmissive target 9 includes a target layer 42 containing a target metal and a diamond base material 41 that supports the target layer 42.

  The target layer 42 contains a metal carbide of a target metal selected from at least one selected from the group of molybdenum (Mo), tantalum (Ta), and tungsten (W), distributed in the layer thickness direction. It is a feature. The first feature is that carbon is contained in the target layer 42 “as carbide” in the target layer 42, and the second feature is that the carbon contained in the metal carbide is “the layer thickness of the target layer 42. It is contained uniformly in the direction.

  The technical significance of “the target layer 42 contains carbon as a carbide” as the first feature will be described in detail below.

  Diamond has unique properties derived from structures with strong sp3 bonds and high order. Among the unique properties of diamond, high heat resistance (melting point 1600 ° C. or higher), high thermal conductivity (600 to 2000 W / m / K), high radiation transparency (light element, atomic number 6) are transmissive targets This is a particularly excellent feature as a supporting substrate. On the other hand, diamond has low wettability with the molten metal and low affinity with the target metal as can be seen from the mismatch in the linear expansion coefficient with the solid metal. Ensuring the adhesion between the target layer 42 and the diamond base material 41 was an issue for improving the reliability of the transmission target 9. The carbon contained in the target layer 42 is expected to play a bridging role at the interface between the target layer 42 and the diamond base material 41.

  However, since carbon allotropes other than diamond and carbon compounds as hydrocarbons are thermally unstable, the role of adhesion between the target layer 42 and the diamond substrate 41 is determined at the operating temperature of the transmission target 9. Difficult to achieve sustainably and stably.

Molybdenum, tantalum, and tungsten contained in the target layer 42 of the present invention are metals in which the standard free energy of formation of carbides is negative, and these metal carbides are thermally stable. Molybdenum carbide, tantalum carbide, and tungsten carbide each have a high melting point (Mo ₂ C: 2692 ° C., TaC: 3880 ° C., WC: 2870 ° C.). Constructing the target layer 42 from at least one of molybdenum carbide, tantalum carbide, and tungsten carbide contributes to the realization of the transmission target 9 having high heat resistance.

  Furthermore, the fact that the target layer 42 contains carbon as a metal carbide means that the above-described metal carbide has a crystal structure, and therefore carbon atoms are distributed at a predetermined spatial density derived from the lattice density. When the target layer 42 contains carbon at a predetermined spatial density, the interface between the target layer 42 and the diamond base material 41 forms a strong laminated interface derived from the carbon-carbon interatomic bond. It becomes possible.

  Next, the technical significance of the second feature “carbon is uniformly contained as a metal carbide in the thickness direction of the target layer 42” will be described in detail below.

  By providing the second feature, even when the transmission target 9 is placed in a high temperature environment during the operation of the radiation generating tube 1, “carbon diffusion from the diamond base material 41 to the target layer 42”, “ It has the effect of suppressing “carbon diffusion in the target layer 42” and exhibits the effect of suppressing the composition variation of the target layer 42.

  That is, according to the second feature, prior to the radiation output operation of the transmissive target 9, carbon is uniformly contained in the thickness direction of the target layer 42 in advance as a metal carbide, whereby the diamond base material 41 and the target layer 42. The effect of “suppressing the concentration gradient of carbon between layers” is exhibited, and the effect of suppressing “carbon diffusion from the diamond base material 41 to the target layer 42” is brought about.

  Further, according to the second feature, prior to the radiation output operation, the transmissive target 9 contains carbon as a metal carbide in the layer thickness direction of the target layer 42 in advance, so that “the carbon in the layer” The effect of “suppressing the concentration gradient” is expressed, and the effect of suppressing “carbon diffusion in the target layer 42” is brought about.

  As described above, the target layer 42 having the first and second characteristics provides the effect of stabilizing the composition of the target layer 42. It is possible to stabilize the output operation of the radiation generating tube 1 and the radiation generating apparatus 20 provided with the transmission target 42 for a long period of time. This technical significance is extremely important in the transmission type target 9 in which it is difficult to obtain a sufficiently large layer thickness compared to the carbon diffusion length Ld.

  In addition, carbon is contained uniformly in the layer thickness direction of the target layer 42, which is the second feature of the present invention, that carbon is contained as a metal carbide in an arbitrary region in the layer thickness direction of the target layer 42. Means that

  Therefore, the uniform carbon content in the thickness direction of the target layer 42 is not necessarily limited to a form having a constant carbon concentration in the thickness direction of the target layer. Other embodiments include a form having a predetermined carbon concentration distribution within a range in which the effect of suppressing the composition variation of the target layer 42 can be obtained. Specifically, a form in which the maximum and minimum atomic concentration ratios of the carbon concentration satisfy one digit or less in the 90% range in the layer thickness direction of the target layer 42 is included as another embodiment of the present invention.

  All of molybdenum, tantalum, and tungsten contained in the target layer 42 belong to a transition metal, and therefore can have a carbide crystal structure exhibiting a plurality of carbon numbers. Is a stable crystal structure. Molybdenum, tantalum, and tungsten are hexagonal di-molybdenum carbide, cubic tantalum carbide, and hexagonal tungsten carbide, respectively. Is the most thermally stable structure.

Therefore, when molybdenum is contained as a target metal, the concentration of metal carbide in the target layer 42 is dimolybdenum carbide concentration [Mo ₂ C] (atm%)> monomolybdenum carbide concentration [MoC] (atm%). This is preferable in terms of suppressing changes in the structure of the target layer. Therefore, if the target layer 42 is composed of a single layer of dimolybdenum carbide (Mo ₂ C), which is the most stable structure, it is possible to provide a transmission type target with even better heat resistance.

Similarly, when tantalum is contained as the target metal, the concentration of metal carbide in the target layer 42 is as follows: monotantalum carbide concentration [TaC] (atm%)> ditantalum carbide concentration [Ta ₂ C] (atm%) It is preferable that Therefore, if the target layer 42 is formed from a single layer of tantalum carbide (TaC), which is the most stable structure, it is possible to provide a transmission type target with even better heat resistance.

Similarly, when tungsten is contained as the target metal, the concentration of metal carbide in the target layer 42 is as follows: monotungsten carbide concentration [WC] (atm%)> ditungsten carbide concentration [W ₂ C] (atm %). Therefore, if the target layer 42 is formed from a single layer of tungsten carbide (WC), which is the most stable structure, it is possible to provide a transmission type target with even better heat resistance.

  The target layer 42 has a layer thickness of about 1 to 1.5 times Dp with reference to the electron penetration depth Dp defined by the tube voltage Va of the radiation generating tube. It is possible to achieve both suppression of electron damage and the forward transmission of radiation generated in the target layer. Since the range of the electron penetration depth Dp is a heat generating portion of the transmission type target 9, the metal carbide is contained in the depth region from the surface of the target layer 42 to the electron penetration depth Dp. It is preferable from the viewpoint of heat resistance of the layer 42 and suppression of composition variation.

In general, the electron penetration depth Dp is determined by the incident energy Ep (eV), that is, the tube voltage Va (V), and the density of the target layer. In the present invention, the electron penetration depth Dp (m) is defined by the following general formula 1 showing good agreement with the actual measurement with the incident energy Ep (= Va) in the range of 1 × 10 ⁴ V to 1 × 10 ⁶ V.
Dp = 6.67 × 10 ⁻¹⁰ × Va ^1.6 / ρ (Formula 1)

Where Va is the tube voltage (V), and ρ is the density of the target layer (kg / m ³ ). The identification of the density of the target layer may be determined by weighing and layer thickness measurement, but the method of determining by the Rutherford backscattering analysis method (RBS method) is preferable as a method for measuring the density of the thin film.

  As a specific layer thickness of the target layer 42, a layer thickness of 0.1 to several tens of micrometers is preferable in that it is possible to further suppress delamination due to stress.

  In addition, the target layer 42 may have a composition containing a target metal and another metal, respectively, but by forming a single composition made of a carbide of a single target metal, in FIG. It is preferable in that the spectrum of the characteristic X-ray contained in the emitted radiation 11 can be sharpened. Since the metal carbide contained in the target layer 42 has a crystal structure, pure metal molybdenum, X-ray diffraction (XRD), high-resolution image of a transmission electron microscope (TEM), electron diffraction (ED), etc. Tantalum and tungsten have different intrinsic crystal structures.

  Next, the diamond base material with which the transmission type target of this invention is provided is demonstrated using Fig.1 (a), (b).

  By setting the base material thickness of the diamond base material 41 to 0.1 mm to 10 mm, it is possible to achieve both thermal conductivity in the base material surface direction and radiation transparency. The diamond base material 41 may be either a single crystal diamond or a polycrystalline diamond, but from the viewpoint of thermal conductivity, the single crystal diamond is a preferred form. Furthermore, since the diamond base material 41 contains nitrogen in the range of 2 ppm to 800 ppm, the impact resistance is improved, so the portability of the radiation generating apparatus to which the transmission target 9 of the present invention can be applied is improved. It is a preferable form from the possible point.

  Next, a method for forming the transmission type target 9 of the present invention will be described with reference to FIGS.

  As shown in FIGS. 4 (a-1) and 4 (a-2), the first method of forming the transmission target 9 is to form a metal carbide layer on the diamond base material 41, and to form the target layer 42. It is a method. As a method for forming the metal carbide layer, any film forming method including chemical vapor deposition (CVD), physical vapor deposition, thermal spraying, and the like can be employed. As shown in FIGS. 4 (b-1) to 4 (b-4), the second method of forming the transmission target 9 is to form a laminate by forming a metal layer 43 on the diamond base material 41. Then, such a laminate is heated in a temperature range of 1000 ° C. or higher and 2000 ° C. or lower in a reduced pressure atmosphere, a deoxygenated atmosphere, or an inert gas atmosphere. By such a method comprising the metal layer forming step and the carbonization step, carbon derived from the diamond base material 41 can be diffused into the metal layer 43 and the metal contained in the metal layer 43 can be carbonized. The above heating temperature is more preferably set to a temperature range of 1500 ° C. or more and 2000 ° C. or less from the viewpoint of shortening the carbonization step.

  Moreover, as a modification of the first forming method and the second forming method, as shown in FIGS. 4C-1 to 4C-4, a substrate made of a material having a low thermophysical temperature. Alternatively, after the metal carbide layer 42 or the metal layer is formed on the substrate 44 and the diamond layer 41 is formed by the CVD method or the like, the substrate 44 may be selectively removed. As the thermophysical temperature of the substrate 44, a melting point or a decomposition temperature is adopted, and these are lower than the target layer 42 or the diamond base material 41, so that the transmission target forming method of the present embodiment can be realized. .

  Next, with reference to FIGS. 5A to 5C, a modified example of the transmission target 9 of the present invention provided with a potential regulating means for regulating the potential of the target layer 42 will be described.

  The target layer 42 is preferably applied with a high voltage of about several tens of kV to 200 kV between the electron emitting portion 2 and stably regulated in terms of withstand voltage. FIG. 5A is an embodiment in which the target layer 42 is formed in the entire area up to the peripheral edge 61 of one surface of the diamond base material 41. In the present embodiment, an anode member (not shown) and the peripheral edge 62 of the target layer 42 are electrically connected via a brazing material and a metallized layer (not shown).

  FIG. 5B is an embodiment in which the target layer 42 is formed in a range surrounded by an outer periphery 62 that is separated from the peripheral edge 61 of one surface of the diamond base material 41 by a predetermined distance. In the present embodiment, the target layer 42 is electrically connected to an anode member (not shown) via an annular electrode 45 in addition to the brazing material and the metallized layer.

  The electrode 45 may be formed on the entire surface of the diamond base material 41 as a lower layer of the target layer 42, or the target layer 42 and the diamond may be formed on a part of the outer periphery 62 of the target layer 42 as shown in FIG. It may be formed so as to bridge the peripheral edge 61 of the base material 41.

  Further, the electrode 45 may be made of not only a pure metal but also a metal nitride, a metal oxide, or a metal carbide as long as the electrode 45 has sufficient conductivity to regulate the potential of the target layer 42. By making the electrode 45 a metal carbide layer composed of a carbide of a metal element different from the target metal contained in the target layer 42, carbon is prevented from diffusing from the target layer 42 to the electrode 45, and the target layer 42. It is possible to further suppress the composition variation of the.

  Moreover, the transmission type target of this invention is good also as a form provided with the other metal carbide layer from which a composition differs from a target layer as an intermediate | middle layer between a target layer and a diamond base material.

  Next, a radiation generation apparatus including the transmission target according to the present invention was prepared according to the following procedure, and the radiation generation apparatus was operated to evaluate the output stability.

Example 1
FIG. 5A shows a schematic diagram of the transmission target 9 created in this example. Moreover, the preparation procedure of the transmissive | pervious target 9 produced in the present Example is shown in FIG.4 (b-1)-FIG.4 (b-4). In addition, FIG. 6 shows the measurement results of the X-ray diffraction method of the target layer 42 of the transmission type target 9 of this example and the metal layer 43 in the process of forming the transmission type target 9. Furthermore, the radiation generating tube 1 provided with the transmission type target 9 produced in the present embodiment is shown in FIG. 2, and the radiation generating apparatus 20 provided with the radiation generating tube 1 is shown in FIG.

  First, as shown in FIG. 4 (b-1), a diamond base material 41 made of a single crystal diamond having a diameter of 6 mm and a thickness of 1 mm is prepared. Next, the diamond base material 41 is prepared using a UV ozone asher device. The residual organic matter on the surface was washed. The prepared single crystal diamond base material contained 50 ppm of nitrogen in the diamond.

  Next, as shown in FIG. 4 (b-2), argon gas is used as a carrier gas and tungsten sintered body is used as a sputtering target with respect to one cleaning surface of the diamond base material 41. The metal layer 43 to be formed was formed by sputtering so as to have a layer thickness of 5 μm.

  When the layer structure of the metal layer 43 made of tungsten obtained in this step was evaluated by an X-ray diffraction method, a diffraction exhibiting a (110) plane derived from pure metal tungsten at a diffraction angle of 2θ = 40.2 degrees. A peak was observed. This X-ray diffraction profile is shown in the lower part of FIG.

  Next, as shown in FIG. 4 (b-3), the laminated body of the tungsten layer 43 and the diamond base material 41 was transported into the image furnace to make a vacuum reduced pressure atmosphere. Next, the image furnace was heated to a temperature of 1600 ° C., and the carbonization of the tungsten layer 43 was performed, so that the transmission target 9 including the target 42 was produced.

  When the layer structure of the target layer 42 obtained in this step was evaluated by X-ray diffraction analysis, a plurality of diffraction peaks derived from monotungsten carbide (WC) were observed. Specifically, main peaks and sub-peaks observed near diffraction angle 2θ = 35.6 degrees and 48.3 degrees are (100) plane derived from tungsten carbide (WC) and (101) plane. It showed. This X-ray diffraction profile is shown in the upper part of FIG.

  The X-rays used in the X-ray diffraction analysis were copper (Cu) Kα rays (8.05 keV), and the Kβ rays were removed with a nickel (Ni) filter.

  As shown in FIG. 6, the metal layer 43 on the diamond base material 41 before the heat treatment is identified as pure metal tungsten, and the target layer 42 on the diamond base material after the heat treatment is made of tungsten carbide. , WC). In addition, the vertical axis | shaft which shows the diffraction peak intensity of FIG. 6 is an arbitrary unit.

  Next, a cross-sectional specimen S1 was prepared in which the cross section of the obtained transmission target 9 includes the interface between the target layer 42 and the diamond substrate 41 by mechanical polishing and FIB processing. When the prepared specimen S1 is mapped by X-ray electron spectroscopy (XPS) to map the composition and the distribution of bonds, it is observed that tungsten exists uniformly corresponding to the layer thickness of the target layer 42, It was observed that carbon was present uniformly corresponding to the target layer 42 and the diamond base material 41. In addition, a sample S2 for observation with a transmission electron microscope (TEM) was prepared by performing FIB processing in the same manner as the sample S1. The specimen S2 is combined with high-resolution image observation of a transmission electron microscope, electron diffraction analysis (ED), and electron beam spectroscopic analysis (EDX) to map the crystallinity distribution, crystal orientation distribution, and composition distribution. ,evaluated. As a result, a crystal structure caused by hexagonal monotungsten carbide corresponding to the target layer 42 was confirmed by electron diffraction and a high resolution image.

  Next, the obtained transmission target 9 was placed in a vacuum chamber (not shown) equipped with an electron gun (not shown), and the target layer 42 was irradiated with the focused electron beam 5 emitted from the electron emission source 3. The emission of characteristic X-rays derived from tungsten Kα rays was confirmed. At this time, a voltage of 100 kV was applied between the electron gun and the transmissive target 9.

Next, the transmission type target 9 prepared in this example was connected to an anode member made of Kovar (not shown) to form an anode. Next, an electron emission source 3 composed of an impregnated electron gun provided with lanthanum boride (LaB ₆ ) as the electron emission portion 2 was connected to a cathode member made of Kovar (not shown) to form a cathode. Furthermore, a silver solder was used to connect the cathode and the anode to each of both openings of the insulating tube made of alumina. Finally, the inside of the container surrounded by the anode, the cathode and the insulating tube was evacuated to 1 × 10 ⁻⁶ Pa. Thus, the radiation generating tube 1 shown in FIG. 2 was created. Furthermore, using the radiation tube 1, the radiation generator 20 shown in FIG. 3 was created, and an evaluation system shown in FIG. 7 for evaluating the driving stability of the radiation generator 20 was prepared.

Driving condition of the driving stability evaluation of the radiation generating apparatus 20, the electron emission unit transmission an acceleration voltage applied to the target 9 + 100 kV, electron current density 4mA / mm 2 which is irradiated to the target layer 42 to ^two, electron Pulse driving was performed by repeating irradiation time and non-irradiation time alternately as a set of 2 seconds and 198 seconds, respectively. When evaluating the stability of the radiation output intensity, the current flowing from the target layer 42 to the ground electrode 66 is measured, and the electron current density irradiated to the target layer 42 is varied within 1% by a negative feedback circuit (not shown). It was controlled to be a value. Furthermore, during the drive evaluation of the radiation generator 20, it was confirmed by the discharge counter 67 that it was stably driven without discharging.

  The stability of the radiation output intensity of the radiation generator 20 is evaluated by pulsing the electron emission source 3 under the above conditions, and once every 100 hours, the radiation generator 1 is stopped and the entire radiation generator tube 1 is The radiation output intensity was measured with the radiation dosimeter 26 after being stopped for 1 hour until the room temperature and the equilibrium temperature were reached. The radiation output intensity was the average value of the signal intensity detected by the radiation dosimeter 26 for 1 second. In the stability evaluation, the radiation output intensity after each elapsed time was evaluated by the variation rate normalized by the initial radiation output intensity. Of these evaluation results, Table 1 shows the rate of change after 100 hours, 200 hours, and 400 hours.

  It was confirmed that the radiation generating apparatus 13 provided with the transmission type target 9 of the present embodiment can obtain a stable radiation output intensity even after a long driving history.

  Furthermore, when the radiation generating tube 1 after the above-described driving test was taken out and the transmission target 9 was observed, no separation between the target layer 42 and the diamond base material 41 was observed.

When the density of the target layer 42 of this example was measured by the RBS method, it was 15.8 × 10 ³ (kg / m ³ ), and the penetration depth Dp with respect to incident electrons having a kinetic energy of 100 keV is: It was 4.2 × 10 ⁻⁶ (m). Accordingly, in the radiation generating tube operating at a tube voltage of 100 kV, at least the range of the electron penetration depth Dp from the surface of the target layer 42 is a metal carbide layer containing as a main component tungsten carbide. I confirmed that it was.

(Example 2)
The transmissive target 9 and the radiation generating tube are the same as in the first embodiment except that the transmissive target 9 is prepared by the manufacturing method shown in FIGS. 4 (a-1) and 4 (a-2). 1. The radiation generator 20 was created. Furthermore, the drive stability of the second example was evaluated using the drive evaluation system of Example 1.

  In this example, a target layer 42 made of tungsten carbide (Tanka 1 Tungsten, WC) was formed on the diamond base material 41 with a thickness of 6 μm by the CVD method. The transmission type target 9 obtained in this example has the schematic configuration shown in FIG.

  When the layer structure of the formed target layer 42 was evaluated by X-ray diffraction analysis in the same manner as in Example 1, a plurality of diffraction peaks derived from monotungsten carbide (WC) were observed. Specifically, main peaks and sub-peaks observed near diffraction angle 2θ = 35.6 degrees and 48.3 degrees are (100) plane derived from tungsten carbide (WC) and (101) plane. It showed. Similarly to Example 1, cross-sectional specimens S3 and S4 were prepared, and the prepared specimen S3 was mapped with composition and bond distribution states by X-ray electron spectroscopy (XPS). Tungsten was observed, and carbon was observed corresponding to the target layer 42 and the diamond base material 41. For the cross-sectional specimen S4, in the same manner as in Example 1, a combination of high-resolution image observation with a transmission electron microscope (TEM), electron diffraction analysis (ED), and electron beam spectroscopic analysis (EDX) Sex distribution, crystal orientation distribution and composition distribution were evaluated. The obtained crystal orientation was mapped. As a result, the crystal structure resulting from the hexagonal monotungsten carbide crystal corresponding to the target layer 42 was confirmed by electron diffraction and a high resolution image.

When the density of the target layer of this example was measured by the RBS method, it was 15.9 × 10 ³ (kg / m ³ ), and the penetration depth Dp with respect to incident electrons having kinetic energy of 100 keV was 4 It was 2 × 10 ⁻⁶ (m). Accordingly, in the radiation generating tube 1 operating at a tube voltage of 100 kV, at least the range of the electron penetration depth Dp from the surface of the target layer 42 is a metal carbide layer containing tungsten carbide as the main component. I confirmed that it was.

  In the same manner as in Example 1, the stability of the radiation output intensity of the radiation generator 20 was evaluated. The results are shown in Table 2.

  It was confirmed that the radiation generating apparatus 13 provided with the transmission type target 9 of the present embodiment can obtain a stable radiation output intensity even after a long driving history.

  Furthermore, when the radiation generating tube 1 after the above-described driving test was taken out and the transmission target 9 was observed, no separation between the target layer 42 and the diamond base material 41 was observed.

9 Transmission target 41 Diamond base material 42 Target layer

Claims (34)

  A transmission type target comprising: a target layer containing a metal carbide that generates X-rays upon electron irradiation; and a diamond base material that supports the target layer.   The transmission target according to claim 1, wherein the target layer contains a target metal that generates X-rays when irradiated with electrons.   The transmission target according to claim 2, wherein the target metal is a metal selected from the group consisting of molybdenum, tantalum, and tungsten.   4. The transmission type target according to claim 1, wherein the metal carbide is located on the diamond base material. 5.   The transmission type target according to any one of claims 1 to 4, wherein the metal carbide is located in a region where X-rays are generated.   6. The transmission type target according to claim 1, wherein the metal carbide is distributed and contained in a layer thickness direction of the target layer.   The transmissive target according to claim 6, wherein the metal carbide is uniformly contained in a thickness direction of the target layer.   The transmission target according to any one of claims 1 to 7, wherein the target layer is a metal carbide layer composed of the metal carbide. When the target layer contains each of ditungsten carbide and monotungsten carbide in a [W ₂ C] mole fraction and a [WC] mole fraction, [W ₂ C] <[WC]. The transmission type target according to any one of claims 1 to 8. When the target layer contains [Mo ₂ C] mole fraction and [MoC] mole fraction, each of dimolybdenum carbide and monomolybdenum carbide, [Mo ₂ C]> [MoC]. The transmission type target according to any one of claims 1 to 8. When the target layer contains each of tantalum carbide and monotantalum carbide in a [Ta ₂ C] mole fraction and a [TaC] mole fraction, [Ta ₂ C] <[TaC]. The transmission type target according to any one of claims 1 to 8.   12. The target layer according to claim 1, wherein the target layer contains at least one of hexagonal dimolybdenum carbide, cubic crystal tantalum carbide, and hexagonal crystal tungsten carbide. The described transmission target.   The periphery of the target layer is located inside the periphery of the diamond substrate, and includes an electrode that bridges from the periphery of the target layer to the periphery of the substrate, and the electrode is different from the metal contained in the target layer The transmission type target according to any one of claims 1 to 12, comprising a metal carbide.   The transmission target according to any one of claims 1 to 13, wherein the diamond base material directly supports the target layer.   The transmission target according to any one of claims 1 to 14, wherein the diamond base material contains polycrystalline diamond.   The transmission target according to any one of claims 1 to 15, wherein the target layer is laminated on the diamond base material without a layer that inhibits heat transfer. The transmission type target according to any one of claims 1 to 16,
An electron emission source having an electron emission portion spaced apart from and opposed to the target layer;
An X-ray generator tube comprising: an envelope provided with at least the electron emission portion and the target layer in an internal space or an inner surface thereof. An X-ray generating tube according to claim 17,
A drive circuit that is electrically connected to each of the target layer and the electron emission portion and outputs a tube voltage applied between the target layer and the electron emission portion;
An X-ray generator comprising: In the range of the electron penetration depth Dp (m) defined by the following general formula 1 in the layer thickness direction of the target layer from the surface facing the electron emission portion of the target layer, the target layer is the metal carbide. The X-ray generator according to claim 18, comprising:
Dp = 6.67 × 10 ⁻¹⁰ × Va ^1.6 / ρ (Formula 1) where Va (V) is the tube voltage, and ρ is the density (kg / m ³ ) of the target layer. .   20. An X-ray imaging apparatus comprising: the X-ray generator according to claim 18; and an X-ray detector that detects X-rays emitted from the X-ray generator and transmitted through a subject.   An X-ray generation target comprising a target layer containing a metal carbide that generates X-rays upon electron irradiation and a diamond base material that supports the target layer, wherein the metal carbide is a region where X-rays are generated An X-ray generation target characterized by being located at   The X-ray generation target according to claim 21, wherein the target layer contains a target metal that generates X-rays upon electron irradiation.   The X-ray generation target according to claim 22, wherein the target metal is a metal selected from the group consisting of molybdenum, tantalum, and tungsten.   The transmission target according to any one of claims 21 to 23, wherein the diamond base material directly supports the target layer.   The transmission target according to any one of claims 21 to 24, wherein the diamond base material contains polycrystalline diamond.   The transmission target according to any one of claims 21 to 25, wherein the target layer is laminated on the diamond base material without a layer that inhibits heat transfer.   27. The X-ray generation target according to any one of claims 21 to 26, wherein the metal carbide is distributed and contained in a thickness direction of the target layer.   28. The X-ray generation target according to claim 27, wherein the metal carbide is uniformly contained in a layer thickness direction of the target layer. When the target layer contains each of ditungsten carbide and monotungsten carbide in a [W ₂ C] mole fraction and a [WC] mole fraction, [W ₂ C] <[WC]. The X-ray generation target according to any one of claims 21 to 28. When the target layer contains [Mo ₂ C] mole fraction and [MoC] mole fraction, each of dimolybdenum carbide and monomolybdenum carbide, [Mo ₂ C]> [MoC]. The X-ray generation target according to any one of claims 21 to 28. When the target layer contains each of tantalum carbide and monotantalum carbide in a [Ta ₂ C] mole fraction and a [TaC] mole fraction, [Ta ₂ C] <[TaC]. The X-ray generation target according to any one of claims 21 to 28. A method for producing a transmission target comprising a metal carbide layer as a target layer, the step of preparing a diamond substrate,
A film forming step of forming a metal layer made of a metal selected from at least one of molybdenum, tantalum, and tungsten on one surface of the diamond substrate;
A carbonization step of heating the diamond base material provided with the metal layer, diffusing carbon from the diamond base material to the metal layer, and forming a metal carbide layer containing a carbide of the metal as a target layer;
A method of manufacturing a transmission type target, comprising:   The said carbonization process is performed at the temperature of 1000 degreeC or more and 2000 degrees C or less under inert gas atmosphere or pressure-reduced atmosphere, The manufacturing method of the transmission type target of Claim 32 characterized by the above-mentioned. A method for producing a transmission target comprising a metal carbide layer as a target layer, the step of preparing a diamond substrate,
A film forming step in which a metal carbide layer made of at least one selected from molybdenum, tantalum, and tungsten and carbon is formed on one surface of the diamond substrate to form a target layer;
A method of manufacturing a transmission type target, comprising:

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