JP2001141674A - Sample holder for measuring diffraction of obliquely emitted x-rays and apparatus and method for measuring diffraction of obliquely emitted x-rays using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To measure a diffraction pattern having a desired S/B ratio by reducing the scattering of air around a sample by a simple method without scaling up an apparatus in the case of the measurement of the diffraction of obliquely emitted X-rays. SOLUTION: A sample holder 15 for measuring the diffraction of obliquely emitted X-rays is constituted of a container 14 holding a sample 3 therein, and an atmosphere control means 13 for controlling the atmosphere in the container 14. An X-ray incident window 11 for permitting primary X-rays 4 to transmit to allow the same to be incident on the sample 3, and an X-ray emitting window 12 for permitting diffracted X-rays to transmit to emit the same to the outside, are formed to the container 14 so as to be separated mutually. When the diffraction of obliquely emitted X-rays is measured, primary X-rays 4 are emitted from an X-ray source 9 in such a state that the atmosphere in the container 14 holding the sample 3 therein is controlled by the atmosphere control means 13 to be diffracted by the sample 3, and the diffracted X-rays 5 are detected and recorded by an X-ray detector 6 to measure the diffraction pattern of the sample 3.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oblique emission X-ray diffraction measurement sample holder used for oblique emission X-ray diffraction measurement for analyzing the structure of a polycrystalline thin film sample, and an oblique emission X-ray using the same. The present invention relates to an X-ray diffraction measurement apparatus and an oblique emission X-ray diffraction measurement method using the same.

[0002]

2. Description of the Related Art In recent years, thin film materials have been used in various electronic devices and play an important role in determining the characteristics of electronic devices. Therefore, appropriate evaluation of the structure of the thin film material and the state of the surface or interface of the thin film material is a key point in developing a new device.

When X-rays are used as a method for evaluating a thin film material, a method for evaluating a thin film material using X-rays is frequently used because of the advantage that a sample to be evaluated can be measured nondestructively.

In the method of evaluating a thin film material using X-rays, in addition to the above-mentioned advantages, it is necessary to obtain not only information on the crystal structure of the thin film material but also information on the surface density, film thickness and roughness of the thin film material. There is an advantage that can be.

[0005] In the conventional method of evaluating a thin film material using X-rays, the measurement arrangement of the thin film material for X-rays is roughly classified into the following two types of arrangements. (1) An arrangement in which X-rays are incident on the surface of the thin film material at a low angle (hereinafter referred to as an oblique incidence arrangement). (2) X-rays incident on the thin film material are applied to the surface of the thin film material. As described above, the thin-film material can be measured with high sensitivity by setting the thin-film material to the oblique incidence configuration or the oblique emission configuration. It is possible. In particular, when the arrangement of the thin film material is an oblique emission arrangement, it is possible to evaluate a minute region in the thin film material by appropriately selecting the probe diameter of the X-ray incident on the thin film material.

[0006] For this reason, when evaluating a minute area in a thin film material, an oblique emission arrangement is generally used as a measurement arrangement of the thin film material.

Hereinafter, the X-ray diffraction measurement of the thin film material in the oblique emission configuration will be described. In the following description, the X-ray diffraction measurement of the thin film material in the oblique emission configuration is particularly referred to as oblique emission X-ray diffraction measurement.

FIG. 4 is a diagram showing an example of a configuration of a conventional oblique emission X-ray diffraction measuring apparatus, showing a configuration around a sample to be evaluated.

As shown in FIG. 4, in the present configuration example, a sample 3 having a thin film 1 formed on a substrate 2 and an X-ray source 9 for emitting a single-wavelength primary X-ray 4 to the sample 3 are provided. , X-ray source 9
Irradiating area limiting means 8 for limiting the irradiating area of the primary X-rays 4 radiated from the sample 3 to the sample 3, and the emission angle α of the diffracted X-rays 5 diffracted at the crystal lattice plane 7 in the sample 3 with respect to the surface of the sample 3 Angle limiting means 10 for limiting the angle
And the diffracted X-rays 5 that have passed through the emission angle limiting means 10 and the angle of the detected diffracted X-rays 5 with respect to the incident direction of the primary X-rays 4 (hereinafter referred to as diffraction angle 2θ).
And an X-ray detector 6 for measuring and recording the X-ray intensity.

As the X-ray source 9, various types of X-ray tubes, monochromatic synchrotron radiation, and the like are used. The primary X-rays 4 emitted from the X-ray source 9 are preferably parallel beams, and the divergence angle of the parallel beams is 0.5.
° or less.

The irradiation area limiting means 8 includes a slit system including one or a plurality of slits, a condensing system including one or a plurality of X-ray reflecting mirrors, various collimators, and an X-ray using a capillary. A conduit or the like is used. The irradiation area of the primary X-ray 4 to the sample 3 which is limited by the irradiation area limiting means 8 is appropriately selected in a range of about several μm to several mm.

The sample 3 is held by a goniometer (not shown) having a rotating mechanism, and can be rotated by the rotating mechanism of the goniometer. Thereby, the sample 3
Of the primary X-rays 4 with respect to the surface of the sample 3 and the emission angle α of the diffracted X-rays 5 with respect to the surface of the sample 3 can be freely set.

The X-ray detector 6 operates in conjunction with the rotation of the sample 3,
The sample 3 is installed so as to rotate around the rotation axis. For the X-ray detector 6, a normal scintillation counter, a proportional counter, a PSPC (position-sensitive proportional counter), an imaging plate, or the like is used. When the detector is used, the diffracted X-ray 5 is detected without moving the X-ray detector 6.

The emission angle limiting means 10 is installed so as to rotate in conjunction with the rotation of the sample 3 and to rotate around the rotation axis of the sample 3, whereby the diffracted X-ray 5 Is kept within a certain range.
In addition, a slit, a blocking member, or the like is used for the emission angle limiting unit 10.

When measuring the thin film 1, it is necessary to set the incident angle ω and the outgoing angle α so that the outgoing angle α of the diffracted X-rays 5 with respect to the surface of the sample 3 is low.
By setting the output angle α of the diffracted X-rays 5 with respect to the surface of the sample 3 to be low, the information from the surface of the sample 3 is emphasized.
Can be measured.

Hereinafter, the oblique emission X configured as described above will be described.
The operation of the line diffraction measurement device will be described.

When primary X-rays 4 of a single wavelength are radiated from the X-ray source 9, the primary X-rays 4 are irradiated on the sample 3 by limiting the irradiation area on the sample 3 by the irradiation area limiting means 8. . The primary X-rays 4 incident on the sample 3 are diffracted on the crystal lattice plane 7 of the sample 3 and emitted as diffracted X-rays 5.

In this conventional example, the rotation of a goniometer (not shown) on which the sample 3 is placed is adjusted so that the angle of emergence α of the diffracted X-rays 5 with respect to the surface of the sample 3 becomes low. The incident angle ω of the primary X-ray 4 with respect to the surface is fixed at a predetermined angle.

Of the diffracted X-rays 5 emitted from the sample 3,
The emission angle α is limited by the emission angle limiting means 10, and the diffracted X-rays 5 passing through the emission angle limiting means 10 reach the X-ray detector 6.

When the diffracted X-rays 5 reach the X-ray detector 6,
The X-ray detector 6 detects the diffracted X-rays 5 and measures and records the diffraction angle 2θ and the X-ray intensity of the detected diffracted X-rays 5.

Since the angle of emergence α of the diffracted X-rays 5 with respect to the surface of the sample 3 is set so as to be low, the diffraction peak of the thin film 1 is detected in the measured diffraction pattern. become.

[0022]

However, in the conventional oblique emission X-ray diffraction measuring apparatus described above, since primary X-rays are radiated to the sample surface in the air,
Air scattering occurs due to the X-rays passing through the gap.

Such air scatter is detected together with the diffracted X-rays by the X-ray detector, and as a result, the oblique emission X-rays are detected.
The background in the line diffraction measurement becomes large.

In the oblique emission X-ray diffractometer, since the irradiation area of the primary X-ray to the sample is limited, the intensity of the diffracted X-ray diffracted on the surface of the sample is weak, so that the background can be sufficiently reduced. To the desired S / B
Measuring a diffraction pattern with a ratio is an important issue.

As a method of removing the air scattering, there is a method of evacuating the periphery of the sample. For example, the technique is disclosed in JP-A-6-102213.

However, in the device disclosed in JP-A-6-102213, since the X-ray transmission region is provided over a range of 180 ° larger than the measurement region, the oblique emission X-ray diffraction measurement is not performed. The configuration is not always optimal for reducing the background. In addition, since the configuration is very large and a dedicated device is required, there is a problem that oblique emission X-ray diffraction measurement cannot be easily performed.

The present invention has been made in view of the above-mentioned problems of the prior art, and when performing oblique-emission X-ray diffraction measurement, a sample can be obtained by a simple method without increasing the size of the apparatus. A sample holder for oblique emission X-ray diffraction measurement capable of measuring a diffraction pattern having a desired S / B ratio by reducing ambient air scattering, an oblique emission X-ray diffraction measuring apparatus using the same, and It is an object of the present invention to provide an oblique emission X-ray diffraction measurement method using the same.

[0028]

According to the present invention, a primary X-ray is incident on a surface of a sample.
The output direction of the diffracted X-rays whose rays are diffracted on the surface of the sample is defined at an angle smaller than a predetermined angle with respect to the surface of the sample, and the diffracted X-rays are incident on the incident direction of the primary X-rays. A sample holder for oblique emission X-ray diffraction measurement used for oblique emission X-ray diffraction measurement for measuring an emission angle and an X-ray intensity, wherein the sample holder is configured to be able to hold the sample therein and transmits the primary X-ray. A container in which an X-ray entrance window for allowing the sample to be held inside and an X-ray exit window for transmitting the diffracted X-ray and emitting the same to the outside are formed separately from each other; Atmosphere control means for controlling the atmosphere inside the container.

The atmosphere control means may be configured to evacuate the inside of the container when measuring the emission angle and the X-ray intensity.

Further, the atmosphere control means is characterized in that the inside of the container is evacuated using a vacuum pump.

Further, the atmosphere control means replaces the air inside the container with helium when measuring the emission angle and the X-ray intensity.

An oblique emission X-ray diffraction measuring apparatus using the oblique emission X-ray diffraction measurement sample holder, comprising: an X-ray source for emitting the primary X-ray;
Irradiation area limiting means for limiting the irradiation area of the ray, and holding the sample holder for oblique emission X-ray diffraction measurement, from the X-ray source through the irradiation area limiting means and the X-ray entrance window, The primary X-rays incident on the sample are:
Defining means for defining to be diffracted at an angle smaller than a predetermined angle with respect to the surface of the sample,
While diffracting on the surface of the sample, detecting the diffracted X-rays emitted from the X-ray exit window to the outside of the oblique emission X-ray diffraction measurement sample holder, and detecting the diffracted X-rays, An X-ray detector for measuring and recording the emission angle and the X-ray intensity with respect to the incident direction of the primary X-ray.

In the oblique-emission X-ray diffraction measuring method using the oblique-emission X-ray diffraction measuring apparatus, the atmosphere in the container of the oblique-emission X-ray diffraction measurement sample holder is controlled by the atmosphere control means. Controlling, radiating the primary X-rays by the X-ray source, limiting an irradiation area of the primary X-rays to the sample by the irradiation area limiting means, and controlling the irradiation from the X-ray source by the defining means. Defining that the primary X-rays incident on the sample through the area limiting means and the X-ray incident window are diffracted at an angle smaller than a predetermined angle with respect to the surface of the sample; The X-ray detector detects the diffracted X-ray diffracted on the surface of the sample and emitted from the X-ray exit window to the outside of the oblique emission X-ray diffraction measurement sample holder, and the detected X-ray is detected. diffraction Line, characterized by measuring and recording the emission angle and the X-ray intensity with respect to the incident direction of the primary X-ray.

(Function) In the present invention configured as described above, the sample holder for oblique emission X-ray diffraction measurement comprises a container for holding a sample inside, and an atmosphere control for controlling the atmosphere inside the container. And primary X-rays are transmitted through an X-ray entrance window provided in the container, are incident on a sample held inside the container, and diffracted X-rays diffracted by the sample are The light is transmitted through an X-ray emission window provided in the container and emitted to the outside of the container.

Here, the oblique emission X-ray diffraction measurement is performed in a state where the atmosphere in the container holding the sample is controlled by the atmosphere control means.
Air scattering around the sample that causes the background is removed, and as a result, a diffraction pattern having a good S / B ratio is measured.

[0036]

Embodiments of the present invention will be described below with reference to the drawings.

FIGS. 1A and 1B are views showing an embodiment of a sample holder for oblique emission X-ray diffraction measurement according to the present invention, wherein FIG. 1A is an external perspective view, and FIG. In this embodiment, the sample 3 to be evaluated is fixed inside in advance,
It is assumed that an X-ray source (not shown) emits primary X-rays 4 to a sample 3 fixed inside.

As shown in FIG. 1, in the present embodiment, a container 14 for holding the sample 3 therein, and an atmosphere control means 13 for controlling the atmosphere inside the container 14 are provided.

Further, in the container 14, an X-ray entrance window 11 for transmitting the primary X-rays 4 radiated from an X-ray source (not shown) and allowing the primary X-rays 4 to enter the sample 3 fixed inside the container 14 is provided. An X-ray emission window 12 for transmitting the diffracted X-rays 5 incident on the sample 3 as the primary X-rays 4 and diffracted by the sample 3 and emitting the X-rays 5 to the outside of the container 14 is formed separately from each other. I have.

The X-ray entrance window 11 and X-ray exit window 12
Also has a function of separating the atmosphere between the inside and the outside of the container 14.

In this embodiment, the incident angle of the primary X-rays 4 with respect to the surface of the sample 3 is the incident angle ω, and the angle of the diffracted X-rays 5 measured from the surface of the sample 3 is the emission angle α.

As the material used for the X-ray incident window 11, a material that transmits the primary X-rays 4 is appropriately selected, and for example, metal Be foil, Al-deposited mylar, or Kapton (heat-resistant polymer film) is used. .

The size of the X-ray entrance window 11 is the primary X-ray window.
Based on the beam shape and the incident angle ω of the line 4, the size is set so that the primary X-ray 4 enters the sample 3 without being blocked by the X-ray entrance window 11.

As the material used for the X-ray exit window 12, a material that transmits the diffracted X-rays 5 is appropriately selected, and the same material as that for the X-ray entrance window 11 described above is used.

The size of the X-ray emission window 12 is
When a thin film is formed on the surface of the sample 3, the size is set so that the emission angle α of the diffracted X-rays 5 with respect to the surface of the sample 3 becomes small, so that the thin film can be measured.

The inside of the container 14 is evacuated by a vacuum pump (not shown) such as a rotary pump through the atmosphere control means 13 to control the atmosphere inside the container 14 to a vacuum state. The atmosphere inside the container 14 is 0.1
By setting a low vacuum of about 3 to 1.33 Pa, it is possible to prevent the X-rays generated near the sample from being scattered by the primary X-rays 4 in the air.

The atmosphere control means 13 can also control the atmosphere inside the container 14 by replacing the air inside the container 14 with He or the like. When the air inside the container 14 is replaced with He or the like, there is an advantage that even if the inside of the container 14 is at atmospheric pressure, X-ray air scattering can be prevented.

As the material of the portion other than the X-ray entrance window 11 and the X-ray exit window 12 of the container 14, an optimum material may be appropriately selected according to the atmosphere inside the container 14, and usually, Al or the like is used. Is used. Also, a transparent material such as glass can be used if the problem of strength is solved. When a transparent material such as glass is used, there is an advantage that the state inside the container 14 can be observed from the outside.

In the oblique emission X-ray diffraction measurement sample holder configured as described above, first, the sample 3 is fixed to a sample table (not shown) or the like inside the container 14. Controls the atmosphere inside the container 14,
After that, the measurement of the sample 3 is started.

An oblique emission X-ray diffraction measuring apparatus using the oblique emission X-ray diffraction measuring sample holder shown in FIG. 1 will be described below.

FIG. 2 is a view showing an embodiment of an oblique emission X-ray diffraction measuring apparatus using the oblique emission X-ray diffraction measuring sample holder shown in FIG. .

In this embodiment, the same parts as those of the conventional oblique emission X-ray diffraction measuring apparatus shown in FIG.
The same reference numerals are given and the detailed description is omitted.

As shown in FIG. 2, in this embodiment, a sample holder 15 for oblique emission X-ray diffraction measurement in which a sample 3 having a thin film 1 formed on a substrate 2 is fixed, and an oblique emission X-ray diffraction measurement X-ray source 9 that emits primary X-rays 4 of a single wavelength to the sample 3 fixed inside the sample holder 15 for irradiation, and an irradiation area of the primary X-rays 4 emitted from the X-ray source 9 to the sample 3 Irradiating area limiting means 8 for limiting the diffraction X-rays 5 diffracted on the crystal lattice plane 7 of the sample 3, and detecting the diffracted X-rays 5 with respect to the incident direction of the primary X-rays 4. An X-ray detector 6 for measuring and recording an emission angle (hereinafter referred to as a diffraction angle 2θ) and an X-ray intensity is provided.

The sample holder 15 for oblique emission X-ray diffraction measurement is
It is held by a goniometer (not shown), which is a defining means having a rotating mechanism, and is rotatable by the rotating mechanism of the goniometer. Thereby, the incident angle ω of the primary X-ray 4 with respect to the surface of the sample 3 and the emission angle α of the diffracted X-ray 5 with respect to the surface of the sample 3 can be freely set.

The oblique emission X configured as described above will now be described.
The operation of the line diffraction measurement device will be described with reference to FIGS.

First, the sample 3 is fixed to a sample stage (not shown) in the container 14 of the sample holder 15 for oblique emission X-ray diffraction measurement, and the sample holder 15 for oblique emission X-ray diffraction measurement to which the sample 3 is fixed is mounted. Is fixed to a sample stage (not shown) of the oblique emission X-ray diffraction measuring apparatus.

Next, the atmosphere control means 13 controls the container 1
The atmosphere inside 4 is controlled.

Next, the primary X-rays 4 having a single wavelength
Is emitted, and the primary X-rays 4 whose irradiation area to the sample 3 is restricted by the irradiation area restricting means 8 are transmitted through the X-ray entrance window 11 and the container 14 of the sample holder 15 for oblique emission X-ray diffraction measurement.
The light is incident on the sample 3 fixed inside.

The primary X-rays 4 incident on the sample 3
Are diffracted by the crystal lattice plane 7 of the sample, and are transmitted as diffracted X-rays 5 through the X-ray emission window 12 to the outside of the oblique emission X-ray diffraction measurement sample holder 15.

In the present embodiment, the output angle α of the diffracted X-rays 5 with respect to the surface of the sample 3 is reduced to a low angle smaller than a predetermined angle by a rotating mechanism of a goniometer (not shown) on which the sample 3 is installed. Thus, the incident angle ω of the primary X-rays 4 on the surface of the sample 3 is fixed at a predetermined angle.

When the diffracted X-ray 5 emitted to the outside of the oblique emission X-ray diffraction measurement sample holder 15 reaches the X-ray detector 6, the X-ray detector 6 detects the diffracted X-ray 5 and detects the X-ray. The diffraction angle 2θ and the X-ray intensity of the diffracted X-ray 5 are measured and recorded.

In the present embodiment, the diffraction pattern of the sample 3 is measured in a state where the atmosphere inside the container 14 holding the sample 3 is controlled by the atmosphere control means 13.
Air scattering due to X-rays generated from the periphery of the sample 3 can be removed without increasing the size of the apparatus.

[0063]

Embodiments of the present invention will be described below.
It should be noted that the present invention is not limited to the examples described below, as long as the object of the present invention is achieved.
Each component may be replaced or the design may be changed.

(First Embodiment) In this embodiment, the diffraction pattern of the sample 3 was measured under the following measurement conditions using the oblique emission X-ray diffraction measuring apparatus shown in FIG.

First, a sample holder 15 for oblique emission X-ray diffraction measurement in which the sample 3 is fixed inside the container 14 is fixed to a sample stage (not shown) of the present apparatus, and the air inside the container 14 is blown by a rotary pump. It is evacuated to control the degree of vacuum inside the container 14 to about 0.13 to 1.33 Pa.

Subsequently, the primary X-ray 4
The diffraction X-rays 5 are emitted with the incident angle ω of 57.5 ° fixed at 57.5 °, and the diffraction angle 2θ and the X-ray intensity of the diffraction X-rays 5 are set to 300.
The diffraction pattern of the sample 3 is measured by measuring and recording for 2 seconds.

A sample 3 was prepared by forming a palladium thin film 1 having a thickness of about 30 nm on a substrate 2 made of quartz by vacuum evaporation.

The sample holder 1 for oblique emission X-ray diffraction measurement
5, the size of the X-ray entrance window 11 is L1 = 15 mm,
t1 = 15 mm, and the size of the X-ray emission window 12 is L
Those with 2 = 12 mm and t2 = 15 mm were used.

The X-ray entrance window 11 and the X-ray exit window 12
Is a metal Be foil, and the X-ray entrance window 1 of the container 14 is
The material of the parts other than 1 and the X-ray emission window 12 is Al.

As the X-ray source 9, a rotating cathode X-ray tube using Cr as a cathode was driven at a tube voltage of 40 kV and a tube current of 200 mA. The X-ray focus is a line focus and the effective focus width is 0.0
5 mm, length 10 mm.

The irradiation area limiting means 8 has a width of 0.1
A 5 mm slit was used and this slit was set at a position 100 mm from the X-ray source 9. The irradiation area limiting means 8 is located at a position 85 mm from the sample 3.

The X-ray detector 6 has a linear PSP.
Using C, this PSPC was placed at a position 300 mm from Sample 3.

As a result of measuring the diffraction pattern of the sample 3 under the above-described measurement conditions, the diffraction pattern shown in FIG. 3 was measured by the X-ray detector 6.

FIG. 3 is a diagram showing a diffraction pattern measured by the X-ray detector 6 shown in FIG.

In FIG. 3, the diffraction pattern of the sample 3 measured in this embodiment is the diffraction pattern A.

As shown in FIG. 3, in this example, a diffraction peak of Pd (111) was observed near the diffraction angle 2θ of 61.3 °, confirming that the palladium thin film 1 was measured. . At this time, diffraction X on the surface of sample 3
The exit angle α of the line 5 was about 3.8 °.

(First Comparative Example) In this comparative example, the diffraction pattern of the sample 3 was measured without using the sample holder 15 for oblique emission X-ray diffraction measurement, as compared with the first embodiment. . The other measurement conditions are the same as in the first embodiment. As a result, a diffraction pattern represented by the diffraction pattern B shown in FIG. 3 was measured.

As shown in FIG. 3, the diffraction pattern A measured in the first embodiment has a lower background angle at a diffraction angle 2θ than the diffraction pattern B measured in the comparative example. Thus, it was confirmed that the air scattering around the sample 3 was removed. Further, it was confirmed that the diffraction pattern A measured in the first example had almost no decrease in the diffraction peak of Pd (111) as compared with the diffraction pattern B measured in the present comparative example.

(Second Embodiment) In the present embodiment, the X-ray incidence windows 11 and X
The material of the X-ray exit window 12 was changed from Be foil to Al vapor-deposited mylar, and the material of the container 14 other than the X-ray entrance window 11 and the X-ray exit window 12 was changed from Al to glass. The diffraction pattern of the sample 3 was measured under the same measurement conditions except that the control method of the atmosphere in the container 14 in the means 13 was changed to a control method of replacing the air inside the container 14 with He.

As a result, a diffraction pattern substantially similar to the diffraction pattern A shown in FIG. 3 was measured. The background on the low-angle side at the diffraction angle 2θ was removed, and the diffraction peak of Pd almost decreased. It was confirmed that it did not.

In this embodiment, since the air in the container 14 in the sample holder 15 for oblique emission X-ray diffraction measurement is replaced with He, a vacuum pump such as a rotary pump is not required, and the inside of the container 14 is eliminated. Has the advantage that the measurement of a diffraction pattern with a reduced background is possible even when is at atmospheric pressure.

(Third Embodiment) In the present embodiment, a diffraction peak of Pd (111) shown in FIG. 3 was used under the following measurement conditions using the same structure as the first embodiment. Has been confirmed to be dependent on the emission angle α.

First, a sample holder 15 for oblique emission X-ray diffraction measurement in which the sample 3 is fixed inside the container 14 is fixed to a sample stage (not shown) of the present apparatus, and the air in the container 14 is exhausted by a rotary pump. Then, the degree of vacuum inside the container 14 is controlled to about 0.13 to 1.33 Pa. Next, sample 3
A diffraction X-ray 5 is emitted with the incident angle ω of the primary X-ray 4 with respect to the surface of the substrate fixed at 58.0 °, and the diffraction angle 2θ and the X-ray intensity of the diffraction X-ray 5 are measured and recorded for 300 seconds. Subsequently, the incident angle ω of the primary X-ray 4 with respect to the surface of the sample 3 is set to 5
From 8 ° to 63 ° in steps of 0.1 °, the angle of incidence ω
Each time is increased by 0.1 °, the diffraction angle 2θ of the diffracted X-ray 5 and the X-ray intensity are measured and recorded for 300 seconds.

By repeating the above operation, the diffraction pattern of the sample 3 is measured, and based on this diffraction pattern,
Fitting is performed by taking the shift amount of the output angle α of the diffracted X-ray 5 with respect to the surface of the sample 3 on the horizontal axis and the diffraction angle 2θ on the vertical axis.

By such a fitting, the thin film 1 made of palladium formed on the substrate 2 made of quartz
Was measured as a surface density of 10.20 g / cm ³ .

[0086]

As described above, in the present invention,
An X-ray entrance window for transmitting a primary X-ray to be incident on the sample held therein, and an oblique emission by transmitting diffracted X-rays diffracted by the sample, the sample being configured to be able to hold the sample inside. A container in which an X-ray emission window for emitting light to the outside of the sample holder for X-ray diffraction measurement is formed separately from each other; and atmosphere control means for controlling an atmosphere inside the container is provided. Oblique emission X-ray diffraction measurement is performed in a state where the atmosphere in the container is controlled by the atmosphere control means, so that air scattering around the sample which causes a background can be removed without increasing the size of the apparatus. As a result, a diffraction pattern having a good S / B ratio can be measured.

[Brief description of the drawings]

FIG. 1 is a view showing an embodiment of a sample holder for oblique emission X-ray diffraction measurement of the present invention, wherein (a) is an external perspective view,
(B) is a sectional view.

FIG. 2 is a cross-sectional view showing one embodiment of an oblique emission X-ray diffraction measurement apparatus using the oblique emission X-ray diffraction measurement sample holder shown in FIG.

FIG. 3 is a diagram showing a diffraction pattern of a sample measured by the X-ray detector shown in FIG.

FIG. 4 is a diagram showing an example of a configuration of a conventional oblique emission X-ray diffraction measuring apparatus.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Thin film 2 Substrate 3 Sample 4 Primary X-ray 5 Diffracted X-ray 6 X-ray detector 7 Crystal lattice plane 8 Irradiation area limiting means 9 X-ray source 11 X-ray entrance window 12 X-ray exit window 13 Atmosphere control means 14 Container 15 Oblique Sample holder for outgoing X-ray diffraction measurement ω Incident angle α Outgoing angle 2θ Diffraction angle

Continued on the front page F term (reference) 2G001 AA01 BA18 CA01 DA01 DA02 DA08 EA09 FA08 GA13 JA14 KA01 KA08 MA05 PA07 QA02 QA10 SA10

Claims (6)

[Claims] 1. A primary X-ray is made incident on a surface of a sample, and an output direction of the diffracted X-ray obtained by diffracting the primary X-ray on the surface of the sample is smaller than a predetermined angle with respect to the surface of the sample. An oblique emission X-ray diffraction measurement sample holder used for oblique emission X-ray diffraction measurement for measuring an emission angle and an X-ray intensity of the diffracted X-ray with respect to an incident direction of the primary X-ray, defined by an angle, An X-ray entrance window for transmitting the primary X-rays and allowing the primary X-rays to enter the sample held therein and transmitting the diffracted X-rays to the outside are configured to be capable of holding the sample therein. A sample holder for oblique emission X-ray diffraction measurement, comprising: a container in which an X-ray emission window for the container is formed separately from each other; and atmosphere control means for controlling the atmosphere inside the container. 2. The oblique emission X-ray diffraction measurement sample holder according to claim 1, wherein the atmosphere control means evacuates the inside of the container when measuring the emission angle and X-ray intensity. A sample holder for oblique emission X-ray diffraction measurement, characterized in that: 3. The oblique-emission X-ray diffraction sample holder according to claim 2, wherein the atmosphere control means evacuates the inside of the vessel using a vacuum pump. Sample holder for diffraction measurement. 4. The sample holder for oblique emission X-ray diffraction measurement according to claim 1, wherein the atmosphere control means uses helium to air inside the container when measuring the emission angle and the X-ray intensity. Oblique emission X characterized by replacing
Sample holder for X-ray diffraction measurement. 5. An oblique emission X-ray diffraction measurement apparatus using the oblique emission X-ray diffraction measurement sample holder according to claim 1, wherein the X-ray radiates the primary X-ray. A source, an irradiation area limiting unit for limiting an irradiation area of the primary X-ray to the sample, and holding the oblique emission X-ray diffraction measurement sample holder, and the irradiation area limiting unit from the X-ray source and The primary X-rays incident on the sample through the X-ray entrance window,
Defining means for defining so as to be diffracted at an angle smaller than a predetermined angle with respect to the surface of the sample; and diffracting at the surface of the sample, and obliquely emitting X-rays from the X-ray exit window. The X-ray detector detects the diffracted X-rays emitted to the outside of the sample holder for diffraction measurement, and measures and records the output angle and X-ray intensity of the detected diffracted X-rays with respect to the primary X-ray incident direction. An oblique emission X-ray diffraction measuring device, comprising: a line detector. 6. An oblique emission X-ray diffraction measurement method using the oblique emission X-ray diffraction measuring apparatus according to claim 5, wherein the atmosphere control means controls the oblique emission X-ray diffraction measurement sample holder. Controlling the atmosphere in the container, radiating the primary X-rays by the X-ray source, restricting the irradiation area of the primary X-rays to the sample by the irradiation area limiting means, The primary X-rays incident on the sample from the radiation source through the irradiation area limiting means and the X-ray incident window are diffracted at an angle smaller than a predetermined angle with respect to the surface of the sample. The X-ray detector diffracts at the surface of the sample,
Detecting the diffracted X-rays emitted from the X-ray exit window to the outside of the oblique emission X-ray diffraction measurement sample holder, and detecting the angle of emission of the detected diffracted X-rays with respect to the incident direction of the primary X-rays And X-ray intensity measurement and recording.