JP2002250704A - X-ray measuring instrument and x-ray measuring method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To measure the partial region of a sample without using a collimator or without accurately arranging a collimator at a specific position close to the sample even if the collimator is used. SOLUTION: The X-ray measuring instrument has an X-ray source for generating X-rays R0 applied to the sample S and an X-ray detector for detecting the X-rays R1 diffracted by the sample S and also has a mask 9 for covering the X-ray irradiation surface of the sample S. The mask 9 is formed from a single crystal substance and has an aperture 15 permitting X-ray R0 to pass. The partial region S0 of the sample S controlled by the aperture 15 can be set to a measuring object.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray measuring apparatus and an X-ray measuring method for measuring the crystal structure and the like of a sample using X-rays. In particular, the present invention relates to an X-ray measurement apparatus and an X-ray measurement method that use a part of a sample as a measurement region.

[0002]

2. Description of the Related Art In the X-ray measuring method, a measuring method in which a partial area of a sample, for example, a minute area is set as a measuring range is conventionally known. In this type of measurement method, generally, X
X-rays generated and diverged from a radiation source are shaped into an X-ray beam having a narrow cross-sectional diameter by a collimator, and the sample is irradiated with the X-rays having the narrow cross-sectional diameter.

[0003]

However, in the conventional X-ray measuring method and the X-ray measuring apparatus for realizing the method, the X-ray which can be narrowed by the collimator is used.
There is a problem in that there is a limit to the cross-sectional diameter of the line, and a minute area smaller than the cross-section cannot be used as the measurement area. In addition, the collimator must be placed as close as possible to the sample with high positional accuracy, and it is difficult to adjust the position of the collimator. There is also a problem that the irradiation position moves.

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned problems, and when performing measurement using X-rays, the collimator can be used without a collimator or even when a collimator is used. It is an object of the present invention to measure a partial area of a sample without arranging the sample at a specific position close to the sample with high accuracy. Another object of the present invention is to make it possible to set a smaller area as a measurement area than when a collimator is used.

[0005]

(1) In order to achieve the above object, an X-ray measuring apparatus according to the present invention comprises: an X-ray source for generating X-rays for irradiating a sample; and an X-ray diffracted by the sample.
An X-ray measurement apparatus having an X-ray detection unit for detecting a line and an operation unit for performing an operation based on the detection result, the X-ray measurement device being formed of a single crystal material, covering an X-ray irradiation surface of the sample, It is characterized by having a mask provided with an opening through which it passes.

In the above configuration, a so-called two-dimensional X-ray detector or the like having a structure for capturing X-rays two-dimensionally, that is, a so-called two-dimensional X-ray detector is employed as the X-ray detecting means. As such a two-dimensional X-ray detector, for example, an X-ray film,
A stimulable phosphor, a CCD (Charge Coupled Device) detector, or the like can be considered.

Here, the stimulable phosphor is an energy storage type radiation detector, and a stimulable phosphor such as BaF
Br: A film obtained by coating a crystal of Er ^{2+ on} a surface of a flexible film, a flat film, or another member by coating or the like. The stimulable phosphor is an object having a property 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 a stimulating excitation light such as a laser beam.

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 stimulable phosphor is further irradiated. Is irradiated with stimulating excitation light, such as laser light, the latent image energy is emitted as light to the outside. By detecting this emitted light with a photoelectric tube or the like,
The diffraction angle and intensity of X-rays that have contributed to the formation of a latent image can be measured. This stimulable phosphor has a sensitivity 10 to 60 times that of a conventional X-ray film, and has a wide dynamic range of 10 ⁵ to 10 ⁶ .

Further, the X-ray film is a flat film formed by providing an emulsion containing silver halide as a main component on one or both surfaces of a plastic film, for example, a thin and flexible plastic film. X-ray detection element. In this X-ray film, X-rays expose a photographic emulsion in the same manner as visible light. When X-rays enter the emulsion, they ionize the silver halide and form development nuclei. The silver particles are released by the development and blackened.

Also, a CCD (Charge Coupled Device)
The detector is an X configured using a CCD image sensor.
A line detector, for example, a plurality of pixels including a plurality of photodiodes or the like arranged in a straight line or a plane corresponding to the X-ray intake, and a CCD that reads out a signal generated in each of these pixels, And a charge-coupled device. The CCD has, for example, an electrode array formed by arranging a plurality of electrodes on a silicon semiconductor substrate in a linear or planar manner with an insulating layer interposed therebetween. By arranging this electrode array corresponding to the pixel array formed in the X-ray inlet, a CCD detector is constituted.

In this CCD detector, when X-rays are applied to each pixel, electric charges are accumulated under an electrode corresponding to the pixel, and a voltage is successively applied between the electrode and the semiconductor substrate, thereby accumulating the electric charge. The transferred charge is output to the outside. According to this CCD detector, when X-rays are incident within a linear range or a plane range where the electrode array extends, both the X-ray incident position and the X-ray intensity can be detected simultaneously.

According to the X-ray measuring apparatus having the above structure, the mask having the opening is arranged in front of the sample and the mask is formed of a single crystal material.
Lines that hit portions other than the opening of the mask do not reach the sample, and X-rays reaching the sample are limited to only the region corresponding to the opening formed in the mask. Therefore, the measurement can be performed on only a part of the sample.

It is desirable that the mask and the sample be in close contact with each other or that the distance be as small as possible. If the mask is close to the sample, the measurement area of the sample can be set more accurately than in the conventional method, and the irradiation area and irradiation position do not change even when the sample is swung.

When an X-ray impinges on a mask, diffracted X-rays may also be generated from the mask. However, in the present invention, the X-ray impinges on the mask because the mask is formed of a single crystal material. At this time, the diffracted X-ray generated from the mask is limited to a local diffraction angle, and the diffracted X-ray can be easily distinguished from the diffracted X-ray from the sample to be measured.

More preferably, preliminary measurement for collecting diffraction X-ray information on a mask made of a single crystal material is performed in advance, and after the main measurement is performed on a sample, the main measurement result is calculated based on the preliminary measurement result. Can be corrected. As the correction process in this case, specifically, the following several methods can be considered.

For example, when a two-dimensional X-ray detector is used as the X-ray detector, information detected two-dimensionally by the two-dimensional X-ray detector is based on intensity data on the same Debye ring. That is, by integrating for each intensity data on the same diffraction angle (2θ), it is often calculated as intensity data of one diffraction angle.

When this calculation method is used, the calculation is performed assuming that the coordinate position of the diffracted X-ray generated from the mask in the preliminary measurement does not contribute to the calculation of the intensity data in the main measurement, that is, intensity = 0 (zero). Can be.
Further, such a coordinate position can be calculated as a region where data does not change in the main measurement, that is, as an intensity corresponding to a background.

Further, the diffraction angle to which such a coordinate position belongs can be defined as a dead area. That is, in this case, it is assumed that there is no data at the diffraction angle corresponding to the dead area, and it is assumed that diffraction X-rays are generated from the sample at the diffraction angle corresponding to the dead area in the main measurement. The diffracted X-ray is diffracted X
It is not treated as line information.

Further, according to the X-ray measuring apparatus of the present invention, the X-ray irradiation area on the sample, that is, the measurement area of the sample is determined by the opening formed in the mask. The measurement of the partial area can be performed. Further, even when a collimator is used, it is possible to measure a partial area of the sample without disposing the collimator at a specific position close to the sample with high positional accuracy.

Further, by reducing the size of the opening formed in the mask, it is possible to make a finer area smaller than the case where a collimator is used.

Next, in the X-ray measuring apparatus having the above configuration,
The shape of the opening can be circular, elliptical, oval, square, rectangular, or any other shape. Further, the thickness of the mask is formed to be sufficient to prevent X-rays from passing therethrough.

Next, in the X-ray measuring apparatus having the above configuration,
The opening desirably has an inclined surface T such that the opening dimension D1 on the side close to the sample S is small and the opening dimension D2 on the opposite side is large, as shown in FIG. As shown in FIG. 8, the shape of the opening may be a shape having no inclined surface as described above. In this case, however, the opening has no corners due to the absence of the inclined surface. K remains, and the presence of the corner K hinders the arrival of X-rays in the measurement area S0, thereby lowering the X-ray intensity irradiating the measurement area S0, or diffracted X-rays and scattered X-rays from the measurement area S0. It is conceivable that the flow of data to the X-ray detector is hindered, and that the X-ray detector causes a count omission. Therefore, from the viewpoint of ensuring the reliability of measurement, it is desirable that the opening be inclined. Further, it is desirable that the inclination angle of the inclined surface is smaller than the X-ray incident angle. This allows more X-rays to be incident on the measurement area of the sample.

Next, in the X-ray measuring apparatus having the above structure, a collimator or a slit is provided between the X-ray source and the mask, and the mask is irradiated with X-rays whose cross-sectional diameter is reduced by the collimator or the like. It is desirable. That is, in the X-ray measurement apparatus according to the present invention, a collimator or a slit and a mask can be used in combination.
The collimator is not always an essential element,
It is preferable because the X-rays can be irradiated with the X-rays narrowed down so as not to protrude from the mask.

(2) Next, in the X-ray measurement method according to the present invention, a mask formed of a single crystal material and having an opening through which X-rays pass is arranged on the X-ray irradiation surface of the sample, and is generated from the X-ray source. Irradiated on the region including the opening of the mask, and diffracted X-rays from the X-ray irradiation region including the opening
X-rays diffracted by the sample and passed through the opening of the mask are detected by detecting the X-rays by the line detecting means and subtracting the diffracted X-rays by the mask from the detection result.

In the above configuration, "subtract" means that the result of the X-ray diffraction measurement performed on the sample is corrected in consideration of the diffraction X-ray information from the mask made of a single crystal material. . Specifically, the following several methods can be considered as the subtraction processing.

For example, considering the case where a two-dimensional X-ray detector is used as the X-ray detector, information detected two-dimensionally by the two-dimensional X-ray detector is based on intensity data on the same Debye ring. That is, by integrating for each intensity data on the same diffraction angle (2θ), it is often calculated as intensity data of one diffraction angle.

In the case of this calculation method, the calculation is performed by assuming that the coordinate position of the diffracted X-ray generated from the mask in the preliminary measurement does not contribute to the calculation of the intensity data in the main measurement, that is, intensity = 0 (zero). it can. Also,
Such a coordinate position can also be calculated as a region where there is no change in data in the main measurement, that is, as an intensity corresponding to the background.

Further, the diffraction angle to which such a coordinate position belongs can be defined as a dead area. In other words, in this method, it is assumed that there is no data at the diffraction angle corresponding to the dead area, and even if diffraction X-rays are generated from the sample at the diffraction angle corresponding to this dead area in the present measurement, , The diffraction X-ray is diffraction X
It is not treated as line information.

According to the X-ray measuring method having the above-described configuration, since the mask having the opening is provided in front of the sample and the mask is formed of a single crystal material, the X-ray irradiated on the sample is
Lines that hit portions other than the opening of the mask do not reach the sample, and X-rays reaching the sample are limited to only the region corresponding to the opening formed in the mask. Therefore, the measurement can be performed on only a part of the sample.

It is desirable that the mask and the sample be in close contact or that the distance be as small as possible. If the mask is close to the sample, the measurement area of the sample can be set more accurately than in the conventional method, and the irradiation area and irradiation position do not change even when the sample is swung.

When an X-ray is applied to a mask, diffracted X-rays may also be generated from the mask. However, in the present invention, since the mask is formed of a single crystal material, the X-ray is applied to the mask. In this case, the diffracted X-rays generated from the mask are limited to a local diffraction angle, and the diffracted X-rays can be easily distinguished from the diffracted X-rays from the sample to be measured. It is not adversely affected by diffracted X-rays from the mask.

According to the X-ray measurement method of the present invention, the X-ray irradiation area on the sample, that is, the measurement area of the sample is determined by the opening formed in the mask, so that a partial area of the sample can be determined without using a collimator. Can be measured. Further, even when a collimator is used, it is possible to measure a partial area of the sample without accurately arranging the collimator at a specific position close to the sample.

Further, by reducing the size of the opening formed in the mask, a much narrower region can be used as the measurement region than when a collimator is used.

In the X-ray measuring method having the above structure, the shape of the opening can be circular, elliptical, oval, square, rectangular, or any other shape. Further, the thickness of the mask is formed to be sufficient to prevent X-rays from passing therethrough.

Next, in the X-ray measuring method having the above configuration,
As shown in FIG. 4, the opening preferably has a slope such that the opening dimension D1 on the side close to the sample is small and the opening dimension D2 on the opposite side is large. As shown in FIG. 8, the shape of the opening may be a shape that does not have the above-described slope, but in this case, the corner K is formed at the opening due to the absence of the slope. In addition, the presence of the corners K hinders the arrival of X-rays in the measurement area, thereby lowering the X-ray intensity irradiating the measurement area, and detecting X-rays diffracted X-rays and scattered X-rays from the measurement area. It is conceivable that the countdown by the X-ray detector occurs due to obstruction to the detector. Therefore, from the viewpoint of ensuring the reliability of measurement, it is desirable that the opening be inclined.
Next, in the X-ray measurement method having the above-described configuration, when an inclined surface is provided in the opening, it is desirable that the inclined angle of the inclined surface is smaller than the X-ray incident angle. This allows more X-rays to be incident on the measurement area of the sample.

Next, in the X-ray measuring method having the above configuration,
The X-ray detecting means is preferably a two-dimensional X-ray detecting means such as an X-ray film, a stimulable phosphor, a CCD detector or the like for detecting X-rays two-dimensionally. 2
The specific structure of the dimensional X-ray detection means is as described above.

Next, in the X-ray measuring method having the above structure, a collimator or a slit is provided between the X-ray source and the mask, and the mask is irradiated with X-rays whose cross-sectional diameter is reduced by the collimator or the like. It is desirable. That is, in the X-ray measurement method according to the present invention, a collimator or a slit and a mask can be used in combination.
The collimator is not always an essential element,
It is preferable because the X-rays can be irradiated with the X-rays narrowed down so as not to protrude from the mask.

[0038]

FIG. 1 shows an embodiment of an X-ray exposure apparatus which is one of the constituent elements of an X-ray measuring apparatus according to the present invention. FIG. 2 shows an embodiment of a reading device, which is another component of the X-ray measuring apparatus according to the present invention. The X-ray measuring apparatus according to the present invention is configured by combining the X-ray exposure apparatus 1 shown in FIG. 1 and the reading apparatus 10 shown in FIG. The X-ray exposure apparatus 1 and the reading apparatus 10 may be installed at different places from each other, or may be installed inside one housing.

In FIG. 1, an X-ray exposure apparatus 1 includes an X-ray source that emits X-rays, that is, an X-ray focus F, and an X-ray focus F
A monochromator 3 for monochromaticizing X-rays emitted from
A collimator 4 for taking out monochromatic X-rays as a parallel X-ray beam having a narrow cross-sectional diameter by a monochromator 3, a sample supporting device 5 for supporting the sample S, and a two-dimensional X arranged cylindrically around the sample S Stimulable phosphor 2 as line detecting means
And

The X-ray focal point F is formed, for example, as a point-focus X-ray focal point. The monochromator 3 is made of, for example, a flat graphite crystal. The collimator 4 has, for example, a sectional diameter of 10 to 1.
A parallel X-ray beam of 00 μm is formed. The stimulable phosphor 2 has an inner surface serving as a fluorescent surface, that is, an X-ray receiving surface.

The sample support device 5 includes a φ rotation device 6 for rotating the sample S about the φ axis, that is, an in-plane rotation,
An arc swing mechanism 7 for rotating the sample S around the center of the sample, that is, an X-ray irradiation point X as indicated by an arrow A, and an ω rotating device 8 for rotating the sample S about the ω axis. The sample S is fixed by, for example, an adhesive or the like, and attached to the φ rotation device 6. In the case of this embodiment, the arc oscillating mechanism 7 is mounted on the ω rotating device 8, and the φ rotating device 6 is mounted on the arc oscillating mechanism 7.

A mask 9 is mounted on the surface of the sample S.
This mounting is performed, for example, by attaching the mask 9 to the sample S using an adhesive.
Or by clamping the mask 9 and the sample S from the outside of each with an appropriate clamping device. In the case of this embodiment, the sample S is formed in a rectangular plate shape as shown in FIGS. 4A and 4B.

The mask 9 is formed of a single crystal material, for example, a single crystal plate of Si, and is formed in a rectangular shape slightly smaller than the sample S. Of course, the mask 9 can also be formed to be planarly larger than the sample S. An opening 15 for X-ray passage is provided at a substantially central position of the mask 9.
Can be opened. In the case of the present embodiment, the opening 15 has an inclined surface T such that the opening dimension D1 on the side close to the sample S is small and the opening dimension D2 on the opposite side is large. The inclination angle theta _T of the inclined surfaces T, as shown in FIG. 4 (a), or the same as the incident angle theta of the incident X-ray R0 with respect to the sample S, it is set to be smaller than. 1 and 4
4 (a) and FIG. 4 (b), the opening 15 is drawn larger than it actually is for easy understanding.

A reading apparatus 10 shown in FIG. 2 has a support 11 for supporting the stimulable phosphor 2 in a plane, a laser light source 14 for emitting laser light, and a laser light for reflecting laser light emitted from the laser light source 14. A light reflecting member 13a, a scanning optical system 12 disposed opposite to the support 1 and receiving light from the light reflecting member 13a, and a laser light detector 16 receiving light from the light reflecting member 13b. Having. The laser light detector 16 is configured to include, for example, a photoelectric converter.

The scanning optical system 12 is driven by the scanning driving device 17 to move the surface of the stimulable phosphor 2 to the X-Y orthogonal
Scan in the direction, that is, in the plane direction. Scan driver 17
Can be configured using any translation mechanism. The laser light detector 16 receives the light and outputs a signal corresponding to the light intensity. An X-ray intensity calculation circuit 18 is connected to an output terminal of the laser light detector 16.

The arithmetic unit 26 is, for example, a CPU (Centra
l Processing Unit: 28 and memory 2
9 The CPU 28 performs calculations for controlling various devices connected to the bus 27. Also, the memory 29
Includes a memory area for storing programs used by the CPU 28, a memory area acting as a work area and a temporary file for the CPU 28, and more specifically, a semiconductor memory, a hard disk, and various other types of storage. It can be formed by a medium.

The X-ray intensity calculation circuit 18 and the scanning driving device 17 are connected to the CPU 28 through the input / output interface 31. The input / output interface 31 has a C for displaying information as a video.
An RT (Cathode Ray Tube) display or another display 32 is connected, and a printer 33 for printing information on a printing material such as paper is connected as necessary.

The X-ray exposure apparatus 1 shown in FIG.
The operation of the X-ray measuring apparatus including the reader 10 shown in FIG. In the measurement using the present X-ray measurement apparatus, a preliminary measurement is first performed on the mask 9, and thereafter,
A series of processing is performed in which the main measurement is performed with the mask 9 attached to the sample S, and the final measurement result is obtained by subtracting, that is, correcting the result of the main measurement by the result of the preliminary measurement. Hereinafter, each process will be described individually.

(Preliminary Measurement for Mask 9) First, FIG.
In the X-ray exposure apparatus 1 described above, the cylindrical stimulable phosphor 2 is placed so that its central axis coincides with the ω axis. Further, the mask 9 alone without the sample S is placed at a predetermined position of the sample support device 5, and the optical arrangement of each X-ray optical element is adjusted so as to be the same as the measurement conditions at the time of the main measurement, that is, the optical axis adjustment. I do. In the preliminary measurement of the mask 9 alone, it is important to irradiate only the mask 9 with X-rays, that is, unlike the main measurement, do not irradiate the opening of the mask 9 with X-rays. It is important that the X-rays do not protrude out of the mask 9 and are not reflected or diffracted from substances other than the mask 9.

That is, in FIG. 3, the incident angle θ0 of the X-ray with respect to the mask 9 (not including the sample S at the present time).
Is set to a predetermined angle corresponding to the sample S, for example, 20 ° to 30 °. Next, in FIG. 1, the arc swing mechanism 7 is operated to adjust the mask 9 so that the mask 9 is inclined at an inclination angle θ1, for example, θ1 = about 45 ° with respect to the ω axis. This adjustment is performed manually in the present embodiment, but can also be performed automatically by attaching a motor or other drive source to the arc swing mechanism 7.

As described above, the inclination of the mask 9, that is, the sample S with respect to the stimulable phosphor 2 at approximately 45 ° is such that the X-ray measurement of the sample S is performed in the tangential direction of the sample surface of the sample S. X-rays from the sample S are detected by the stimulable phosphor 2 over a wide range of diffraction angles from a diffracted X-ray R3 emitted along the sample to a diffracted X-ray R4 emitted along the direction perpendicular to the sample surface of the sample S. This is to make it possible. Therefore,
Due to the long length of the stimulable phosphor 2 in the axial direction (that is, the vertical direction in FIG. 1), the tangential diffraction X-ray R3 and the vertical diffraction can be obtained even when the inclination angle of the sample surface deviates from 45 °. When both X-rays R4 can be detected by the stimulable phosphor 2, the angles may be changed.

After the above setting is completed, the φ rotating device 6 is operated to rotate the mask 9 about the φ axis, that is, in-plane rotation, and the monochromator 3 and the collimator 4 are radiated from the X-ray focal point F. The transmitted X-rays are made incident on a mask 9 that rotates in the plane. At this time, when the Bragg diffraction condition is satisfied between the incident X-ray and the crystal lattice plane of the mask 9, X-ray diffraction occurs in the mask 9.

Since the mask 9 is made of a single crystal material, diffracted X-rays are generated only from a very limited part.
Therefore, several diffraction points are obtained on the surface of the stimulable phosphor 2 as shown in FIG. FIG. 5B shows the relationship between the diffraction points and the diffraction angles. In the figure,
..,... Indicate equal diffraction angle lines corresponding to the diffraction points.

The stimulable phosphor 2 is used in the reader 1 shown in FIG.
0, the scanning optical system 12 is scanned and moved in the XY plane, and the laser beam is radiated for reading. By the calculation of the CPU 28, the diffraction point of FIG. The coordinate position of the X-ray image in the XY plane can be obtained.

The CPU 28 sums, for example, integrates the intensities of the diffracted X-ray image for the mask 9 thus obtained for each equal diffraction angle line, thereby obtaining each diffraction angle as shown in FIG. The X-ray intensity for each (2θ) can be calculated. In FIG. 5C,...
Corresponds to each of the equal diffraction angle lines in FIG.

In this embodiment, the CPU 28
The diffraction X-ray image relating to the mask 9, that is, the coordinate position of each diffraction point B is stored in the memory 29 (see FIG. 2) as a blank area.

(Main Measurement on Sample S) Next, FIG.
As shown in FIG. 4A and FIG. 4B, a mask 9 is mounted on the surface to be measured of the sample S by bonding or another method. next,
The sample S is attached to a predetermined position of the φ rotation device 6 of the sample support device 5 in FIG. Then, under the same optical conditions as in the preliminary measurement, except that the X-ray also strikes the opening 15 of the mask 9, the φ rotation device 6 is operated to rotate the sample S about the φ axis, That is, the X-rays emitted from the X-ray focal point F and passing through the monochromator 3 and the collimator 4 are made incident on the sample S rotating in the plane while being rotated in the plane.

At the time of the X-ray incidence, as shown in FIG. 4A, the incident X-ray R0 irradiates an area wider than the opening 15 of the mask 9 and irradiates the mask 9 in a portion other than the opening 15. R0 does not reach the sample S, and only the X-ray R0 that has passed through the opening 15 reaches the sample S. This allows
The X-ray R0 is applied only to the minute region S0 of the sample S corresponding to the area of the opening 15.

As described above, according to the X-ray measuring apparatus of the present embodiment, in particular, the X-ray exposure apparatus 1, the mask 9 having the opening 15 is provided in front of the sample S, and the mask 9 is formed of a single crystal material. X irradiated on the sample S
Among the lines R0, those that hit portions other than the openings 15 of the mask 9 do not reach the sample S, but the X-rays R0 reaching the sample S
Is limited only to a region corresponding to the opening 15 formed in the mask 9. For this reason, it is possible to measure only a partial area of the sample S, usually only a minute area.

In this case, when the X-ray R0 hits the mask 9, diffracted X-rays may also be generated from the mask 9, but in this embodiment, since the mask 9 is formed of a single crystal material, When the mask 9 is irradiated with X-rays, the diffracted X-rays generated from the mask 9 are limited to a local diffraction angle, and the diffracted X-rays are
Can be easily distinguished from diffracted X-rays.

According to the X-ray measuring apparatus according to the present embodiment, in particular, the X-ray exposure apparatus 1, the X-ray irradiation area on the sample S, that is, the measurement area S0 of the sample is determined by the opening 15 formed in the mask 9. It is possible to measure a partial area of the sample without using the collimator 4. Also,
Even when the collimator 4 is used, the partial area S0 of the sample S can be measured without disposing the collimator 4 at a specific position close to the sample S with high positional accuracy.

Further, by making the size of the opening 15 formed in the mask 9 narrower, it is possible to make a finer area smaller than the case where the collimator 4 is used, as the measurement area S0. Also, in the present embodiment, the inclined surface T
The provided, yet equal the inclination angle theta _T of the inclined surface T to X-ray incident angle theta, or because more is set smaller, the opening as shown in FIG. 6 (a) and 6 (b) 1
5 has more X-rays R than in the case where no inclined surface is provided.
0 can be taken into the opening 15, so that a large amount of X-rays R0 can be supplied to the measurement area S0 of the sample S.

In FIG. 4A, X incident on the sample S
Since the line R0 is limited to the minute region S0, the number of crystal grains included in the irradiation field is small. Therefore, diffracted X-rays generated from these crystal grains travel in a specific diffraction angle direction, and therefore, a zero-dimensional X-ray detector such as a SC (Scintillation Counter) or a PSPC (Position Sensiti).
In one-dimensional X-ray detectors such as a ve Proportional Counter, the X-ray detectors must be scanned and moved in order to capture the diffracted X-rays.

On the other hand, according to the present embodiment using the stimulable phosphor 2 which is a two-dimensional X-ray detector, such X-ray
Even if the scanning movement of the line detector is not performed, the minute area S of the sample S
X-ray diffraction from zero can be captured two-dimensionally. Thereby, one rotating system can be omitted as compared with the case of using a 0-dimensional X-ray detector, a one-dimensional X-ray detector, or the like.
The structure of the device can be simplified and the measurement time can be shortened.

When the X-ray exposure processing for the stimulable phosphor 2 is performed by the X-ray exposure apparatus 1 of FIG. 1 as described above, the surface of the stimulable phosphor 2 is placed on the surface of FIG. As shown, diffraction points a, b, c,..., F are formed at positions exposed by the diffracted X-rays from the sample S. Further, the diffraction points shown in FIG. 5A are formed so as to overlap with each other, as indicated by “x”, corresponding to the diffraction X-rays from the mask 9 covering the sample S.

FIG. 6B shows the diffraction points and FIG.
The relationship with the equi-diffraction angle lines shown in FIG. Diffraction points a, b,... Corresponding to sample S
.., F are listed on the equi-diffraction angle line,...

The stimulable phosphor 2 that has been subjected to the exposure process is subjected to a reading process by the reading device 10 shown in FIG.
Then, the CPU 28 in the arithmetic unit 26 individually obtains the X-Y coordinate position and the X-ray intensity of the diffraction X-ray image formed on the surface of the stimulable phosphor 2, and further obtains the X-rays belonging to the same diffraction angle. The sum of the intensities is calculated, for example, by integration.

Now, suppose that without any correction,
,..., Or by integrating the X-ray intensity for each of the other equal diffraction angles, the diffracted X-rays from both the mask 9 and the sample S are the same as shown in FIG. When the diffraction angles are the same, they are added to form a high peak. When the diffraction angle of the diffraction X-ray from the sample S is different from the diffraction angle of the diffraction X-ray from the mask 9, A new peak appears at a position different from.

The X-ray intensity distribution shown in FIG. 6C does not show the correct X-ray intensity distribution for the sample S because it also contains the diffraction X-ray information of the mask 9. In order to solve this inconvenience, the CPU 28 treats the coordinate position set as the blank area B (see FIG. 5B) in the previous preliminary measurement as not included in the above-described integration operation, and Is integrated for each equal diffraction angle line.

As a result, the X-ray intensity distribution as shown in FIG. 7, that is, the overlapping distribution curve of FIG.
(C) minus the distribution curve for mask 9;
That is, an X-ray intensity distribution corresponding to the excluded one is obtained. This measurement result is shown in FIG.
Is displayed as an image on the screen of the printer, or is printed on a printing material by the printer 33. The observer can know the crystal structure and the like of the sample S by examining the peak position and the peak height in the graph of FIG.

As described above, in the present embodiment, FIG.
In FIG. 4A and FIG. 4B, the diffraction X-rays from the mask 9 covering the sample S are set as blank areas and excluded from the target of the integration operation, so that they are not affected by the diffraction X-rays from the mask 9. The X-ray intensity distribution can be accurately obtained based only on the diffracted X-rays from the sample S.

FIG. 8 shows a main portion of another embodiment of the X-ray measuring apparatus according to the present invention, in particular, a portion of the sample S and the mask 9. Other parts in this embodiment can be the same as those shown in FIGS. In the present embodiment, the opening 15 is formed as a simple columnar space without providing the inclined surface T as shown in FIG.

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 described above, the plane shape of the opening 15 is circular, but the plane shape of the opening 15 can be elliptical, oval, square, rectangular, or any other shape. .

In the reading device 10 shown in FIG.
Although the stimulable phosphor 2 is supported in a flat surface by the support 11, the stimulable phosphor 2 is not limited to a flat surface, but may be supported in a cylindrical shape, for example. In this case, the scanning optical system 12 is arranged so as to be rotatable on the central axis of the stimulable phosphor 2 and move linearly on the central axis. The scanning optical system 12 is rotated around the central axis to perform main scanning in the circumferential direction of the cylindrical stimulable phosphor 2, and further linearly moves on the central axis to thereby provide a stimulable phosphor. 2 is linearly sub-scanned, whereby the entire surface of the stimulable phosphor 2 is read and scanned.

[0076]

As described above, the X according to the present invention is
According to the X-ray measurement apparatus and the X-ray measurement method, a mask having an opening is arranged in front of the sample and the mask is formed of a single crystal material. The part that hits the portion does not reach the sample, and the X-rays that reach the sample are limited to only the region corresponding to the opening formed in the mask. Therefore, the measurement can be performed on only a part of the sample.

When X-rays are applied to a mask, diffracted X-rays may also be generated from the mask. In the present invention, since the mask is formed of a single crystal material, the mask is irradiated with X-rays. At this time, the diffracted X-ray generated from the mask is limited to a local diffraction angle, and the diffracted X-ray can be easily distinguished from the diffracted X-ray from the sample to be measured.

Further, since the X-ray irradiation area on the sample, that is, the measurement area of the sample is determined by the opening formed in the mask, a partial area of the sample can be measured without using a collimator. Further, even when a collimator is used, it is possible to measure a partial area of the sample without accurately arranging the collimator at a specific position close to the sample.

Further, by reducing the size of the opening formed in the mask, a narrower area can be used as the measurement area than when a collimator is used.

[Brief description of the drawings]

FIG. 1 is a perspective view, partially cut away, showing an embodiment of an X-ray exposure apparatus which is one of the constituent elements of an X-ray measurement apparatus according to the present invention.

FIG. 2 is a perspective view showing an embodiment of a reading device which is another component of the X-ray measuring device according to the present invention.

FIG. 3 is a plan view of the X-ray exposure apparatus of FIG. 1 when viewed from the direction of arrow III.

FIG. 4 is a diagram showing a main part of the X-ray exposure apparatus of FIG. 1,
(A) is a sectional view showing a sectional structure of a main part thereof,
(B) is a plan view showing the planar structure of the main part.

5A and 5B are diagrams illustrating an example of a diffraction X-ray image formed on the surface of a two-dimensional X-ray detector with respect to a mask, wherein FIG. 5A illustrates only the diffraction X-ray image, and FIG. The relationship between a line image and an equal diffraction angle line is shown, and (c) shows an X-ray intensity distribution diagram.

FIG. 6 is a diagram showing an example of a diffracted X-ray image formed on the surface of a two-dimensional X-ray detector for both a sample and a mask, where (a) shows only the diffracted X-ray image and (b) ) Shows the relationship between the diffraction X-ray image and the equal diffraction angle, and (c) shows the X-ray intensity distribution diagram.

FIG. 7 is a graph showing an example of a diffraction X-ray intensity distribution diagram concerning only the sample, which is obtained by calculation based on the diffraction X-ray image shown in FIG.

FIG. 8 is a view showing a main part of another embodiment of the X-ray measuring apparatus according to the present invention, and showing a portion corresponding to the portion shown in FIG. 4; It is a sectional view showing, and (b) is a top view showing the plane structure of the part.

[Explanation of symbols]

 Reference Signs List 1 X-ray exposure apparatus (X-ray measuring apparatus) 2 Stimulable phosphor (two-dimensional X-ray detecting means) 4 Collimator 9 Mask 10 Reader 15 Opening D1, D2 Opening dimension F X-ray focal point K Corner R0 Incident X-ray R1 Diffracted X-ray R3 Tangential diffracted X-ray R4 Vertical diffracted X-ray S Sample S0 Measurement area X Sample center

Claims (6)

[Claims] 1. An X-ray source comprising: an X-ray source for generating X-rays for irradiating a sample; X-ray detection means for detecting X-rays diffracted by the sample; and calculation means for performing an operation based on the detection result An X-ray measurement apparatus, comprising: a mask formed of a single crystal material, covering an X-ray irradiation surface of the sample, and provided with an opening through which X-rays pass. 2. The apparatus according to claim 1, wherein the opening has an inclined surface having an inclination angle smaller than an incident angle of the X-ray so as not to block an optical path of the X-ray entering and exiting the sample, and facing the sample. An X-ray measuring apparatus characterized in that an X-ray irradiation area of a sample is determined based on the size of the opening on the side. 3. The method according to claim 1, wherein
An X-ray measuring apparatus, wherein the line detecting means is a two-dimensional X-ray detector. 4. A mask formed of a single crystal material and having an opening through which X-rays pass is arranged on an X-ray irradiation surface of a sample, and X-rays generated from an X-ray source are applied to a region of the mask including the opening. X-ray detection means detects diffracted X-rays from an X-ray irradiation area including the opening, and subtracts the X-ray diffracted by the mask from the detection result, thereby diffracting the sample to diffract the opening of the mask. An X-ray measurement method comprising detecting X-rays that have passed. 5. The opening according to claim 4, wherein the opening has an inclined surface having an inclination angle smaller than an incident angle of the X-ray so as not to interrupt an optical path of the X-ray entering and exiting the sample. X-ray measuring method characterized in that the X-ray irradiation area of the sample is determined according to the size of the side opening. 6. The method according to claim 4, wherein
An X-ray measuring method, wherein the line detecting means is a two-dimensional X-ray detector.