JP2002039970A - X-ray device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable X rays of different wavelengths to be used easily in an X-ray measurement. SOLUTION: The X-ray device includes a plurality of X-ray generators 4A and 4B for generating X rays to irradiate a sample S, and a second-dimensional X-ray detector 3 for detecting X rays coming from the sample S. The plurality of X-ray generators 4A and 4B can bring X rays of different wavelengths by different angles into the sample S, and moreover at least one of the plurality of X-ray generators 4A and 4B is equipped with an X-ray condenser 6 for collecting X rays. Since the X-ray condenser 6 is set to the side where X rays are emitted from the X-ray generators 4A and 4B, it becomes possible to irradiate X rays of a practically full intensity to the sample S even if the X-ray generators 4A and 4B are micro focus ones. Accordingly, it is practically possible to set the plurality of X-ray generators to one sample S.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray apparatus for performing measurement using X-rays.

[0002]

2. Description of the Related Art In measurement using X-rays, it may be necessary to change the wavelength of the X-rays, that is, the energy of the X-rays. For example, X for single crystal structure analysis
In the X-ray measurement, X-rays of MoKα ray and CuKα ray are used according to the constituent elements of the substance to be measured and the lattice constant.
In addition, Cu (copper) rays are used for qualitative measurement and quantitative measurement, which are general measurement methods in powder diffraction measurement, and other X-rays, such as Cr lines, are used for stress measurement for measuring surface stress of a sample. Used.

The Bragg equation, that is, λ = 2d sin θ
As can be seen from FIG. 6, the longer the wavelength (λ) of the X-ray, the larger the peak angle (θ) of the same sample. When performing stress measurement using X-rays, 2θ = 180 as much as possible.
Measuring the peak at a large diffraction angle close to ° increases the measurement accuracy. However, the angle measurement range is generally not so wide for various reasons. Therefore,
The wavelength of the incident X-ray is selected so that the peak having a high X-ray intensity falls within the angle measurement range, taking into account the peak shift due to the distortion. Further, the wavelength of the sample and the incident X-ray are compatible. For example, in the case of a combination of an Fe sample and a Cu line, the amount of fluorescent X-rays increases, so that the S / N ratio deteriorates. For the above reasons,
Generally, a Cr line is used for the Fe sample, and an Fe line is used for the Al sample. In other cases, a Co line, a Ni line, or the like may be used in some cases.

In the conventional X-ray apparatus, only one X-ray generator is provided for the object to be measured. Therefore, when changing the wavelength of X-rays, the operator must replace the X-ray target. In addition, each time the replacement is performed, the X-ray focal point must be aligned with other X-ray elements.

[0005]

However, the alignment of the X-ray element as described above becomes more difficult as the X-ray focal point becomes smaller, and the number of X-ray elements increases or the X-ray element becomes a focusing element. It becomes even more difficult. It can be said that these relationships change exponentially.

In order to solve such a problem, the present inventor previously provided a plurality of X-ray generating means constituting the X-ray apparatus, and selected one of them as necessary. A technique was considered in which a measurement was performed, and when it became necessary to change the wavelength of X-rays, another X-ray generation means was selected from the plurality of X-ray generation means and used.

However, in the case of an X-ray generator generally used in the past, in order to obtain strong X-rays, the input power had to be set large. To accommodate this, the target and the cooling means for cooling the target had to be large, that is, the X-ray generating section had to be large. And as a result, 1
It is practically difficult to include a plurality of X-ray generating means in one X-ray apparatus, and thus the above idea of providing a plurality of X-ray generating means in an X-ray apparatus could not be realized.

The present invention has been made in view of the above problems, and has as its object to facilitate the use of X-rays of different wavelengths in performing X-ray measurement.

[0009]

In order to achieve the above object, an X-ray apparatus according to the present invention comprises a plurality of X-ray generating means for generating X-rays irradiated on a sample; An X-ray apparatus having two-dimensional X-ray detection means for detecting, wherein the plurality of X-ray generation means can make X-rays incident on the sample at different angles from each other, and further collect X-rays X-ray focusing means is provided in at least one of the plurality of X-ray generation means.

In the above configuration, the "two-dimensional X-ray detecting means" is an X-ray detecting means having a structure capable of receiving X-rays in a plane area and measuring the X-ray at each point in the plane area. For example, it can be constituted by an X-ray dry plate, an X-ray film, a stimulable phosphor, a planar CCD (Charge Coupled Device) sensor, or the like.

The "X-ray focusing means" refers to the divergent X-rays.
A means of focusing a line on a specific point,
For example, two curved reflectors 51 as shown in FIG.
52, a cylindrical X-ray reflecting mirror 52 as shown in FIGS. 6 and 7, and two flat plate monochromators 56 and 5 having a wide mosaic angle width as shown in FIG.
7 or a device using a parallel X-ray beam forming means 58 and a zone plate 59 as shown in FIG.

In the X-ray condensing means shown in FIG. 5, two reflectors 51 and 52 are arranged in a right-angled positional relationship with each other. The X-rays guided to the curved reflector 51 and reflected by the first curved reflector 51 are reflected by the second curved reflector 5.
The light is reflected at 2 and collected at point P. At this time, the X-rays are directed to the first curved reflector 51 in the left-right direction by the second curved reflector 5.
At 2, the light is focused in the vertical direction by total reflection. The slit 62 prevents unnecessary X-rays from reaching the focal point P.

The X-ray focusing means shown in FIGS. 6 and 7 is disclosed, for example, in Japanese Patent Application Laid-Open No. 5-332954, and includes a bending mechanism 65 constituted by two U-shaped members 66 and 67. The radius of curvature r of the cylindrical X-ray reflecting mirror 52 is adjusted. The X-ray R radiating from the X-ray source F is X
The light is totally reflected by an inner surface 52a having a semicircular cross section of the line reflecting mirror 52,
The points P are collected in both the vertical direction shown in FIG. 6 and the horizontal direction shown in FIG.

The light collecting means shown in FIG.
X-rays R emitted from the X-ray source F can maintain the X-ray intensity, that is, two flat plates having a wide mosaic angle width that does not greatly attenuate the X-ray intensity. After being diffracted by the monochromators 56 and 57, the light is converged on the point P.

The X-ray focusing means shown in FIG. 9 comprises a parallel parabolic reflector 58 as a parallel beam forming means, a spectral crystal 68 as a spectral means, a zone plate 59, and a parallel parabolic reflection means. A casing 69 hermetically surrounding the area from the mirror 58 to the zone plate 59;
And an exhaust device 71 for removing air from the inside of the device.

The parallel parabolic reflecting mirror 58 is, for example, shown in FIG.
The parabolic reflector 72a shown in (a), that is, the parabolic reflector 72a formed by finishing the X-ray reflecting surface of the appropriate member 73 into a parabolic surface H is arranged side by side in two vertical and horizontal directions. It is formed by. When the divergent X-rays are incident on these parallel parabolic reflectors 72a, divergent beams are formed into parallel beams in both the vertical and horizontal directions, and as a result, as shown by a symbol R2, parallel beams having a rectangular cross section are formed. An X-ray beam is formed.

As is well known, the spectral crystal 68 is a crystal that, when receiving X-rays including X-ray components having a plurality of different wavelengths, functions to extract only a specific wavelength component from the received X-rays. What kind of material is used as the spectral crystal 68 is appropriately selected according to the wavelength to be extracted.

The zone plate 59 is, for example, as shown in FIG.
As shown in (a) and (b), an X-ray transmission band 74 that can transmit X-rays and an X-ray shield 75 that does not transmit X-rays are alternately arranged in layers. This zone plate 59
The X-ray shielding band 7 having a predetermined pattern is formed on the substrate 76 by using an appropriate patterning method, for example, a photolithography method.
5 can be produced. In this case, the X-ray transmission band 74 is formed by the portion of the substrate 76 existing between the adjacent X-ray shield bands 75.

The substrate 76 is formed of, for example, Si ₃ N ₄ (silicon nitride), BN (boron nitride) or the like. The X-ray shielding band 75 is formed of, for example, Au, Ta (tantalum), Ni, or the like. The number of zones formed by the pair of X-ray transmission bands and X-ray shielding bands is set to, for example, about 300 to 400.

Since an electromagnetic wave in the X-ray region has a refractive index close to 1, it cannot be imaged using a lens as in the case of visible light. Instead, a zone plate is used. The zone plate is, for example, a circular diffraction grating, by which X-rays can be imaged.
When the number of zones is 100 or more, it can be treated as almost the same as a lens used in refraction optics.

In FIG. 11B, an X-ray R0 emitted from an X-ray source F reaches a focal point P through an X-ray transmission band 74. The band widths of the X-ray transmission band and the X-ray shield band are set such that the optical path length of the X-ray passing through the m-th X-ray transmission band and the (m + 1) -th X-ray transmission band is shifted by the wavelength. All the X-rays that reach the focal point P reinforce each other and play the role of the focal point of the lens.

Referring to FIG. 9, the X-ray source F is
X-rays R <b> 0 radiated from and radiated from the casing 69 are taken into the casing 69. In the case of the structure shown in FIG. 9 using the parallel parabolic reflector 58 as the parallel beam forming means, a point focus, that is, an X-ray focal point having a dimension in which the vertical width and the horizontal width are almost equal to each other is used as the X-ray source F. desirable. Since X-rays that spread almost equally in two perpendicular directions are emitted from the point-focused X-ray source, such X-rays can be efficiently converted into parallel X-ray beams by the parallel parabolic reflector 58. is there.

The X-rays taken into the casing 69 are shaped into a parallel X-ray beam R2 having a rectangular cross section by the parallel parabolic reflector 58, and are incident on the spectral crystal 68.
The spectral crystal 68 converts the incident X-ray into a single color, that is, extracts only the X-ray of a specific wavelength and outputs
Emitted toward.

Since the zone plate 59 has the property of converging the parallel X-ray beam to a specific point, the monochromatic parallel X-ray beam incident on the zone plate 59 converges on a minute converging point P. In this case, since the X-rays received by the zone plate 59 are X-ray beams formed exactly in parallel by the parallel parabolic reflecting mirror 58, the focal point P formed by the zone plate 59 is extremely low. And the diameter can be, for example, 10 μm or less.

Although it is functionally possible to obtain focused light only by combining the reflecting mirror 58 and the zone plate 59 without using the spectral crystal 68, a plurality of X-rays are incident on the zone plate 59. X including X-ray component of wavelength
If it is a line, that is, a continuous X-ray, there is a possibility that blurring due to chromatic aberration occurs at the light-collecting point P formed by the zone plate 59, and the light-collecting point P having a minute area clearly defined cannot be obtained. is there. On the other hand, if the parallel X-ray beam incident on the zone plate 59 is made monochromatic by the dispersive crystal 68 as in the present embodiment, the influence of chromatic aberration can be reduced, and therefore, an extremely small area having a clearly defined area can be reduced. A converging point P can be obtained.

The casing 6 is provided by the exhaust device 71.
By evacuating the inside of 9 and removing air, attenuation of X-rays due to air scattering can be prevented, and thus, X-rays with high intensity can be focused on the converging point P having a very small area.

In the structure shown in FIG. 9, a parallel type parabolic reflecting mirror having a structure in which parabolic reflecting mirrors 72a are arranged in parallel in two directions in the vertical and horizontal directions as parallel beam forming means, a so-called side-by-side type. Instead of using a parabolic reflector, a structure in which a vertical parabolic reflector and a horizontal parabolic reflector are separated and arranged on the X-ray optical axis is adopted. You can also. Further, a structure in which the parabolic reflector 72a is provided only in one of the vertical direction and the horizontal direction can be adopted.

As the parallel beam forming means, FIG.
1A is not limited to the parabolic reflector 72a shown in FIG.
The parabolic reflector 72b shown in FIG.
A parabolic reflector 72b having a structure in which a metal reflective film 77 is formed on the paraboloid surface can be used. A parabolic multilayer mirror 78 as shown in FIG. 12, that is, a structure in which the surface of the base 73 is formed into a smooth mirror-like parabolic surface H, and a multilayer film 79 is formed on the parabolic surface. Alternatively, a parabolic multilayer mirror 78 having a structure that reflects X-rays by diffraction can be used. The base 73 is formed of, for example, a single crystal Si (silicon) plate, stainless steel, or the like.

Since the paraboloid cannot be made of a soft metal, it is made of a hardly deformable metal. However, if a metal film, for example, Au (gold) is formed on the surface of the paraboloid, the reflection efficiency is improved. This is because the critical angle at which total reflection occurs becomes large.

The multilayer film 79 includes a heavy element layer 81 and a light element layer 8.
2 are alternately stacked a plurality of times, and the surface on which the X-rays R0 generated and diverged from the X-ray source F are incident is a parabolic surface H. Each layer can be formed by using an appropriate film formation method, for example, a sputtering method.

By periodically repeating a multilayer structure of the heavy element layer 81 and the light element layer 82 by a plurality of layers, a specific X-ray, for example, CuKα ray can be efficiently diffracted. You can get a line. Furthermore, by making the surface of the multilayer film 79 a parabolic surface H, incident X-rays can be diffracted or reflected in a parallel direction over the entire surface, and an accurate parallel beam can be obtained.
That is, if the parabolic multilayer mirror 78 is used, a monochromatic parallel X-ray beam can be obtained with a very high intensity.

When the X-rays are totally reflected, the X-rays must be made incident on the total reflection surface from a low angle, that is, the expected angle must be reduced, so that the X-rays that can be focused can be focused. Is considered to be low. On the other hand, in the multilayer film 79 in which X-rays are diffracted on a paraboloid, the expected angle θ0 can be set large, so that X-rays with high intensity can be collected at the focal point.

In order to be able to diffract X-rays in each layer, the stacking thickness of a pair of the heavy element layer 81 and the light element layer 82, that is, the stacking thickness for one cycle, is X
The stack thickness t2 on the X-ray incidence side is larger than the stack thickness t1 on the X-ray incidence side. For example, t1 ≒ 30Å, t2 ≒
Set to about 40 °. The heavy element may be, for example, W (tungsten), and the light element may be, for example, Si, C (carbon), B ₄ C, or the like.

According to the X-ray apparatus of the present invention having the above structure, the X-ray focusing means is provided on the X-ray emitting side of the X-ray generating means, so that the X-ray generating means has a small capacity and a small shape. Even when a certain so-called microfocus X-ray generating means is used, it is possible to irradiate the sample with X-rays of sufficient intensity for practical use. Therefore, a plurality of X-ray generating means are arranged for one sample. Has become practically possible. By arranging a plurality of types of X-ray generating means for one sample in such a manner, it is possible to easily use X-rays of different wavelengths when performing X-ray measurement on the sample. Become.

In the X-ray apparatus according to the present invention having the above structure, the X-ray generating means has a focal size of 60 μm × 60 μm.
It is desirable that the X-ray generation means has a structure in which a microfocus of m or less is formed on the target.

In general, X-ray generators include a sealed tube system having a structure in which the inside is sealed in a high vacuum state, and an open tube system having a structure in which the inside can be evacuated to atmospheric pressure or evacuated to a high vacuum state. The focus size employed in these X-ray generators is a normal focus of about 1 mm × 10 mm, a fine focus of about 0.4 mm × 8 mm, and a long fine focus of 0.4 mm × 12 mm. Also, a broad focus of 2 mm × 12 mm or the like is known. Also, in the open pipe,
In some cases, a minute focus having a focus size of 0.1 mm × 1 mm or less is used.

Each of the focus sizes as described above is employed to generate X-rays having sufficient intensity and resolution in X-ray measurement. The capacity of the sealed tube is about 2 KW, The capacity is set to 12 KW or more. When the current flowing through the wire increases, the amount of heat generated by the resistance increases in proportion to I ² R. Therefore, it is necessary to reduce the resistance value by making the wire thicker or to reduce the contact resistance of the connection portion. If the electric power used exceeds 1 KW, a single-phase 200 V is usually used, since making the electric wire thick increases the cost and is not a good solution. Further increase, 3 phase 2
00V is used. Therefore, the single-phase 200
V, 3 phase 200V is used for the rotating cathode open tube.

Since the X-ray generator having a large focus size and requiring large power as described above has a large shape, conventionally, a plurality of such X-ray generators are arranged around a sample to be measured. Attempting to do so would require a distance between them, which was physically possible but not practical. This is because such an arrangement causes various inconveniences such as a large floor area, a heavy apparatus, difficult alignment, and a high price.

On the other hand, in recent years, due to the improvement in the performance of the X-ray condensing device, even an X-ray generator having a structure that requires a small focus size and a small electric capacity can be used for X-ray measurement. It has been confirmed by the present inventors that X-rays of sufficient intensity can be obtained. Specifically, a small-power X-ray generated by forming a focus size of φ60 μm or less, that is, a so-called micro-focus size on a target using a single-phase 100 V which is a widely used household power source, is used. X-ray measurement can be performed without practical problems by condensing the line with the X-ray condensing device.

The relationship between the focal point size and the output of the X-ray tube is, for example, 8 W at φ10 μm, 25 W at φ20 μm,
It is 100 W at φ40 μm and 300 W at φ60 μm.

The X-ray generator of the microfocus type has properties such as a small input power, a small target, and a small cooling device for cooling the target. Installation is easier, maintenance is easier, and maintenance costs can be reduced.
Further, such a microfocus type X-ray generator can be constituted by either a sealed tube system or an open tube system, and is itself small in size, and its accompanying devices such as a power supply and a casing are very small. Can be formed. As a result, it is possible to arrange a plurality of X-ray generators around the sample.

Next, in the X-ray apparatus according to the present invention having a structure using a plurality of X-ray generating means, one of the X-ray generating means is constituted by a Mo target, and the other is constituted by a Cu target. The X-ray generation means having the Mo target is arranged so that X-rays enter the sample from the front of the sample, and the X-ray incidence angle by the X-ray generation means having the Mo target and the X-ray having the Cu target It is desirable to set the difference from the X-ray incident angle by the generating means to substantially 40 °. Here, “substantially 40 °” means a case where the angle slightly deviates from 40 ° depending on the adjustment method.

When the optical arrangement of the X-ray apparatus is set as described above, a single crystal structure analysis can be performed by selectively using either one of two types of characteristic lines, MoKα ray and CuKα ray. Conventionally, when changing the type of X-rays between the above two types of wavelengths, the X-ray tube of the X-ray generator is replaced one by one, and the alignment of the optical system is performed each time. The measurement was very difficult because the measurement was performed from the beginning. On the other hand, according to the present invention, it is possible to very easily select one of the X-rays having different wavelengths and perform the X-ray measurement.

Next, in the X-ray apparatus according to the present invention having a structure using a plurality of X-ray generating means, one of the X-ray generating means is Cu
The X-ray generation means having the Cr target has an X-ray detection range of 155 ° by the X-ray detection means.
As described above, it is desirable to provide it near the end of the X-ray detection means.

According to this configuration, a qualitative analysis and a quantitative analysis of a powder sample, that is, a polycrystalline sample are performed by using an X-ray generator constituted by a Cu target,
F using an X-ray generator composed of a target
Measurement of the surface stress of the e-sample can be easily and selectively performed by one X-ray apparatus. In particular, in the X-ray measurement using the conventional large-capacity X-ray generator, the diffraction angle (so-called 2θ) can be only up to about 155 ° due to the structural limitation of the housing and the collimator table. According to an X-ray apparatus, an X-ray generator using a Cr target is used to obliquely X-ray the sample.
By making the line incident, a 2θ angle measurement range of −40 ° to + 165 ° can be secured, and it is possible to exert its power in measuring surface stress.

[0046]

FIG. 1 shows a plan structure of an embodiment of an X-ray apparatus according to the present invention. FIG. 2 shows the same X
3 shows a side structure of the wire device. The X-ray apparatus shown here is an apparatus particularly suitable for structural analysis of a single crystal substance.
As shown in FIG. 1, the X-ray apparatus includes a first X-ray generation unit 1A, a second X-ray generation unit 1B, a sample support device 2 for supporting a single crystal sample S at a predetermined position, and an X-ray output from the sample S. A stimulable phosphor 3 as two-dimensional X-ray detecting means for detecting a line;

The first X-ray generation unit 1A includes a first X-ray generation device 4A, an X-ray collection device 6 provided on the X-ray emission side of the first X-ray generation device 4A, and an X-ray collection device 6 X-ray passage tube 7 provided on the X-ray emission side of
And an X-ray shutter 8 provided on the X-ray emission side.
The first X-ray generator 4A has at least an X-ray focal point at C
u, a filament 12 that emits thermoelectrons when energized, a power supply unit 13 that applies a voltage to the filament 12, and a target 11a
And a casing 9 for airtightly storing the filament 12.

On the other hand, the second X-ray generation unit 1B
X-ray generator 4B, X-ray collector 6 provided on the X-ray emission side of second X-ray generator 4B, and X-ray passage provided on the X-ray emission side of X-ray collector 6 It has a tube 7 and an X-ray shutter 8 provided on the X-ray emission side of the X-ray passage tube 7. The second X-ray generator 4B includes a target 11b having at least an X-ray focal point formed of Mo, a filament 12 that emits thermoelectrons when energized, a power supply unit 13 that applies a voltage to the filament 12, a target 11b and a filament. And a casing 9 for airtightly storing the casing 12.

In the present embodiment, the first X-ray generator 4A and the second X-ray generator 4B are formed as so-called microfocus type X-ray generators. Micro focus on top, for example 60 μm × 60
A focus having a size of μm or less, that is, an X-ray focus is formed. Such a microfocus can be formed with an electric energy of about 8 W (watt). Therefore, the power supply unit 13 can be connected to a normal 100 V commercial power supply to receive power supply.

The X-ray generator of the type using a single-phase 100V power supply with a micro focus as described above is a single-phase 200V power supply with a normal focus or a fine focus.
The external shape can be significantly reduced as compared with the X-ray generator of the type using the above-described power supply.

In the first X-ray generation unit 1A and the second X-ray generation unit 1B, the X-ray collector 6 has, for example, the structure shown in FIG. 5, FIG. 6, FIG. 7, FIG. An X-ray focusing device can be used. Also, X
The line passage tube 7 can be formed by, for example, a hollow pipe made of aluminum. The X-ray shutter 8 has an arbitrary structure that can switch between passing and blocking of X-rays.

The second X-ray generation unit 1B provided with the Mo target is arranged in front of the sample S, and the first X-ray generator 1A provided with the Cu target is used for the second X-ray generation device 1A centering on the sample S.
It is disposed at an angular position of θ ≒ 40 ° with respect to X-ray generation unit 1B.

The sample supporting device 2 for supporting the sample S is shown in FIG.
As shown in the figure, the φ rotating unit 14 directly supporting the sample S
A カ イ (chi) rotating unit 16 supporting the φ rotating unit 14;
ω rotating unit 17 supporting φ rotating unit 14 and χ rotating unit 16
And a so-called three-axis rotating structure.

The φ rotation unit 14 rotates the sample S about a φ axis passing through the sample S, that is, rotates the sample S in a plane. Also,
The rotation unit 16 rotates the sample S as indicated by the arrow A by the φ rotation unit 14 about the χ axis passing through the sample S in the direction perpendicular to the paper of FIG. In addition, the ω rotation unit 17 rotates around the ω axis which is an axis passing through the intersection of the φ axis and the χ axis.
The rotating section 16 rotates the sample S. It should be noted that the specific structure of each of the rotating parts described above can be freely configured as needed.

The sample support device 2 constituted by a three-axis rotating structure includes a φ rotating unit 14, a Δ rotating unit 16 and an ω rotating unit 1.
By selectively operating any or all of 7,
An arbitrary diffraction surface of the single crystal sample S can be irradiated with X-rays.

Next, the stimulable phosphor 3 is an energy storage type radiation detector which is also called a stimulable phosphor, and a stimulable phosphor, for example, a microcrystal of BaFBr: Er ²⁺ is applied to a flexible film. Formed on the surface of a flat film or other member by coating or the like. The stimulable phosphor is an object capable of accumulating X-rays and the like in the form of energy, and further capable of emitting the energy as light to the outside upon irradiation with stimulating excitation light such as laser light.

That is, when the stimulable phosphor is irradiated with X-rays or the like, energy is accumulated as a latent image inside the stimulable phosphor corresponding to the irradiated portion, and the energy is further accumulated on the stimulable phosphor. When stimulating excitation light such as laser light is irradiated, the latent image energy is emitted as light and emitted to the outside. By detecting the emitted light with a photoelectric tube or the like, the detection position and intensity of X-rays that have contributed to the formation of a latent image can be measured. This stimulable phosphor is 1 to conventional X-ray film.
It has a sensitivity of 0 to 60 times and a wide dynamic range of 10 ⁵ to 10 ⁶ .

In the present embodiment, in FIG. 1, the X-rays of the second X-ray generation unit 1B which receives X-rays from the front of the sample S are shown.
Assuming that the X-ray optical axis Xa of the first X-ray generation unit 1A disposed at an angle of θ ≒ 40 ° with respect to the line optical axis Xb is 0 °, at least its left side is + 144 ° and its right side is −60 °
The stimulable phosphor 3 is curved around a cylindrical shape so as to cover the angle range described above and arranged around the sample S. As a result, the stimulable phosphor 3 sets the X-ray optical axis Xb of the second X-ray generation unit 1B to 0 °, its left side + 100 ° and its right side −1.
They are arranged in an angular positional relationship that can cover an angle range of 00 °.

In FIG. 1, the first X-ray generation unit 1A
Alternatively, when X-rays emitted from the second X-ray generation unit 1B enter the sample S, if the Bragg diffraction condition is satisfied between the incident X-rays and the crystal lattice plane of the sample S, the diffraction X A line is emitted. The diffracted X-rays expose the stimulable phosphor 3 to form a latent image at the exposed point. FIG. 3 shows an example of a reader for reading a latent image formed on the stimulable phosphor 3.

The reading device 19 shown here has a support 21 for supporting the stimulable phosphor 3, a laser light source 24 for emitting laser light as stimulating excitation light, and an emission from the laser light source 24. Light reflecting member 23 that reflects laser light
a, a scanning optical system 22 disposed opposite to the support 21 and receiving light from the light reflecting member 23a, and a laser light detector 26 receiving light from the light reflecting member 23b.
And The laser light detector 26 includes, for example, a photoelectric converter.

The scanning optical system 22 is driven by the scanning driving device 27 to scan the surface of the stimulable phosphor 3 in two directions orthogonal to XY, that is, in a plane direction. The scanning drive device 27 can be configured using any parallel moving mechanism. The laser light detector 26 receives the light and outputs a signal corresponding to the light intensity. The output terminal of the laser light detector 26 has X
The line intensity calculation circuit 28 is connected.

The arithmetic unit 36 has a CPU (Central Processes).
sing unit) 38 and a memory 39. Memory 39
Is a storage medium including various storage areas such as a storage area for storing a program used by the CPU 38 and a storage area acting as a work area and a temporary file for the CPU 38, and more specifically, a semiconductor memory, a hard disk, It can be formed by other various storage media. The CPU 38 performs an operation for controlling various devices connected to the input / output interface 41 according to a program stored in the memory 39.

The X-ray intensity calculation circuit 28 and the scanning driving device 27 are connected to the CPU 38 through the input / output interface 41, respectively. The input / output interface 41 is connected to a display 42 for displaying information as an image, for example, a CRT (Cathode Ray Tube) display, and further connected to a printer 43 for recording information on a stamping material such as paper. You.

The components of the reading device 19 shown in FIG. 3 except for the display 42 and the printer 43 can be arranged below the base 18 in FIG. It is desirable to provide a transport mechanism for transporting the image data between the measurement position shown in FIG. 2 and the reading position shown in FIG.

In FIG. 1, the stimulable phosphor 3 which has been measured is mounted on the support 21 shown in FIG.
When reading is performed by irradiating a laser beam while scanning and moving in the Y plane, the coordinate position of the diffracted X-ray image in the XY plane can be obtained by the operation of the CPU 38. In addition, the support 21 may have a planar shape as shown or a cylindrical shape. When the support 21 has a planar shape,
The scanning optical system 22 scans and moves in a plane. On the other hand, when the support 21 has a cylindrical shape, the scanning optical system 22
The surface of the stimulable phosphor 3 supported in a cylindrical shape is scanned by rotating about the central axis of one cylinder and simultaneously moving linearly in the direction of the cylinder axis.

The CPU 38 sums the intensities of the diffracted X-ray images for the sample S obtained in this manner for each Debye ring, that is, for each equal diffraction angle line, that is, sums the values.
For example, by integrating, the X-ray intensity for each diffraction angle (2θ) can be calculated.

Since the X-ray apparatus according to the present embodiment is configured as described above, at the time of measurement, first, the single crystal sample S to be measured is attached to the φ rotating unit 14 in FIG. Then, according to the constituent elements and the lattice constant of the sample S,
In FIG. 1, a desired one of the first X-ray generation unit 1A and the second X-ray generation unit 1B is operated, and X-rays of a desired wavelength are incident on the sample S. In conventional X-ray equipment, when changing the X-ray source to one with a different wavelength, replace the X-ray generator with one with a target made of a different material and readjust the alignment of the X-ray optical element. However, in the present embodiment, two X-ray generating units 1A are required.
And 1B are provided in an aligned state in advance, so that the X-ray can be freely changed between the Cu wavelength and the Mo wavelength and incident on the sample S, which is very convenient.

The first X-ray generation unit 1A uses C
The uKα ray is incident on the sample S from an oblique direction of θ ≒ 40 °, and the angle measurement range 2θ is −60 ° to + 144 °. On the other hand, the MoKα ray from the second X-ray generation unit 1B is incident on the sample S from the front direction of the sample S, that is, θ = 0 °, and the angle measurement range 2θ is −100 ° to + 100 °. Each of the X-ray generation units has a sufficient angle measurement range for analyzing the structure of the single crystal sample S.

FIG. 4 shows another embodiment of the X-ray apparatus according to the present invention. This embodiment is an embodiment in which a polycrystalline powder material is used as a sample S for measurement. In this embodiment, the first X-ray generator 4A constituting the first X-ray generation unit 1A includes a Cr (chromium) target 11A.
c and the second X-ray constituting the second X-ray generation unit 1B
The line generator 4B has a Cu target 11a. In FIG. 4, the same components as those shown in FIG. 1 are denoted by the same reference numerals, and description thereof will be omitted.

The installation angle position θ1 of the first X-ray generation unit 1A is defined as +1 on the left side with respect to the X-ray optical axis Xc of 0 °.
The angle range from 65 ° to the right -40 ° is set so as to be covered by the stimulable phosphor 3. As a result,
The first X-ray generation unit 1A is disposed close to the left end of the stimulable phosphor 3. On the other hand, the second X-ray generation unit 1B
Is set to an appropriate angle as desired.

The X of the present embodiment having the above configuration
According to the X-ray apparatus, Cu by the second X-ray generation unit 1B
Performing a general powder diffraction measurement using Kα radiation and performing a surface stress measurement of, for example, an Fe-containing material using a Cr line by the first X-ray generation unit 1A according to the wishes of the measurer It can be done selectively. Also in the case of this wavelength selection, the measurer can immediately select a desired wavelength without performing complicated alignment.

When a conventional X-ray generator having a large focus size and a large electric capacity is used, structural limitations due to a housing of the X-ray generator, a collimator table attached to the X-ray generator, and the like are used. Accordingly, the diffraction angle range 2θ that can be measured is limited to about 155 °. On the other hand, an X-ray generation unit 1A formed in a small size using a microfocus X-ray generation device and an X-ray focusing device 6
According to the present embodiment having the structure using the first X-ray generation unit 1A and the first X-ray generation unit 1A, the installation angle θ1 of the first X-ray generation unit 1A is increased. -40 ° ~ +
A wide angle measurement range up to 165 ° can be secured,
It is very convenient for measuring residual stress.

As described above, the present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and can be variously modified within the scope of the invention described in the claims.

For example, in the embodiment shown in FIG.
Are provided with two X-ray generators 4A and 4B,
Three or more X-ray generators may be provided. Also, two-dimensional X
The X-ray detector is not limited to the stimulable phosphor 3, and an X-ray film or another two-dimensional X-ray detector can be used.

In FIG. 1, the X-ray passage tube 7 prevents unnecessary X-rays from going to the sample S, and the direct beam from the X-ray generator 4A or XB The X-ray passage tube 7 is not an element that must be used, although it prevents the phosphor from going to the luminescent phosphor 3. Also, the X-ray shutter 8 is not an element that must be used.

[0076]

As described above, according to the X-ray apparatus of the present invention, since the X-ray focusing means is provided on the X-ray emission side of the X-ray generating means, the capacity of the X-ray generating means is small. It is possible to perform X-ray measurement using a so-called microfocus X-ray generation means that is small and small in size, so that it is possible to provide a plurality of X-ray generation means for one sample. It became practically possible. If a plurality of types of X-ray generating means are provided for one sample, X-rays having different wavelengths can be easily used when performing X-ray measurement on the sample.

[Brief description of the drawings]

FIG. 1 is a plan view showing a planar structure of an embodiment of an X-ray apparatus according to the present invention.

FIG. 2 is a side view showing a side structure of the X-ray apparatus of FIG.

FIG. 3 is a perspective view showing an example of an X-ray reader attached to the X-ray apparatus of FIG.

FIG. 4 is a plan view showing another embodiment of the X-ray apparatus according to the present invention.

FIG. 5 is a perspective view showing an example of an X-ray focusing device used in the X-ray device of FIG.

FIG. 6 is a plan sectional view showing another example of the X-ray focusing device used in the X-ray device of FIG. 1;

FIG. 7 is a front view of the apparatus of FIG. 6;

FIG. 8 is a perspective view showing still another example of the X-ray focusing device used in the X-ray device of FIG.

FIG. 9 is a perspective view showing still another example of the X-ray focusing device used in the X-ray device of FIG.

FIG. 10 is a sectional view showing an embodiment of a reflecting mirror used in the apparatus of FIG. 9;

FIG. 11 is a diagram showing an example of a zone plate used in the apparatus of FIG.

FIG. 12 is a sectional view showing another embodiment of the reflecting mirror used in the apparatus of FIG. 9;

[Explanation of symbols]

 Reference Signs List 1A, 1B X-ray generating unit 2 Sample supporting device 3 Storage phosphor (two-dimensional X-ray detecting means) 4A, 4B X-ray generating device (X-ray generating means) 6 X-ray focusing device (X-ray focusing device) 7 X-ray passage tube 8 X-ray shutter 11a, 11b, 11c Target 12 Filament 13 Feeding unit 19 Reader F X-ray source H Parabolic surface P Focus point R X-ray S sample

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2G001 AA01 AA10 BA18 CA01 DA01 DA02 DA09 EA01 EA09 FA06 GA01 GA13 HA01 HA12 HA15 JA08 KA07 KA08 LA02 MA04 NA10 NA17 PA12 SA02 SA04

Claims (5)

[Claims] 1. A plurality of X-ray generating means for generating X-rays irradiated to a sample, and a two-dimensional X-ray detecting means for detecting X-rays emitted from the sample.
An X-ray apparatus comprising: a plurality of X-ray generating means, wherein the plurality of X-ray generating means can make X-rays incident on the sample at different angles from each other; At least one of the plurality of X-ray generating means
An X-ray apparatus, comprising: 2. An X-ray apparatus according to claim 1, wherein said X-ray generation means forms a microfocus having a focal size of 60 μm × 60 μm or less on a target. 3. The method according to claim 1, wherein
An X-ray apparatus, wherein the line generating means is driven by a single-phase 100V power supply. 4. The method according to claim 1, wherein one of the X-ray generating means has a Mo target, and the other one of the X-ray generating means has a Cu target. The X-ray generation unit having the Mo target is arranged so that X-rays are incident on the sample from the front of the sample. The difference from the X-ray incidence angle by the X-ray generation means is about 40 °.
Line equipment. 5. The method according to claim 1, wherein one of the X-ray generating means has a Cu target, and the other one of the X-ray generating means has a Cr target. The X-ray generation means having the Cr target is provided near an end of the X-ray detection means so that the X-ray detection range of the X-ray detection means is 155 ° or more. apparatus.