JP2616452B2 - X-ray diffractometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray diffraction measuring apparatus, and more particularly to an X-ray diffraction measuring apparatus capable of obtaining high reproducibility of a measurement result.

[0002]

2. Description of the Related Art Conventionally, when performing energy dispersive X-ray diffraction using white X-rays, a mechanism for causing white X-rays to be incident on an object to be measured and an energy spectrum of diffracted X-rays from the object to be measured are measured. Devices with mechanisms have been used. Such an apparatus is disclosed in, for example, Japanese Patent Application Laid-Open No. 2-145948.
And Japanese Unexamined Patent Publication No. 1-254849.

[0003]

By using a strong X-ray source typified by synchrotron radiation in the above-mentioned measuring apparatus, a weak diffraction of a spectrum from an object to be measured including an extremely small point of interest is performed. When trying to observe the peak, there is a problem that the background of the spectrum is slightly changed every measurement, and the reproducibility of the measurement result is lost.
The object of the present invention is to solve such conventional problems,
Excluding the background component of the spectrum for each measurement,
An object of the present invention is to provide an X-ray diffraction measurement device capable of obtaining high reproducibility of a measurement result.

[0004]

According to the present invention, there is provided a mechanism for inputting white X-rays from an X-ray source to an object to be measured, a mechanism for measuring an energy spectrum of diffracted X-rays from the object to be measured,
An X-ray diffraction measuring apparatus comprising: a mechanism for counting and measuring the intensity of diffracted X-rays from the object to be measured; and a mechanism for rotating the object to be measured to a desired angle.

In the present invention, a movable monochromator is disposed on an optical path between an object to be measured and a diffracted X-ray energy spectrum measuring mechanism, and the diffracted X-ray intensity counting and measuring mechanism detects the diffracted X-rays from the measured object. Being arranged to enter via the movable monochromator, or
A set of movable monochromators is provided on the optical path between the X-ray source and the object to be measured, and the set of movable monochromators transmits monochromatic X-rays to the object under the same optical path as when the set is removed. Preferably, they are arranged to be incident.

[0006]

[Function] The reason why the background of the spectrum changes subtly for each measurement is that the angle at which the X-rays are incident on the DUT varies, and the appearance of multiple reflections inside the DUT changes. is there. The geometrical orientation of the object to be measured with respect to the surface to be measured and, when most of the object to be measured is a single crystal, the crystallographic orientation of the object at the same time, the relative angle with the direction of the incident X-ray must be accurately determined. By keeping it constant, it is possible to completely eliminate the change in the background every measurement.
If the background can be made constant, the background can be easily removed by subtracting or removing the spectrum of the substrate from the spectrum of the sample. The present invention provides a diffraction X from an object to be measured so that the above-described measurement can be performed.
The problem was solved by providing a mechanism for counting and measuring the intensity of the line and a mechanism for rotating the object to be measured to a desired angle in the energy dispersive X-ray diffraction apparatus.

A movable monochromator is disposed on the optical path between the object and the diffraction X-ray energy spectrum measuring mechanism, and the diffraction X-ray intensity counting and measuring mechanism detects the diffracted X-rays from the object by the movable type. A set of movable monochromators is provided so as to be incident via a monochromator, or is provided on the optical path between the X-ray source and the object to be measured. When placed so that monochromatic X-rays enter the object under the same optical path as when it was removed,
The sample orientation can also be adjusted very precisely.

[0008]

Next, embodiments of the present invention will be described with reference to the drawings. Embodiment 1 FIG. 1 is a schematic configuration diagram of a first embodiment of the X-ray diffraction measuring apparatus according to the present invention. The X-ray diffraction measuring apparatus includes a slit 2 as a mechanism for irradiating a sample 4 with white X-rays 1 from an X-ray source, a semiconductor detector 6 for measuring an energy spectrum of a diffracted X-ray 9 from the sample 4, The apparatus includes a set of slits 10 for counting and measuring the intensity of diffracted X-rays from the sample 4 and a lithium ion chamber 11, and a sample stage 3 on which the sample 4 is mounted and which can be tilted and rotated. When this apparatus is used, a sample 4 (for example, a 100 Å-thick polycrystalline Si substrate on a single-crystal Si substrate) in which a white X-ray 1 is set on a sample stage 3 which can be rotated at a small angle and in-plane through a slit 2. When the energy spectrum of the diffracted X-ray 9 guided through the slit 7 and the solar slit 8 to the semiconductor detector 6 set at a fixed diffraction angle 5 direction is incident on the film at a small angle, The sample stage 3 is tilted and rotated while using a set of slits 10 provided at various diffraction angles 12 and a helium ion chamber 11 (a detector suitable for X-ray counting may be used) to thereby make incidence. Angle of X-ray 1 with respect to sample 4 surface and sample 4
Of the single crystal substrate can be adjusted to be constant.

Embodiment 2 FIG. 2 is a schematic structural view of a second embodiment of the X-ray diffraction measuring apparatus according to the present invention. In FIG. 2, a movable monochromator 13 is provided in front of the slit 7 so that the angle of the incident X-ray 1 with respect to the surface of the sample 4 and the crystal orientation of the single crystal substrate of the sample 4 can be adjusted more precisely than in the first embodiment. Then, a set of slits 10 and a helium ion chamber 11 are installed behind the slit. In this case, the movable monochromator 13 is inserted in front of the slit 7 when adjusting the azimuth of the sample 4, and is used by moving from the front of the slit 7 when measuring the energy spectrum.

Embodiment 3 FIG. 3 is a schematic structural view of an X-ray diffraction measuring apparatus according to a third embodiment of the present invention. In FIG. 3, a movable monochromator 15 is inserted in front of the slit 2 in addition to the first embodiment in order to perform more precise sample orientation adjustment than in the second embodiment. At this time, the monochromator 15 must emit monochromatic X-rays 16 at the same position and direction as the incident white X-rays 1. Also in this case, the movable monochromator 15 is inserted in front of the slit 2 when adjusting the azimuth of the sample 4, and is used by moving from the front of the slit 2 when measuring the energy spectrum. Naturally, if the second and third embodiments are used together, the sample orientation can be adjusted very precisely.

FIG. 4 shows a single crystal Si using the first embodiment.
FIG. 4A is a view showing a measurement result when a polycrystalline Si film having a thickness of 100 Å on a substrate is measured. FIG. 4A is a raw energy spectrum. In order to remove the background of this spectrum, a single crystal S without a polycrystalline Si film was used.
By measuring the i-substrate in exactly the same orientation and excluding the spectrum in FIG. 4A, a spectrum in which the background is extremely flat and the diffraction peak is apparent as shown in FIG. 4B is obtained. Such an effect is an effect of the present invention in which the variation of the sample orientation for each measurement can be extremely reduced.

[0012]

As described above, according to the X-ray diffraction measuring apparatus of the present invention, the change in the background of the spectrum for each measurement in the energy dispersive X-ray diffraction is extremely small, and the high reproducibility of the measurement results is obtained. can get. In addition, a movable monochromator is arranged on the optical path between the object to be measured and the diffraction X-ray energy spectrum measurement mechanism, and the diffraction X-ray intensity counting and measuring mechanism uses the movable monochromator for diffracting X-rays from the object to be measured. When a set of movable monochromators is disposed on the optical path between the X-ray source and the object to be measured, and the set of movable monochromators is removed. If the monochromatic X-rays are arranged so as to be incident on the object under the same optical path as above, the orientation of the sample can be adjusted very precisely, and the reproducibility of the measurement results is further improved.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of an embodiment of the present invention.

FIG. 2 is a schematic configuration diagram of another embodiment of the present invention.

FIG. 3 is a schematic configuration diagram of still another embodiment of the present invention.

FIG. 4 is a diagram showing an example of a measurement result when diffracted X-rays are measured using the apparatus of the present invention.

[Explanation of symbols]

 Reference Signs List 1 white X-ray 2 slit 3 sample stage 4 sample 5 diffraction angle 6 semiconductor detector 7 slit 8 solar slit 9 diffracted X-ray 10 set of slits 11 helium ion chamber 13 movable monochromator 15 movable monochromator 16 monochromatic X-ray

Claims (3)

(57) [Claims] 1. A mechanism for inputting white X-rays from an X-ray source to an object to be measured, a mechanism for measuring an energy spectrum of diffracted X-rays from the object to be measured, and a diffraction X-ray from the object to be measured.
An X-ray diffraction measuring apparatus, comprising: a mechanism for counting and measuring the intensity of a line; and a mechanism for rotating the object to be measured at a desired angle. 2. A movable monochromator is arranged on an optical path between an object to be measured and a diffracted X-ray energy spectrum measuring mechanism. 2. The X-ray diffraction measurement apparatus according to claim 1, wherein the X-ray diffraction measurement apparatus is arranged so as to enter through a monochromator. 3. A set of movable monochromators is provided on the optical path between the X-ray source and the object to be measured, and the set of movable monochromators has the same optical path as when the monochromator is removed. 3. The X-ray diffraction measurement apparatus according to claim 1, wherein the X-ray diffraction measurement device is arranged so as to be incident on an object to be measured.