Patent Application
20130188774
The present invention relates to a transmission-type radiation target that is suitable for diagnostic applications, nondestructive radiography, and the like in the fields of medical and industrial devices and a method for producing the transmission-type radiation target.
A well-known example of the radiation target is a transmission-type target. Since transmission-type targets have advantages in that an electron emission source, the target, and a radiation extraction window can be aligned in a line, the applications of the transmission-type targets in miniaturized, high-definition radiation generating apparatuses are expected.
PTL 1 discloses an anode including a beryllium substrate on which tungsten is disposed. PTL 1 also discloses a method for preventing separation of the tungsten from the beryllium substrate, which is caused by stress generated by a difference in linear expansion amount between the tungsten and the beryllium substrate, by disposing an interlayer composed of copper, chromium, iron, titanium, or the like therebetween. PTL 2 discloses a method for improving cooling efficiency for radiating the heat generated in a target layer by disposing an interlayer as a thermal diffusion layer between a metal base material composed of a copper alloy or a silver alloy and the target layer composed of a metal material such as molybdenum, chromium, tungsten, gold, silver, copper, or iron. The interlayer is composed of a mixture of copper or silver with diamond powder or titanium.
PTL 1 Japanese Patent Laid-Open No. 2000-306533
PTL 2 Japanese Patent Laid-Open No. 2002-93355
Existing transmission-type targets having an interlayer sometimes show a gradual decrease in the output radiation intensity in test runs. Although the mechanism that causes the variation in output has not been clearly determined, it is presumably related to the change in adhesion of the interlayer.
An object of the present invention is to reduce the variation in the output radiation intensity by maintaining adhesion of a target layer over a prolonged period, and to obtain the stable output radiation in terms of intensity.
A radiation target according to the present invention includes a supporting substrate, a target layer that emits radiation when irradiated with an electron beam, and an interlayer located between the supporting substrate and the target layer. The interlayer has a thickness of 1 μm or less and contains titanium as a main component. At least part of the titanium shows the β-phase at 400° C. or less.
A method for producing a radiation target according to the present invention includes the steps of forming a first layer containing titanium and at least one metal selected from V, Nb, and Ta on a substrate; forming a second layer containing a target metal on the first layer; and performing a β-phase stabilization treatment in which the first layer is maintained at 600° C. or more and 1600° C. or less.
Further features of the present invention will become apparent from the following description of exemplary embodiments with reference to the attached drawings.
A radiation generating tube 1 will be now described.
The degree of vacuum in the internal space 12 can be any degree of vacuum with which the mean free path can be maintained so that the electrons can at least fly between the electron emission source 3 and the target 8. The applicable degree of vacuum is 1E-4 Pa or less. The degree of vacuum in the internal space 12 can be selected accordingly in consideration of the type of the electron emission source 3 used. In cases where a cold cathode electron emission source or the like is used, the degree of vacuum is more preferably 1E-6 Pa or less. Optionally, in order to maintain the degree of vacuum in the internal space 12, a getter may be installed in the internal space 12 or in an additional space communicating with the internal space 12.
The electron emission source 3 disposed inside the envelope 6 can be any electron emission source as long as the amount of electron emission is controllable from the outside of the envelope 6. The hot cathode electron emission source or cold cathode electron emission source can be used accordingly. The electron emission source 3 can be electrically connected to a driving circuit 14 installed outside the envelope 6 so that the amount of the electron emission and the On-Off state of the electron emission can be controlled via a current introduction terminal 4 that penetrates through the envelope 6. The electron emission source 3 includes an electron emission portion 2. The electron emission portion 2 can be disposed in any position as long as the electrons emitted from the electron emission portion 2 impinge the below-described target 8. As shown in
A radiation generating apparatus 13 will be now described.
The target 8 will be now described. As shown in
The target layer 82 is located on one surface of the target 8, which is on the side irradiated with the electrons. The target layer 82 contains a heavy metal as the target substance. Metals having an atomic number of 39 or more, such as tungsten and gold, can be used as the target substance. The thickness of the target layer 82 is determined in consideration of the targeted radiation energy, the density of the target layer 82, and the accelerating voltage of incident electrons. The thickness of the target layer 82 can be 1 to 20 μm, for example.
The supporting substrate 80 structurally supports the target layer 82 that is a thin film. In order to maintain the strength of the layered body, the supporting substrate preferably has a thickness (thickness of substrate) of 100 μm or more. More preferably, the supporting substrate 80 has a thickness of 500 μm or more, because heat locally generated in the target layer 82 can be released outside the target 8 efficiently. When the supporting substrate 80 contains a light element such as beryllium, graphite, or diamond as a main component, a transmission-type target 8 including the supporting substrate 80 functioning as a radiation-transmissive member can be formed. The transmission-type target 8 allows forward radiation, which is emitted from the surface of the target 8 that is on the opposite side (hereafter, referred to as forward) to the side irradiated with the electron beam 5 (hereafter, referred to as backward), to exit from the radiation generating tube 1 or the radiation generating apparatus 13. When the target 8 is made transmissive, the maximum thickness of the supporting substrate 80 is determined in consideration of the radiation transmittance of the supporting substrate. For example, when the transmission-type target 8 includes a supporting substrate 80 composed of diamond, the supporting substrate preferably has a thickness of 2 mm or less from the viewpoint of radiation transmittance. Since diamond has a high melting point, low density, and high thermal conductivity, diamond is a particularly preferable material that can be used for the supporting substrate 80 of the transmission-type target 8. The diamond used for the supporting substrate 80 may have any crystal structure, such as a polycrystal or a single crystal structure and is preferably a single-crystal diamond from the viewpoint of thermal conductivity.
The interlayer 81 will be now described. As shown in
When the interlayer 81 has an excessively small thickness, the anchoring force between the supporting substrate 80 and the target layer 82 become insufficient and cannot maintain adhesion therebetween. Accordingly, the interlayer 81 preferably has a thickness of at least 1 nm or more, or about 10 layers of atoms or more. In contrast, when the interlayer 81 has an excessively large thickness, the temperature change during the radiation output of the target 8 causes the stresses at each of the interfaces of the layers constituting the target 8 due to the difference in linear expansivity between the supporting substrate 80 and the target layer 82. This may result in poor adhesion in microscopic scale. Accordingly, the interlayer 81 preferably has a thickness of 1 μm or less. The interlayer 81 also serves as a heat transfer layer that transfers the heat generated in the target layer during the radiation output of the target 8 to the supporting substrate 80 efficiently. Consequently, an excessively large thickness of the interlayer 81 results in poor thermal conductivity, which causes the target 8 to be superheated during the radiation output. This may cause a variation in the output radiation intensity. Accordingly, the interlayer 81 more preferably has a thickness of 0.1 μm or less. Note that “during the radiation output” refers to the state in which the target layer 82 is irradiated with the electron beam 5 emitted from the electron emission source 3 and emitting radiation with the predetermined intensity.
The material for the interlayer 81 needs to be a material with which a sufficient adhesion can be achieved at the connection interfaces with the target layer 82 and with the supporting substrate 80. In addition, in order to maintain a layered structure with the target layer 82 that is to be heated up to about 1000° C., the material for the interlayer 81 is required to have heat resistance so as not to melt during the operation of the target 8. The interlayer 81 is characterized in that the interlayer 81 contains titanium as a main component and at least part of the titanium shows the β-phase as a low-temperature phase of 400° C. or less. The interlayer 81 having such characteristics satisfies the above requirements of heat resistance and can maintain adhesion of the target 8 and good heat dissipation even when the target 8 is subjected to cyclic temperature history between in-operation and at-rest. As a result, the target 8 shows an effect of maintaining a high output stability over a prolonged period.
Pure titanium exists in two phases having a transformation temperature of 882° C. in a temperature region of its melting point of 1670° C. or less. One is a low-temperature phase referred to as the α-phase, which is shown in a lower temperature region of 882° C. or less and has a hexagonal close-packed crystal structure. The other is a high-temperature phase referred to as the β-phase, which is shown in a higher temperature region of 882° C. or more and having a body-centered cubic crystal structure. In the present invention, pure titanium refers to titanium with a purity of 100%, which contains no metal element that forms an alloy with titanium in the composition. In accordance with the temperature history in which the target layer 82 is heated up to about 1000° C. during operation, the titanium contained in the interlayer repeatedly undergoes a phase transition from the α-phase to the β-phase in the heating-up process and a phase transition from the β-phase to the α-phase in the cooling-down process.
The inventors of the present invention have determined the characteristics of the interlayer that had experienced a plurality of operational histories, and acquired the knowledge that a target that has experienced a plurality of operational histories shows a gradual decrease in radiation output, that the interlayer is a polycrystal including a plurality of grains, and that an interlayer of the target that has experienced a plurality of operation histories has a coarse grain size, which is related to the phase transition from the β-phase to the a-phase that occurs in the cooling-down process.
On the basis of this knowledge, the inventors of the present invention have found that the grains of the interlayer 81 containing titanium as a main component can be prevented from being coarse by configuring the interlayer 81 to show the β-phase as a low-temperature phase, and thereby adhesion of the target 8 can be maintained even when the target has experienced a plurality of operational histories.
The interlayer 81 showing the β-phase as a low-temperature phase includes an interlayer in which not necessarily all of the titanium shows the β-phase, but part of the titanium shows the β-phase. The form in which part of the titanium shows the β-phase includes the form in which the α-phase and β-phase coexist as an eutectoid. Note that, in the present invention, the low-temperature phase refers to a phase in a temperature range of 400° C. or less, but not a specific phase (α-phase or β-phase) of titanium. The temperature of 400° C. is a reference temperature associated with the boundary temperature between in-operation and at-rest temperatures of the target 8.
In order to show the β-phase as a low-temperature phase, the interlayer 81 containing titanium may have a composition containing a β-phase-stabilizing metal as a trace component as well as titanium as a main component. In addition, the interlayer 81 may be composed of an alloy of titanium and a β-phase-stabilizing metal. The β-phase-stabilizing metal is a metal that, when being added to pure titanium, has an effect of lowering the phase transformation temperature of titanium at which the titanium changes from being in a state containing only the a-phase to being in a state containing the β-phase so as to be less than the phase transformation temperature of pure titanium. Referring to
As shown above, the addition of vanadium to pure titanium modifies the phase-transition temperature characteristics in terms of lowering the α-β phase-transition temperature (phase transition point) so as to be less than that of pure titanium, that is, 882° C. Therefore, vanadium is a β-phase-stabilizing metal for titanium.
The maximum content of β-phase-stabilizing metal in the interlayer 81 is preferably 50 atm % or less, which means that the interlayer 81 contains titanium as a main component and β-phase-stabilizing metal as a trace component. The interlayer 81 needs to contain titanium as a main component and β-phase-stabilizing metal as a trace component so that the interlayer 81 achieves static adhesion to the target layer 82 and to the supporting substrate 80. Static adhesion refers to adhesion between layers that has no relation to the temperature history but that is mainly governed by the compatibility between the materials respectively contained in each layer.
The minimum content of β-phase-stabilizing metal in the interlayer 81 can be determined from the first transformation curve. Specifically, in order to obtain dynamic adhesion, the interlayer 81 preferably contains β-phase-stabilizing metal in an amount of 1.5 times or more the minimum β-phase-stabilizing metal content with which the α-phase titanium and the β-phase titanium coexist as an eutectoid at 400° C. Dynamic adhesion refers to adhesion between layers that changes with the temperature history upon the occurrence of a phase transition.
The β-phase-stabilizing metal for titanium is not limited to the above vanadium (V) and other examples thereof include niobium (Nb) and tantalum (Ta). In other words, the β-phase-stabilizing metal contained in the interlayer 81 of the target 8 is at least one metal selected from V, Nb, and Ta. The interlayer 81 may contain other elements as long as the effect of lowering the β-α phase transition temperature of pure titanium is not impaired.
The minimum vanadium, niobium, and tantalum contents with which the a-phase titanium and the β-phase titanium coexist as an eutectoid at 400° C. are 2.2 atm %, 1.8 atm %, and 2.0 atm %, respectively, which are almost the same content. Thus, by containing 3.3 atm % or more and 50 atm % or less of the β-phase-stabilizing metal, the interlayer 81 can show the β-phase as a low-temperature phase stably regardless of the type of the β-phase-stabilizing metal.
When the interlayer 81 is composed of a polycrystal with an average grain size of 0.1 μm or less in the in-plane direction of the interlayer 81, coarsening of the grains of titanium may be prevented to a higher degree even in the cases where the interlayer 81 has a long operational and temperature history.
The method for producing the target 8 will be now described with reference to
The amount of each metal component added to the substrate 80 in the step of forming the first layer in the method for producing the target according to the present invention will be now described. The preferred β-phase-stabilizing metal concentration Cβ=[Mβ/([Mβ]+[MTi]) in the interlayer 81 is represented by the following general formula (1):
0.033≦[Mβ]/([Mβ]+[MTi])≦0.5 general formula (1)
where [Mβ] is the β-phase-stabilizing metal concentration in the interlayer 81 mentioned above, and [MTi] is the titanium concentration in the interlayer 81.
By transforming the general formula (1) into a formula for the content ratio [Mβ]/[MTi], the general formula (2) can be uniquely obtained.
0.035≦[Mβ]/[MTi]≦1 general formula (2)
Thus, the method for producing the target according to the present invention includes setting the amount (corresponding to [Mβ]) of at least any metal selected from vanadium, niobium, and tantalum added to the substrate 80 to be 0.035 or more and 1 or less in terms of atomic ratio relative to the amount (corresponding to [MTi]) of titanium added to the substrate 80 in the step of forming the first layer.
The method for producing the target according to the present invention includes performing the below-described β-phase stabilization treatment at least on the first layer 81. The β-phase stabilization treatment step includes heating the first layer 81 and thereby gives the first layer an effect of stably maintaining a composition containing titanium that shows the β-phase as a low-temperature phase. The β-phase stabilization treatment step includes maintaining the first layer 81 in the temperature range of 600° C. or more and 1600° C. or less for a predetermined time. More specifically, the heating treatment includes at least one of the following treatments: a solution treatment in which the first layer 81 is maintained in the temperature range of 900° C. or more and 1600° C. or less for a predetermined time and then rapidly cooled and an age hardening treatment in which the first layer 81 is maintained in the temperature range of 600° C. or more and 880° C. or less for a predetermined time. Selection of the solution treatment and the age hardening treatment can be made accordingly in consideration of heat resistance or the like of the target 8 or other members of the radiation generating tube 1.
The β-phase stabilization treatment step may be performed in the step of forming the first layer 81, that is, before the step of forming the second layer in the production process for the target 8. This is because diffusion at the interface between the supporting substrate 80 and the interlayer 81 is thereby promoted, which selectively improves adhesion between the supporting substrate 80 and the interlayer 81.
The β-phase stabilization treatment step may be performed in the step of forming the second layer 82 in the production process for the target 8. This is because the migration of the target material on the first layer in the deposition process of the second layer is thereby promoted, which improves adhesion between the interlayer 81 and the target layer 82.
The β-phase stabilization treatment step may be performed after the step of forming the second layer 82 in the production process for the target 8. This is because the residual stress generated between layers due to the difference in linear expansivity between the stacked layers of the target 8 is thereby reduced, which reduces the distortion and separation of the layered target.
The heating time for the solution treatment may be determined in consideration of the type of material or the thicknesses of the substrate, first layer, and second layer. For example, the heating time for the solution treatment can be in the range of 10 minutes to 10 hours. The heating time for the age hardening treatment can be in the range of 20 minutes to 20 hours.
The manner in which the interlayer 81 and the target layer 82 are stacked on the supporting substrate 80 is not limited to that in which the entirety of one surface of the supporting substrate 80 is covered as shown in
Examples of available methods for fixing the target 8 to the shield 7 include a method using a conductive connection member such as silver solder (not shown) and a method of pressure-bonding.
The radiation generating apparatus 13 and the radiation generating tube 1 may include not only one each of electron emission source 3 and target 8 as shown in
A high-pressure synthetic diamond produced by Sumitomo Electric Industries, Ltd. was prepared as a supporting substrate 80 as shown in
Then, as shown in
Then, as shown in
Next, the layered body including the supporting substrate 80, the interlayer 81, and the target layer 82 being stacked on top of one another in this order was put into an image furnace (not shown) evacuated to a degree of vacuum of 1E-5 Pa. The layered body was then maintained within the image furnace at 700° C. for 1 hour. After the heating step, the image furnace was cooled down to room temperature over 2 hours and ventilated. Then, the layered body was taken out. Between the step of forming the target layer 82 and the step of performing β-phase stabilization treatment, the layered body was put into the image furnace without introduction of air.
As described above, a target 8 that included the supporting substrate 80, the interlayer 81, and the target layer 82 being stacked on top of one another in this order was manufactured.
The interlayer 81 and the target layer 82 were formed in a multilayer so as to respectively have predetermined thicknesses by controlling the deposition time in accordance with predetermined calibration curve data based on the relationship between thickness and deposition time when each layer was formed as a single layer. The measurement of thickness for determining the calibration curve data was made using spectroscopic ellipsometer UVISEL ER produced by HORIBA, Ltd.
The resulting target 8 was die-cut to form intermediate samples (not shown). The intermediate samples were subjected to mechanical polishing and FIB processing to be processed into a size so that the target layer 82, the interlayer 81, and the interface between the interlayer and the supporting substrate 80 were included therein. Thus, a cross-section specimen S1 was prepared. As in the case of preparing the cross-section specimen S1, the intermediate samples were processed using FIB processing and a SIMS detector in combination to be processed so that the interlayer 81 stacked on the supporting substrate 80 was exposed. Thus, a film-surface specimen S2 was prepared.
The distribution of the composition and bonding of each layer in the cross-section specimen S1 was visualized on a map using a transmission electron microscope (TEM) and electron beam spectrometry (energy dispersive X-ray spectrometry: EDX) in combination. It was thereby confirmed that a carbon-predominant region corresponding to the supporting substrate 80, titanium-predominant region corresponding to the interlayer 81, and tungsten-predominant region corresponding to the target layer 82 were stacked. The distribution of the composition of the interlayer 81 in the film-surface specimen S2 was visualized on a map using the transmission electron microscope (TEM) and electron beam spectrometry (energy dispersive X-ray spectrometry: EDX) in combination. It was thereby confirmed that titanium and niobium were distributed in the same region as each other in both interlayers 81 of the cross-section specimen S1 and the film-surface specimen S2.
The thickness of the interlayer 81 in the cross-section specimen S1 was measured using the transmission electron microscope (TEM) and found to be 100 nm.
Then, crystallinity, grain size, and composition distribution of the cross-section specimen S1 and the film-surface specimen S2 were evaluated by bright-field observation and dark-field observation using the transmission electron microscope, and by electron beam spectrometry (energy dispersive X-ray spectrometry: EDX) in combination. As a result, a plurality of grains were observed in the interlayer 81. The average grain size thereof was 85 nm. It was confirmed that each grain contained titanium and niobium. The titanium and niobium contents of the interlayer 81 were 54.9 atm % and 45.1 atm %, respectively.
The crystal form of the grains in the cross-section specimen S1 and the film-surface specimen S2 was evaluated by bright-field observation and dark-field observation using the transmission electron microscope, by electron diffraction (ED), and by electron beam spectrometry (energy dispersive X-ray spectrometry: EDX) in combination. The samples were maintained at 400° C. during evaluation. From the result of the electron diffraction, it was confirmed that a body-centered cubic crystal structure predominated in titanium contained in the interlayer 81. In other words, it was confirmed that the interlayer 81 of this Example showed the β-phase at 400° C. It was also confirmed that, even when the samples were kept at a room temperature of 25° C., the interlayer 81 showed the β-phase similarly to the result under the heating condition of 400° C.
Then, as shown in
Next, as shown in
As shown in
As shown in
The driving conditions during the stability evaluation of the radiation generating apparatus 13 were as follows: an accelerating voltage applied to the target 8 relative to the electron emission portion 2 of +90 kV, a current density of electrons on the irradiated target layer 82 of 4 mA/mm2, and a pulse driving intermittent electron irradiation at 10 second intervals. During the stability evaluation of the output radiation intensity, a current from the target layer 82 to the grounding electrode was detected and the current density of electrons on the irradiated target layer was controlled to have a variation coefficient of 1% or less using a negative feedback circuit (not shown). During the running evaluation of the radiation generating apparatus 13, stable running without discharge was confirmed using a running discharge counter 25.
The stability evaluation of the output radiation intensity of the radiation generating apparatus 13 was performed as follows: The electron emission source 3 was subjected to the pulse driving under the above conditions. At every 100 hours, the radiation generating apparatus was temporarily stopped for 2 hours till the entirety of the radiation generating tube 1 reached a temperature equal to room temperature and the output radiation intensity was determined with a radiation dosimeter 26. The output radiation intensity was an average intensity of the signal detected by the radiation dosimeter 26 over 1 second. The stability evaluation was conducted using the coefficient of variation obtained by normalizing the output radiation intensity observed in each time step with the initial output radiation intensity. These evaluation results are shown in Table 1.
It was confirmed that the radiation generating apparatus 13 including the target 8 of this Example provides stable output radiation intensity even in cases where there is a long driving history.
In this Example, a target 8 was manufactured as in the first example, except that the deposition rate was controlled in the step of forming the interlayer 81 so that the amount of niobium added on the supporting substrate 80 per unit time was 0.176 (in terms of atomic ratio) relative to the amount of titanium added to the supporting substrate 80 per unit time.
Intermediate samples, a cross-section specimen S1, and a film-surface specimen S2 were prepared as in Example 1 using the target 8 manufactured in this Example.
As in the first example, mapping of the distribution of composition and bonding was carried out for each layer of the prepared cross-section specimen S1 using the TEM and EDX in combination. It was thereby confirmed that a carbon-predominant region corresponding to the supporting substrate 80, titanium-predominant region corresponding to the interlayer 81, and tungsten-predominant region corresponding to the target layer 82 were stacked. Next, as in the first example, mapping of the composition distribution of the interlayer 81 in the film-surface specimen S2 was carried out using the TEM and EDX in combination. It was thereby confirmed that titanium and niobium were distributed in the same region as each other in both interlayers 81 of the cross-section specimen S1 and the film-surface specimen S2.
As in the first example, the thickness of the interlayer 81 in the cross-section specimen S1 was measured using the TEM and found to be 99 nm.
As in the first example, crystallinity, grain size, and composition distribution of the cross-section specimen S1 and the film-surface specimen S2 were evaluated by bright-field observation and dark-field observation using the TEM, and by EDX in combination. As a result, a plurality of grains were observed in the interlayer 81. The average grain size thereof was 103 nm. It was confirmed that each grain contained titanium and niobium. The titanium and niobium contents of the interlayer 81 were 85.0 atm % and 15.0 atm %, respectively.
As in the first example, the crystal form of the grains in the cross-section specimen S1 and the film-surface specimen S2 was evaluated by bright-field observation and dark-field observation using the TEM, by ED, and by EDX in combination. The samples were maintained at 400° C. during evaluation. From the result of the electron diffraction, it was confirmed that the titanium contained in the interlayer 81 had a crystal form including both the grains with a body-centered cubic structure and the grains with a hexagonal close-packed structure. In other words, it was confirmed that the interlayer 81 in this Example was in the α-β eutectoid phase at 400° C. and showed the β-phase. It was also confirmed that, even when the samples were kept at a room temperature of 25° C., the interlayer 81 was in the α-β eutectoid phase and showed the β-phase similarly to the result under the heating condition of 400° C.
As in the first example, as shown in
As in the first example, the stability evaluation of the output radiation intensity was also conducted in this Example using the experimental system shown in
It was confirmed that the radiation generating apparatus 13 including the target 8 of this Example provides stable output radiation intensity even in cases where there is a long driving history.
In this Example, a target 8 was manufactured as in the first example, except that the sputtering target composed of vanadium was used in place of that composed of niobium and that the deposition rate was controlled in the step of forming the interlayer 81 so that the amount of vanadium added on the supporting substrate 80 per unit time was 0.25 (in terms of atomic ratio) relative to the amount of titanium added on the supporting substrate 80 per unit time.
Intermediate samples, a cross-section specimen S1, and a film-surface specimen S2 were prepared as in Example 1 using the target 8 manufactured in this Example.
As in the first example, mapping of the distribution of composition and bonding was carried out for each layer of the prepared cross-section specimen S1 using the TEM and EDX in combination. It was thereby confirmed that a carbon-predominant region corresponding to the supporting substrate 80, titanium-predominant region corresponding to the interlayer 81, and tungsten-predominant region corresponding to the target layer 82 were stacked. Next, as in the first example, mapping of the composition distribution of the interlayer 81 in the film-surface specimen S2 was carried out using the TEM and EDX in combination. It was thereby confirmed that titanium and vanadium were distributed in the same region as each other in both the interlayers 81 of the cross-section specimen S1 and the film-surface specimen S2.
As in the first example, the thickness of the interlayer 81 in the cross-section specimen S1 was measured using the TEM and found to be 100 nm.
As in the first example, crystallinity, grain size, and composition distribution of the cross-section specimen S1 and the film-surface specimen S2 were evaluated by bright-field observation and dark-field observation using the TEM, and by EDX in combination. As a result, a plurality of grains were observed in the interlayer 81. The average grain size thereof was 91 nm. It was confirmed that each grain contained titanium and vanadium. The titanium and vanadium contents of the interlayer 81 were 80.2 atm % and 19.8 atm %, respectively.
As in the first example, the crystal form of the grains in the cross-section specimen S1 and the film-surface specimen S2 was evaluated by bright-field observation and dark-field observation using the TEM, by ED, and by EDX in combination. The samples were maintained at 400° C. during evaluation. From the result of the electron diffraction, it was confirmed that the titanium contained in the interlayer 81 had a crystal form including both the grains with a body-centered cubic structure and the grains with a hexagonal close-packed structure. In other words, it was confirmed that the interlayer 81 in this Example was in the α-β eutectoid phase at 400° C. and showed the β-phase. It was also confirmed that, even when the samples were kept at a room temperature of 25° C., the interlayer 81 was in the α-β eutectoid phase and showed the β-phase similarly to the result under the heating condition of 400° C.
As in the first example, as shown in
As in the first example, the stability evaluation of the output radiation intensity was also conducted in this Example using the experimental system shown in
It was confirmed that the radiation generating apparatus 13 including the target 8 of this Example provides stable output radiation intensity even in cases where there is a long driving history.
This Example employed the same method as in the first example, except that the stability evaluation of the output radiation intensity from the radiation generating tube 1 was conducted using the radiation generating tube 1 manufactured in the first example and the measuring system illustrated in
It was confirmed that the radiation generating tube 1 including the target 8 of this Example provides stable output radiation intensity even in cases where there is a long driving history.
In this Comparative example, a target 48 was manufactured as in the first example, except that the deposition rate was controlled in the step of forming the interlayer 81 so that the amount of niobium added to the supporting substrate 80 per unit time was 0.010 (in terms of atomic ratio) relative to the amount of titanium added to the supporting substrate 80 per unit time.
The intermediate samples, the cross-section specimen S1, and the film-surface specimen S2 were prepared as in the first example using the target 48 manufactured in this Comparative example.
As in the first example, mapping of the distribution of composition and bonding was carried out for each layer of the prepared cross-section specimen S1 using the TEM and EDX in combination. It was thereby confirmed that a carbon-predominant region corresponding to the supporting substrate 80, titanium-predominant region corresponding to the interlayer 81, and tungsten-predominant region corresponding to the target layer 82 were stacked. Next, as in the first example, mapping of the composition distribution of the interlayer 81 in the film-surface specimen S2 was carried out using the TEM and EDX in combination. It was thereby confirmed that titanium and niobium are distributed in the same region as each other in both the interlayers 81 of the cross-section specimen S1 and the film-surface specimen S2.
As in the first example, the thickness of the interlayer 81 in the cross-section specimen S1 was measured using the TEM and found to be 99 nm.
As in the first example, crystallinity, grain size, and composition distribution of the cross-section specimen S1 and the film-surface specimen S2 were evaluated by bright-field observation and dark-field observation using the TEM, and by EDX in combination. As a result, a plurality of grains were observed in the interlayer 81. The average grain size thereof was 139 nm. It was confirmed that each grain contained titanium and niobium. The titanium and niobium contents of the interlayer 81 were 99.0 atm % and 1.0 atm %, respectively.
As in the first example, the crystal form of the grains in the cross-section specimen S1 and the film-surface specimen S2 was evaluated by bright-field observation and dark-field observation using the TEM, by ED, and by EDX in combination. The samples were maintained at 400° C. during evaluation. From the result of the electron diffraction, it was confirmed that the titanium contained in the interlayer 81 had a crystal form including only grains with a hexagonal close-packed structure. In other words, it was confirmed that the interlayer 81 in this Comparative example shows the α-phase at 400° C. but not the β-phase. It was also confirmed that, even when the samples were kept at a room temperature of 25° C., the interlayer 81 showed the a-phase but not the β-phase similarly to the result under the heating condition of 400° C. As in the first example, as shown in
As in the first example, the stability evaluation of the output radiation intensity was also conducted in this Comparative example using the experimental system shown in
It was confirmed that the radiation generating apparatus 13 including the target 8 of this Comparative example provides less stable output radiation intensity compared with that of Examples 1 to 4 in cases where there is a long driving history.
According to the present invention, it is possible to maintain stable adhesion between the supporting substrate and the target layer even over a prolonged period of operation, which results in a reduction in the variation in the output radiation intensity caused by temperature rise of the target layer. Thus, it is possible to provide a radiation target having highly-reliable radiation emission characteristics.
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. The scope of the following claims is to be accorded the broadest interpretation so as to encompass all such modifications and equivalent structures and functions.
This application claims the benefit of International Patent Application No. PCT/JP2012/051297, filed Jan. 23, 2012, which is hereby incorporated by reference herein in its entirety.
| Number | Date | Country | Kind |
|---|---|---|---|
| PCT/JP2012/051297 | Jan 2012 | JP | national |
