JP2008197025A - Crystal structure analysis method and crystal structure analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To accurately analyze a crystal structure by using X-ray diffraction measurement. <P>SOLUTION: The intensity of diffracted X rays, which are diffracted by an object specimen when applying X rays to the object specimen, is detected on a wide opening angle condition and on a narrow opening angle condition, with a relative ratio between the two taken as "a diffracted X-ray intensity ratio of the object specimen". Further, the intensity of diffracted X rays, which are diffracted by a reference specimen when X rays are applied to the reference specimen with its crystal completeness assured, is detected on a wide opening angle condition and on a narrow opening angle condition, with a relative ratio between the two taken as "a diffracted X-ray intensity ratio of the reference specimen". A reflection index used in X-ray analysis on the reference specimen is selected independently of a reflection index used in X-ray analysis on the object specimen. A value obtained by dividing "the intensity ratio of the object specimen" by "the intensity ratio of the reference specimen" is taken as "a standardized diffracted X-ray intensity ratio" to analyze a crystalline state from this value. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a crystal structure analysis method and a crystal structure analysis apparatus useful for structural analysis of bulk crystals, semiconductor thin film crystals, and multiple quantum well structures. The present invention is particularly useful for examining the incompleteness of heteroepitaxially grown thin film crystals having a large lattice mismatch, the presence / absence of structural deterioration of strained epitaxial thin films and strained superlattice lattices, the extent and characteristics thereof, and the like.

  Conventionally, the importance of the quantity “critical film thickness” (or “critical strain”) is well known in the production of strained epitaxial layers and strained superlattice structures using materials such as InGaAs / GaAs and Si / SiGe. The evaluation of critical film thickness and the evaluation of the lattice relaxation process in the region beyond the critical film thickness were important evaluation targets. The X-ray diffraction method has been frequently used for evaluation of critical film thickness and lattice relaxation process, as well as PL measurement method and TEM analysis method.

  However, the critical film thickness values evaluated by these various evaluation methods generally do not coincide with each other, which is one of the causes of the inconsistency, and the conventional X-ray diffraction evaluation is more sensitive to structural degradation than other evaluation methods. (IJFritz, PLGourley, and LRDawson, Appl.Phys.Lett.51.1004-1006 (1987) and PLGourley, IJFritz, and LRDawson, Appl.Phys.Lett.52,377- 379 (1988).

  That is, the critical film thickness value obtained by the X-ray diffraction method is larger than the critical film thickness value obtained from other PL values, and it is pointed out that a correct value cannot be obtained, and the density of defects, etc. It has been reported that it is unsuitable for detection of initial structural degradation in the case of small. In addition, there are few further studies on the question “Why X-ray diffractometry does not provide detection sensitivity?”, And methods for improving detection sensitivity from the standpoint of X-ray diffractometry have been completely studied so far. It has never been done.

  In the above X-ray diffraction evaluation, the rocking curve measurement method was mainly used, but methods such as reciprocal lattice mapping were later developed. However, in these newly developed methods as well, Concerning the problem of “detection sensitivity of structural deterioration compared with other measurement methods”, no remarkable improvement effect and detailed examination were found.

  Under such circumstances, the present inventors have recently submitted an evaluation analysis method using a new X-ray diffraction method that improves this detection sensitivity problem (K. Nakashima and K. Tateno, J. Appl. Crystallogr. 37, 14-23 (2004) In this method, diffraction profiles measured under two different measurement conditions are displayed with reference peaks superimposed, and the difference in diffraction intensity is compared to determine the presence and extent of structural degradation with good detection sensitivity. Is an evaluation method for determining

  However, in order to be able to apply this method, it was necessary to be able to observe a reference peak serving as a reference in addition to the analysis target peak in the measurement profile. However, in bulk crystals or heteroepitaxially grown thin film crystals with a large degree of lattice mismatch, a peak that becomes a reference peak often appears in the vicinity of the peak to be analyzed. The above method could not be applied.

I.J.Fritz, P.L.Gourley, and L.R.Dawson, Appl.Phys.Lett. 51.1004-1006 (1987) P.L.Gourley, I.J.Fritz, and L.R.Dawson, Appl.Phys.Lett.52,377-379 (1988) K. Nakashima and K. Tateno, J. Appl.Crystallogr. 37, 14-23 (2004)

  Evaluation of structural degradation using the X-ray diffraction method, which is important in the fabrication of strained epitaxial layers and strained superlattice structures, such as evaluation of critical film thickness and evaluation of lattice relaxation processes in regions beyond the critical film thickness In order to solve the problem of poor detection sensitivity compared to the case of using other PL measurement methods, which has been a problem in the past, and to evaluate structural deterioration using the X-ray diffraction method, A new evaluation and analysis method that improves detection sensitivity compared with the method is provided.

  In particular, when a conventionally proposed method cannot be applied, that is, in a bulk crystal or a heteroepitaxially grown thin film crystal having a large degree of lattice mismatch, a peak that becomes a reference peak cannot be observed in the vicinity of the analysis target peak. A new evaluation analysis method that can be applied to such cases is provided.

  Note that the deterioration of the crystal structure may be dislocations, defects, crystal orientation distribution, disorder of crystal composition, and the like.

The structure of the crystal structure analysis method of the present invention that solves the above-described problem is that when the sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the sample is detected by an X-ray detector, A method for analyzing the crystal structure of
Using a target sample to be analyzed as a sample and irradiating the target sample with X-rays under a first measurement condition in which no aperture stop means is disposed between the target sample and the X-ray detector, Detecting the intensity of the diffracted X-ray diffracted by the target sample with the X-ray detector, and setting the detected intensity as the diffracted X-ray intensity of the target sample at a wide aperture angle;
An aperture stop means is disposed between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the target sample is irradiated with X-rays. The intensity of the diffracted X-ray diffracted by the target sample and passing through the aperture stop means is detected by the X-ray detector, and this detected intensity is set as the diffracted X-ray intensity of the target sample at a narrow aperture angle. Process,
Obtaining a relative ratio between the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle, and setting this relative ratio as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample is detected by the X-ray detector, and the detected intensity is set as the diffracted X-ray intensity of the reference sample at a wide aperture angle. Process,
The reference sample is irradiated with X-rays under the fourth measurement condition in which the reflection index is the reflection index selected in the third measurement condition but the other measurement conditions are the same with respect to the second measurement condition. Detecting the intensity of the diffracted X-rays diffracted at the aperture stop means by the X-ray detector and setting the detected intensity as the diffracted X-ray intensity of the reference sample at a narrow aperture angle; ,
Obtaining a relative ratio between the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle, and setting this relative ratio as the diffraction X-ray intensity ratio of the reference sample;
The relative ratio between the diffracted X-ray intensity ratio of the target sample and the diffracted X-ray intensity ratio of the reference sample is obtained, and this relative ratio is defined as a normalized diffracted X-ray intensity ratio. The crystal structure state of the target sample is determined.

The structure of the crystal structure analysis method of the present invention is as follows.
A method of analyzing the crystal structure of the sample by detecting the intensity of diffracted X-rays diffracted by the sample with an X-ray detector when the sample is irradiated with X-rays;
A target sample to be analyzed is used as a sample, and the target sample is gradually changed under the first measurement condition in which an aperture stop means is not disposed between the target sample and the X-ray detector. The X-ray detector detects the intensity of the diffracted X-ray diffracted by the target sample, and the peak intensity among the detected intensities of the target sample at a wide aperture angle is detected. A step of diffracted X-ray intensity;
An aperture stop means is arranged between the target sample and the X-ray detector, but other measurement conditions are the same as the first measurement conditions, and the target sample is gradually changed while changing the incident angle. The X-ray detector detects the intensity of the diffracted X-ray that has been diffracted by the target sample and diffracted by the target sample and passed through the aperture stop means, and the peak intensity is detected from the detected intensities. A step of setting the diffraction X-ray intensity of the target sample at a narrow aperture angle;
Dividing the X-ray intensity of the target sample at a narrow aperture angle by the X-ray intensity of the target sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays while gradually changing the angle, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and the peak intensity is detected from the detected intensities. The step of setting the diffracted X-ray intensity of the reference sample at a wide aperture angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but the other measurement conditions are the same. The X-ray detector detects the intensity of diffracted X-rays that are irradiated with a line, diffracted by the reference sample, and passed through the aperture stop means, and the peak intensity is narrowed from the detected intensity. A step of setting the diffraction X-ray intensity of the reference sample at the opening angle;
Dividing the X-ray intensity of the reference sample at a narrow aperture angle by the X-ray intensity of the reference sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the reference sample;
Divide the diffracted X-ray intensity ratio of the target sample by the diffracted X-ray intensity ratio of the reference sample, and use this divided value as the normalized diffracted X-ray intensity ratio. The crystal structure state of is determined.

The structure of the crystal structure analysis method of the present invention is as follows.
A method of analyzing the crystal structure of the sample by detecting the intensity of diffracted X-rays diffracted by the sample with an X-ray detector when the sample is irradiated with X-rays;
A target sample to be analyzed is used as a sample, and the target sample is gradually changed under the first measurement condition in which an aperture stop means is not disposed between the target sample and the X-ray detector. The X-ray detector detects the intensity of the diffracted X-ray diffracted by the target sample, and the integrated value obtained by integrating the detected intensity is used as the diffraction X of the target sample at a wide aperture angle. The step of making the line strength;
An aperture stop means is arranged between the target sample and the X-ray detector, but other measurement conditions are the same as the first measurement conditions, and the target sample is gradually changed while changing the incident angle. The X-ray detector detects the intensity of the diffracted X-ray that has been diffracted by the target sample and diffracted by the target sample and passed through the aperture stop means, and the integrated value obtained by integrating the detected intensity is narrowed. A step of setting the diffraction X-ray intensity of the target sample at the opening angle;
Dividing the X-ray intensity of the target sample at a narrow aperture angle by the X-ray intensity of the target sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays while gradually changing the angle, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and an integrated value obtained by integrating the detected intensity is widened. A step of setting the diffraction X-ray intensity of the reference sample at the opening angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but the other measurement conditions are the same. The X-ray detector detects the intensity of diffracted X-rays that are irradiated with a line, diffracted by the reference sample, and passed through the aperture stop means, and the integrated value obtained by integrating the detected intensity is a narrow aperture angle. The step of setting the diffraction X-ray intensity of the reference sample at
Dividing the X-ray intensity of the reference sample at a narrow aperture angle by the X-ray intensity of the reference sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the reference sample;
Divide the diffracted X-ray intensity ratio of the target sample by the diffracted X-ray intensity ratio of the reference sample, and use this divided value as the normalized diffracted X-ray intensity ratio. The crystal structure state of is determined.

The structure of the crystal structure analysis method of the present invention is as follows.
The reference sample is an Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal, which is a complete crystal substrate.

The structure of the crystal structure analysis apparatus of the present invention is as follows.
A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition in which the target sample to be analyzed is held in the sample holding unit, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector, The target sample is irradiated with X-rays from an X-ray source, the intensity of diffracted X-rays diffracted by the target sample is detected by the X-ray detector, and the calculation unit calculates the detected intensity at a wide aperture angle. Memorize | stored in the said memory | storage part as the diffraction X-ray intensity of an object sample,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the second measurement conditions are used. The target sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means is detected by the X-ray detector, and the calculation unit calculates the detected intensity. Memorize | stored in the said memory | storage part as the diffraction X-ray intensity of the object sample in a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and the X-ray intensity and wide aperture angle of the target sample at a narrow aperture angle. The relative ratio with the X-ray intensity of the target sample is stored in the storage unit as the diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays from the X-ray source under the conditions, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and the arithmetic unit widens the detected intensity. Storing in the storage unit as the diffracted X-ray intensity of the reference sample at the aperture angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but other measurement conditions are the same. In the fourth measurement condition, X-rays are emitted from the X-ray source to the reference sample. The X-ray detector detects the intensity of the diffracted X-ray that has been irradiated, diffracted by the reference sample, and passed through the aperture stop means, and the arithmetic unit detects the detected intensity at a reference angle at a narrow aperture angle. Is stored in the storage unit as the diffracted X-ray intensity of
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and the X-ray intensity and wide aperture angle of the reference sample at a narrow aperture angle. The relative ratio with the X-ray intensity of the reference sample is stored in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and the relative ratio between the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample The relative ratio is defined as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the normalized diffraction X-ray intensity ratio value.

The structure of the crystal structure analysis apparatus of the present invention is as follows.
A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition, a target sample to be analyzed is held in the sample holder, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector. The X-ray source irradiates the target sample with X-rays while gradually changing the angle, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample. Stored in the storage unit as the diffracted X-ray intensity of the target sample at a wide aperture angle,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the incident angle is gradually increased. The X-ray source irradiates the target sample with X-rays while changing the intensity, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means, The calculation unit stores the peak intensity from the detected intensity in the storage unit as the diffraction X-ray intensity of the target sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the target sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the target sample in the storage unit as a diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The X-ray source irradiates the reference sample with X-rays while gradually changing the incident angle under conditions, and the X-ray detector detects the intensity of the diffracted X-ray diffracted by the reference sample, and the calculation The unit stores the peak intensity from the detected intensity in the storage unit as the diffracted X-ray intensity of the reference sample at a wide aperture angle,
The X-ray source while gradually changing the incident angle under the fourth measurement condition in which the reflection index is set to the reflection index selected in the third measurement condition with respect to the second measurement condition but the other measurement conditions are the same. The reference sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample and passed through the aperture stop means is detected by the X-ray detector, and the calculation unit detects the detected intensity Storing the intensity of the peak from the above as the diffracted X-ray intensity of the reference sample at a narrow aperture angle in the storage unit,
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the reference sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the reference sample in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and divides the diffraction X-ray intensity ratio of the target sample by the diffraction X-ray intensity ratio of the reference sample. The division value is used as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the normalized diffraction X-ray intensity ratio value.

The structure of the crystal structure analysis apparatus of the present invention is as follows.
A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition, a target sample to be analyzed is held in the sample holder, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector. The X-ray source irradiates the target sample with X-rays while gradually changing the angle, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample. The integrated value obtained by integrating the intensity is stored in the storage unit as the diffraction X-ray intensity of the target sample at a wide aperture angle,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the incident angle is gradually increased. The X-ray source irradiates the target sample with X-rays while changing the intensity, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means, The calculation unit stores the integrated value obtained by integrating the detected intensity in the storage unit as the diffracted X-ray intensity of the target sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the target sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the target sample in the storage unit as a diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The X-ray source irradiates the reference sample with X-rays while gradually changing the incident angle under conditions, and the X-ray detector detects the intensity of the diffracted X-ray diffracted by the reference sample, and the calculation The unit stores an integrated value obtained by integrating the detected intensity as the diffracted X-ray intensity of the reference sample at a wide aperture angle in the storage unit,
The X-ray source while gradually changing the incident angle under the fourth measurement condition in which the reflection index is set to the reflection index selected in the third measurement condition with respect to the second measurement condition but the other measurement conditions are the same. The reference sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample and passed through the aperture stop means is detected by the X-ray detector, and the calculation unit detects the detected intensity Is stored in the storage unit as the diffracted X-ray intensity of the reference sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the reference sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the reference sample in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and divides the diffraction X-ray intensity ratio of the target sample by the diffraction X-ray intensity ratio of the reference sample. The division value is used as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the normalized diffraction X-ray intensity ratio value.

The structure of the crystal structure analysis apparatus of the present invention is as follows.
The reference sample is an Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal, which is a complete crystal substrate.

[Action]
In the present invention, by using the evaluation means, it is possible to configure an evaluation analysis method that can separate and independently perform evaluation analysis on the analysis target peak and analysis and correction using the reference peak. Even if it is not observed in the vicinity of the peak to be analyzed, the evaluation analysis technique works well, and it produces an effect of detecting and evaluating structural deterioration with high detection sensitivity in a more general case.
In particular, by using an analysis method that guarantees that the reflection index at the time of sample measurement for comparison reference can be freely selected independently of the reflection index for measurement of the sample to be analyzed, it is more general that the reflection index cannot be selected in common. In this case, it can be formulated into an applicable analysis method.

According to the present invention, X-ray diffractometry is used for structural deterioration such as evaluation of critical film thickness and evaluation of lattice relaxation process in a region exceeding the critical film thickness, which are important in the production of strained epitaxial layers and strained superlattice structures. To solve the problem of poor detection sensitivity compared to the case of using other PL measurement methods, etc., which has been a problem in the past, and evaluate structural deterioration using the X-ray diffraction method The detection sensitivity can be improved as compared with the conventional method. In particular, when a peak that becomes a reference peak that is frequently encountered in a bulk crystal or a heteroepitaxially grown thin film crystal with a large degree of lattice mismatch cannot be observed in the vicinity of the peak to be analyzed, that is, conventionally proposed. Even when the method cannot be analyzed, structural degradation can be evaluated and analyzed with high detection sensitivity. In addition, the effect of the present invention is that by performing the correction, it is possible to display a universal ratio with 1.0 when there is no structural deterioration.
Furthermore, by using an analysis method that guarantees that the reflection index at the time of measurement of the reference sample can be freely selected independently of the reflection index of the measurement of the sample to be analyzed, it is more general that the reflection index cannot be selected in common by both. Analysis can also be applied to cases. That is, according to the present invention, analysis can be performed using experimental data measured by freely selecting a reflection index in consideration of convenience in measurement.

In the best mode for carrying out the present invention, a single layer and a multilayer structure crystal made of an arbitrary bulk crystal or an arbitrary material system produced by epitaxial growth on an arbitrary substrate are subjected to structural evaluation by X-ray diffraction. Is assumed.
At this time, the crystal structure analysis method of the present invention is:
(1) A step of measuring a plurality of diffraction profiles having the same reflection index (hkl) while keeping the other measurement conditions the same under the condition where only the aperture angle condition of the light receiving system for diffracted X-rays is changed;
The diffraction intensity value at the peak top point is absolutely measured for each analysis target peak (or series of peaks) in each measurement profile obtained by the above process, and the light receiving system is measured for each analysis target peak based on this value. Calculating a relative ratio of diffraction intensity values between measurement profiles having different aperture angle conditions;
The ratio of the diffraction intensity values obtained by the above process is arranged from the viewpoint of the relative ratio of the diffraction intensity value in the narrow condition of the light receiving system aperture angle condition to the diffraction intensity value in the wide condition of the light receiving system aperture angle condition. It is characterized by determining the degree of crystal deterioration and structural deterioration of the analysis target layer (or analysis target multilayer structure crystal) corresponding to each analysis target peak (or a series of peaks) by evaluating the size of A structural analysis method of the crystal
And,
(2) In addition to the sample to be analyzed, a sample with a guaranteed crystal integrity is prepared as a comparative reference sample, and the light receiving system applied to the sample to be analyzed described in (1) above A plurality of measurements of the diffraction profile under the condition where only the opening angle condition is changed are also performed on the comparative reference sample. In this comparative reference sample measurement, all the measurement conditions related to incident X-rays, light receiving system measurement arrangement conditions, scan speed, and other measurement conditions such as (1) are kept for comparison while maintaining the conditions used for the measurement of the sample to be analyzed. A plurality of diffraction profiles are measured by the same procedure as in (1). However, in this measurement, the reflection index hkl used for the measurement of the reference sample for comparison is freely selected independently of the measurement conditions of (1). A step of calculating a relative ratio of diffraction intensity values between measurement profiles having different light receiving system aperture angle conditions in the same procedure as in (1) with respect to the comparative reference sample peak in the diffraction profile thus obtained; ,
By using the relative ratio of the diffraction intensity value to the obtained comparative reference sample peak, it was normalized by dividing the relative ratio of the diffraction intensity value to the analysis target peak obtained in the analysis method of (1) above. Calculating a relative ratio of diffraction intensity values;
By comparing the relative ratios of the normalized diffraction intensity values obtained in the previous step, the analysis target layer (or analysis target multilayer structure crystal) corresponding to each analysis target peak (or series of peaks) is analyzed. A crystal structure analysis method characterized by determining crystallographic integrity and the degree of structural deterioration.

In the best mode for carrying out the present invention,
(3) In the analysis method of (2) above, a crystal structure analysis characterized by using a complete crystal substrate such as a Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal as a comparative reference sample. Is the law.

  Next, each example of the present invention will be described.

  As a specific example 1 of the present invention, an example in which a structure evaluation of a GaN epitaxial thin film sample produced on a (0001) sapphire substrate by MOVPE growth method is applied to the present invention will be described below. Note that sapphire and GaN have a lattice mismatch degree of about 19%, which is a typical example of a material system having a large lattice mismatch degree. Therefore, in the X-ray diffraction measurement, the sapphire substrate peak is not observed in the vicinity of the GaN epitaxial layer peak, and is therefore a typical example in which no diffraction peak that can be a reference peak is observed in the vicinity of the GaN epitaxial layer peak. .

  As GaN epitaxial thin film samples, two target samples (sample A and sample B) having different growth conditions were prepared, and the degree of structural deterioration was evaluated for each sample.

As an example of the present invention, FIG. 1 shows a 0006 reflection X-ray diffraction measurement profile of a GaN sample A. In the figure, two profiles measured under two types of light receiving system aperture angle conditions (first measurement condition and second measurement condition) are displayed. In each profile, only a peak due to the GaN layer is observed. . The light receiving system aperture angle condition used is one wide light receiving system aperture angle condition (first measurement condition) in which no light receiving slit is placed in front of the X-ray detector, and the other one is in front of the X-ray detector. This is an extremely narrow light receiving system aperture angle condition (second measurement condition) in which a light receiving analyzer crystal is inserted.
The first measurement condition and the second measurement condition in the X-ray diffraction measurement are different in the light receiving system aperture angle condition, but the other measurement conditions are the same.

In the display of FIG. 1, the vertical axis indicates the diffraction intensity in units of counts / second, and the horizontal axis indicates the incident angle of the X-ray irradiated to the sample.
“Diffraction intensity” refers to the intensity detected by the X-ray detector when the X-ray generated from the X-ray source is irradiated onto the sample and the intensity of the diffracted X-ray emitted after being diffracted by the crystal lattice of the sample is detected ( Diffraction X-ray intensity). The vertical axis in FIG. 1 indicates this diffraction intensity (diffracted X-ray intensity).

In addition, as is well known in the X-ray diffraction method, the X-ray source is stationary and the sample is gradually rotated to change the incident angle of the X-rays applied to the sample. Is detected. In this case, for example, in the biaxial diffractometer, a goniometer is used to rotate the X-ray detector by 2θ ° in synchronization with the rotation of the sample by θ °. The horizontal axis of FIG. 1 shows the change state of the incident angle of X-rays irradiated on the sample.
Note that detecting the diffracted X-ray intensity (diffraction intensity) while rotating the sample to change the incident angle of the X-ray is referred to as “scan”.
Furthermore, a characteristic curve that follows the diffraction intensity at each incident angle is referred to as a “profile”.
Further, the diffracted X-rays emitted from the sample travel toward the X-ray detector with a predetermined radiation angle (solid angle). Therefore, when an aperture stop means (slit or analyzer crystal) is arranged in the path (light receiving system) between the sample and the X-ray detector, only the diffracted X-rays within the aperture angle range of the aperture stop means are X-rays. It will be incident on the detector.

  In the measurement of both profiles shown in FIG. 1, all the measurement conditions other than the light receiving system aperture angle conditions such as the X-ray source conditions, scan speed, reflection index, etc. are kept the same. It is important that the relative intensity difference between the profiles can be regarded as an absolute display of the diffraction intensity difference caused by the difference in the light receiving system aperture angle condition.

  When attention is paid to this point, it can be seen from FIG. 1 that the absolute diffraction intensity of the peak of the GaN layer when measured under extremely narrow light receiving system aperture angle conditions is significantly higher than the absolute diffraction intensity when measured under wide light receiving system aperture angle conditions. It turns out that it has decreased. By evaluating and analyzing the magnitude of this reduction, it is possible to evaluate the crystal perfection and the degree of structural deterioration of the GaN layer that is the analysis target layer. Specifically, the diffraction intensity ratio of the GaN peak in the two profiles (specifically when the incident angle is around 63 °) (= the diffraction intensity when the light receiving system aperture angle is extremely narrow / the wide light receiving system aperture) When the diffraction intensity (when using the angle) is obtained from the figure, a small value of about 0.01 is obtained, and it can be concluded that the degree of structural deterioration is large.

More specifically, first, X-ray diffraction measurement is performed on the target sample A under a wide light receiving system aperture angle condition (first measurement condition), and a GaN peak in the profile (diffracted X-ray intensity of the target sample at a wide aperture angle). Ask for.
Next, subject sample A is subjected to X-ray diffraction measurement under an extremely narrow light receiving system aperture angle condition (second measurement condition), and a GaN peak in the profile (diffracted X-ray intensity of the subject sample at a narrow aperture angle) is obtained. Ask.
Then, “a GaN peak (diffracted X-ray intensity of the target sample at a narrow aperture angle) in a profile obtained by X-ray diffraction measurement of the target sample A under an extremely narrow light receiving system aperture angle condition (second measurement condition)” is “ By dividing by the GaN peak (diffracted X-ray intensity of the target sample at a wide aperture angle) in the profile obtained by X-ray diffraction measurement of the target sample A under a wide light receiving system aperture angle condition (first measurement condition), As the “diffracted X-ray intensity ratio of the target sample A”, the above-described value of about 0.01 is obtained.

  The result of the same measurement performed on sample B is shown in FIG. All the measurement conditions used were the same as those used in the measurement of FIG. 1, so that the degree of structural deterioration between samples could be easily compared. From FIG. 2, the diffraction intensity ratio with respect to the sample B when the incident angle is around 64.2 °, that is, the diffraction X-ray intensity ratio of the target sample B (= diffraction intensity with an extremely narrow light receiving system aperture angle / wide light reception). The diffraction intensity when the system opening angle is taken is about 0.06.

More specifically, first, X-ray diffraction measurement is performed on the target sample B under a wide light receiving system aperture angle condition (the first measurement condition described above), and a GaN peak in the profile (diffracted X-ray of the target sample at a wide aperture angle). Strength).
Next, the target sample B is subjected to X-ray measurement under an extremely narrow light receiving system aperture angle condition (the second measurement condition described above), and a GaN peak in the profile (diffracted X-ray intensity of the target sample at a narrow aperture angle) Ask for.
Then, “a GaN peak (diffracted X-ray intensity of the target sample at a narrow aperture angle) in a profile obtained by X-ray diffraction measurement of the target sample B under an extremely narrow light receiving system aperture angle condition (second measurement condition)” is “ By dividing by the GaN peak (diffracted X-ray intensity of the target sample at a wide aperture angle) in a profile obtained by X-ray diffraction measurement of the target sample B under a wide light receiving system aperture angle condition (first measurement condition), As the “diffracted X-ray intensity ratio of the target sample B”, the above-described value of about 0.06 is obtained.

  Here, a wide light receiving system aperture angle condition and a narrow light receiving system aperture angle condition will be described with reference to FIGS. 3A to 3E showing an X-ray diffraction apparatus.

  In FIG. 3A, 10 is an X-ray source, 11 is a sample holder, 12 is an X-ray detector, and 13 is a slit. The sample holder 11 is provided with a sample 20.

  X-rays generated from the X-ray source 10 are applied to the sample 20 held by the sample holding unit 11. Then, diffracted X-rays are generated by diffraction of the crystal lattice of the sample 20, and the diffracted X-rays are emitted. The emitted diffracted X-ray enters the X-ray detector 12 and the intensity of the diffracted X-ray is detected. At this time, by the scanning operation, the detector is rotated 2θ ° synchronously when the sample 20 (sample holding unit 11) is rotated θ °.

  Then, the slit 13 can be arranged in the path between the sample 20 and the X-ray detection unit 11, that is, the light receiving system in which the diffracted X-rays travel, or the slit 13 can be omitted. The “wide light receiving system opening angle condition” corresponds to the case where there is no slit 13, and the “narrow light receiving system opening angle condition” corresponds to the case where there is the slit 13.

  As shown in FIG. 3B, when the sample 20 having high crystallinity is irradiated with X-rays, the X-ray diffracted on the crystal surface is hardly scattered and has a narrow radiation angle. Therefore, as shown in FIG. 3C, when the slit 13 is inserted between the crystal and the X-ray detector 20, most of the diffracted X-rays pass through the slit 13 and reach the X-ray detector 12. Therefore, the diffraction intensity measured is high. Therefore, since the diffraction intensity detected when the slit 13 is inserted does not decrease compared to that when the slit 13 is not inserted, the value of the ratio of the respective diffraction intensities becomes high.

  On the other hand, as shown in FIG. 3D, when the sample 20 having low crystallinity is irradiated with X-rays, the X-ray diffracted on the crystal surface is often scattered and has a wide radiation angle. Therefore, when the slit 13 is inserted between the crystal and the X-ray detector 12, most of the diffracted X-rays do not pass through the slit 13 and cannot reach the X-ray detector 12, so that the measured diffraction intensity is low. Therefore, since the diffraction intensity detected when the slit 13 is inserted is lower than that when the slit 13 is not inserted, the value of the ratio of the respective diffraction intensities is low.

  In actual measurement, a narrow light receiving system aperture angle condition can be realized by using an analyzer crystal 14 as shown in FIG. In general, the analyzer crystal 14 uses a (220) asymmetric surface of Si crystal or Ge crystal. FIG. 4A shows a state where the condition of the light receiving system aperture angle is widened so that the analyzer crystal 14 is not interposed in the light receiving system.

  Next, FIG. 5 shows the results of measurement and evaluation using a GaAs substrate crystal as a comparative reference sample and using the same measurement conditions as those used in FIGS. At this time, the reflection index was also selected as 004 independently of FIGS. The GaAs substrate crystal employed as a comparative reference sample is a sample in which the integrity of the crystal is guaranteed.

The reflection index is an index representing the reflection of X-rays by the lattice plane that satisfies the Bragg condition of the crystal.
The reflection index used under the measurement conditions used to obtain the measurement evaluation results shown in FIGS. 1 and 2 and the reflection index used under the measurement conditions used to obtain the measurement evaluation results shown in FIG. It is different. Other measurement conditions are the same.

  In other words, the “measurement condition” here refers to the intensity and wavelength of X-rays incident on the sample, the sensitivity of the X-ray detector, the aperture angle of the aperture stop means, the reflection index of each sample, the scan speed, and the like.

FIG. 5 shows that the diffraction intensity ratio in two measurements (measurement under a wide light receiving system aperture angle condition and extremely narrow light receiving system aperture angle condition) is about 0.25. It can be experimentally confirmed that this value does not depend on the index even if the reflection index is selected as 002 or 006 and is evaluated, and a substantially constant value is obtained. From this experimental fact, when a perfect crystal is selected as a comparative reference sample, it can be experimentally guaranteed that the diffraction intensity ratio does not depend on the reflection index, and a constant value determined by other measurement conditions can be obtained. Therefore, in the measurement of FIG. 5, it is justified to select and analyze the reflection index independently of FIGS.
From the experimental results using 004 reflection in FIG. 5 based on the above results, under the measurement conditions employed in this example, the diffraction intensity ratio under two different light receiving system aperture angle measurement conditions is It was confirmed that the measurement conditions were about 0.25 (independent of the reflection index used for measurement).

More specifically, the reference sample is first placed under a wide light receiving system aperture angle condition (the third measurement condition in which the reflection index is selected independently of the first measurement condition but the other measurement conditions are the same). A line diffraction measurement is performed to obtain a GaAs peak (diffracted X-ray intensity of the reference sample at a wide aperture angle) in the profile.
Next, a reference sample under extremely narrow light receiving system aperture angle conditions (the fourth measurement condition in which the reflection index is the reflection index selected in the third measurement condition for the second measurement condition but the other measurement conditions are the same). X-ray diffraction measurement is performed to obtain a GaAs peak in the profile (diffracted X-ray intensity of the reference sample at a narrow aperture angle).
Then, "GaAs peak in the profile of the reference sample measured under extremely narrow light receiving system aperture angle condition (third measurement condition) (diffracted X-ray intensity of the reference sample at narrow aperture angle)" By dividing by the GaAs peak (diffracted X-ray intensity of the reference sample at a wide aperture angle) in the profile obtained by measuring the reference sample under the angular condition (fourth measurement condition), the “diffracted X-ray intensity ratio of the reference sample” ", The above-mentioned value of about 0.25 is obtained.

  The comparative reference sample is a complete crystal, that is, a sample in which the crystal integrity is guaranteed, and the term “crystal integrity is guaranteed” as used herein means a semiconductor crystal whose crystal quality is generally commercially available. It shows that it is about the crystal quality of the substrate.

  Therefore, using the “diffracted X-ray intensity ratio of the reference sample (= 0.25)”, the diffraction intensity ratio of the GaN peak of the sample A as the analysis target layer (“diffracted X-ray intensity ratio of the target sample A” = When the corrected diffraction intensity ratio (normalized diffraction X-ray intensity ratio) is obtained by dividing (0.01), a value of 0.01 / 0.25 = 0.04 is obtained. If the normalized diffraction X-ray intensity ratio value is 1.0, it means that the analysis target layer is a complete crystal, and as the normalized diffraction X-ray intensity ratio value becomes smaller than 1.0, It shows that the degree of structural deterioration increases. In this sense, it is understood that the “corrected diffraction intensity ratio (standardized diffraction X-ray intensity ratio)” is an amount that displays the degree of structural degradation more universally, compared to the analysis of FIG. 1 alone. You can see that it has advantages. From the obtained value of 0.04 (value of normalized diffraction X-ray intensity ratio), it became clear that the GaN peak of the target sample A, which is the analysis target layer, significantly includes the influence of structural deterioration.

  When the corrected diffraction intensity ratio (standardized diffraction X-ray intensity ratio) is similarly obtained for sample B, a value of 0.06 / 0.25 = 0.24 is obtained. Since this value is smaller than 1.0, it can be easily concluded that there is structural deterioration in Sample B. In addition, it can be concluded from the comparison with the value of sample A that the degree of structural deterioration of sample B is not as great as that of sample A, and it is simple and universally analyzed that sample B has better crystallinity than sample A. did it.

  As described above, in the present invention, since the standardized diffraction X-ray intensity ratio is obtained, it can be seen that the presence or absence and the degree of structural deterioration can be detected and evaluated with higher detection sensitivity than in the conventional case. It was.

  In addition, as a reference sample in which the integrity of the crystal is guaranteed, a complete crystal substrate such as a Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal can be used.

Next, the crystal structure analysis apparatus according to Example 2 of the present invention is shown in schematic configuration diagrams in FIGS. 6A and 6B and flow diagrams in FIGS. This will be described with reference to c).
The crystal structure analysis apparatus 100 according to the second embodiment is one apparatus that performs the “crystal structure analysis method” according to the first embodiment. 6A shows a state in which X-ray diffraction measurement is performed under wide light receiving system aperture angle conditions (first measurement condition and third measurement condition), and FIG. 6B shows an extremely narrow light receiving system aperture. A state in which X-ray diffraction measurement is performed under angular conditions (second measurement condition and fourth measurement condition) is shown.

  As shown in FIGS. 6A and 6B, the crystal structure analysis apparatus 100 includes an X-ray diffraction apparatus 30, a calculation unit 40, and a storage unit 50. Data can be transmitted and received between the calculation unit 40 and the storage unit 50.

  The X-ray diffraction apparatus 30 includes an X-ray source 31, a sample holder 32, X-ray detectors 33 and 34, and an analyzer crystal 35. The detection sensitivities of the X-ray detector 33 and the X-ray detector 34 are the same. The sample holder 21 holds the target sample 21 or the reference sample 22.

In the X-ray diffraction measurement, the X-ray generated from the X-ray source 31 is irradiated to the sample 21 (or 22) held by the sample holding unit 32. Then, diffraction X-rays are generated by diffraction of the crystal of the sample 21 (22), and the diffraction X-rays are emitted.
Under the first measurement condition and the third measurement condition (wide aperture angle condition) shown in FIG. 6A, the diffracted X-ray enters the X-ray detector 33 and the intensity of the diffracted X-ray is detected. The detected diffracted X-ray intensity is sent from the X-ray detector 33 to the calculation unit 40.
6B, the diffracted X-rays are diffracted and reflected by the analyzer crystal 35 before entering the X-ray detector 34 under the second and fourth measurement conditions (extremely narrow aperture angle conditions). The intensity of the diffracted X-ray is detected. The detected diffracted X-ray intensity is sent from the X-ray detector 34 to the calculation unit 40.
The scanning operation is performed regardless of the first, third measurement conditions, or the second, fourth measurement conditions, and the sample holder 32 holding the sample 21 (22) is gradually rotated. Accordingly, the detectors 33 and 34 and the analyzer crystal 35 are gradually rotated at an angle twice the rotation angle of the sample holder 32.

  The first and third measurement conditions (wide aperture angle conditions) and the second and fourth measurement conditions (extremely narrow aperture angle conditions) differ in the arrangement state of the detectors 33 and 34 and the analyzer crystal 35. The change of the arrangement state can be performed by manual control or automatic control.

Further, after the target sample 21 to be analyzed is held on the surface side of the sample holding unit 32 and X-ray diffraction measurement is performed, the reference sample 22 is held on the surface side of the sample holding unit 32 and X-ray diffraction is performed. Measure.
As a modification of this sample exchange, the target sample 21 is held on the front surface side of the sample holding unit 32, the target sample 22 is held on the back side of the sample holding unit 32, and X-ray diffraction measurement is performed on the target sample 21. When the target sample 21 is directed to the X-ray source 31 side and X-ray diffraction measurement is performed on the reference sample 22 thereafter, the sample holder 32 is rotated by 180 degrees, and the reference sample 22 is moved to the X-ray source. It can also be configured to be directed to the radiation source 31 side.

  Next, the X-ray diffraction measurement operation will be described with reference to FIGS. 6 (a), 6 (b) and 7 (a) to 7 (c).

  As shown in FIG. 6A, the target sample 21 to be analyzed is set in the sample holder 32 in an arrangement state that satisfies a wide light receiving system aperture angle condition (step 1).

  In a state where the analyzer crystal 35 is not set in the light receiving system and a wide light receiving system aperture angle condition is set, the intensity of diffracted X-rays radiated from the target sample 21 is scanned while irradiating the target sample 21 with X-rays ( (Diffraction X-ray intensity) is measured by the X-ray detector 33. The measurement condition at this time is defined as “first measurement condition” (step 2).

  The computing unit 40 obtains the diffracted X-ray intensity at the peak from the measurement profile indicating the diffracted X-ray intensity obtained under the “first measurement condition”. The obtained diffracted X-ray intensity is defined as “diffracted X-ray intensity of the target sample at a wide aperture angle” (step 3).

  The “diffracted X-ray intensity of the target sample at a wide aperture angle” is stored in the storage unit 50 (step 4).

  As shown in FIG. 6B, in a state where the analyzer crystal 35 is set in the light receiving system and the light receiving system has a narrow opening angle condition, scanning is performed while irradiating the target sample 21 with X-rays. The intensity of the diffracted X-ray that has been radiated and transmitted through a narrow aperture angle (diffracted X-ray intensity) is measured by the X-ray detector 34. The measurement condition at this time is the “second measurement condition” in which the other measurement conditions are maintained while only the light receiving system aperture angle is different from the “first measurement condition” (step 5).

  The computing unit 40 obtains the diffracted X-ray intensity at the peak portion from the measurement profile indicating the diffracted X-ray intensity obtained under the “second measurement condition”. The obtained diffracted X-ray intensity is defined as “diffracted X-ray intensity of the target sample at a narrow aperture angle” (step 6).

  The “diffracted X-ray intensity of the target sample at a narrow aperture angle” is stored in the storage unit 50 (step 7).

  The “diffracted X-ray intensity of the target sample at a wide aperture angle” and “diffracted X-ray intensity of the target sample at a narrow aperture angle” stored in the storage unit 50 are read into the arithmetic unit 40 (step 8).

  The calculation unit 40 divides “diffracted X-ray intensity of the target sample at a narrow aperture angle” by “diffracted X-ray intensity of the target sample at a wide aperture angle” to obtain “diffracted X-ray intensity ratio of the target sample”. Calculate (step 9).

  The “diffracted X-ray intensity ratio of the target sample” is stored in the storage unit 50 (step 10).

  Next, as shown in FIG. 6A, the reference sample 22 in which the integrity of the crystal is guaranteed is set in the sample holder 32 in an arrangement state in which a wide light receiving system aperture angle condition is satisfied (step 11). .

  In a state where the analyzer crystal 35 is not set in the light receiving system and the light receiving system has a wide opening angle condition, the reference sample 22 is scanned while being irradiated with X-rays, and the intensity of diffracted X-rays emitted from the reference sample 22 ( (Diffraction X-ray intensity) is measured by the X-ray detector 33. The measurement conditions (“third measurement condition”) at this time are the reflection index selected independently of the above-mentioned “first measurement condition”, but the other measurement conditions are the same (step 12). .

  The computing unit 40 obtains the diffracted X-ray intensity at the peak from the measurement profile indicating the diffracted X-ray intensity obtained under the “third measurement condition”. The obtained diffracted X-ray intensity is defined as “diffracted X-ray intensity of the reference sample at a wide aperture angle” (step 13).

  The “diffracted X-ray intensity of the reference sample at a wide aperture angle” is stored in the storage unit 50 (step 14).

  As shown in FIG. 6B, in a state where the analyzer crystal 35 is set in the light receiving system and the light receiving system has a narrow opening angle condition, scanning is performed while irradiating the reference sample 22 with X-rays. The intensity of the diffracted X-ray that has been radiated and transmitted through a narrow aperture angle (diffracted X-ray intensity) is measured by the X-ray detector 34. The measurement condition (“fourth measurement condition”) at this time is the reflection index selected in “third measurement condition” with respect to the “second measurement condition” described above, but the other measurement conditions are the same. Yes (step 15).

  The computing unit 40 obtains the diffraction X-ray intensity at the peak portion from the measurement profile indicating the diffraction X-ray intensity obtained under the “fourth measurement condition”. The obtained diffracted X-ray intensity is defined as “diffracted X-ray intensity of the reference sample at a narrow aperture angle” (step 16).

  The above-mentioned “diffracted X-ray intensity of the reference sample at a narrow aperture angle” is stored in the storage unit 50 (step 17).

  The “diffracted X-ray intensity of the reference sample at a wide aperture angle” and “diffracted X-ray intensity of the reference sample at a narrow aperture angle” stored in the storage unit 50 are read into the arithmetic unit 40 (step 18).

  The calculation unit 40 divides the “diffracted X-ray intensity of the reference sample at a narrow aperture angle” by the “diffracted X-ray intensity of the reference sample at a wide aperture angle” to obtain the “diffracted X-ray intensity ratio of the reference sample”. Calculate (step 19).

  The “diffracted X-ray intensity ratio of the reference sample” is stored in the storage unit 50 (step 20).

  The “diffracted X-ray intensity ratio of the target sample” and the “diffracted X-ray intensity ratio of the reference sample” stored in the storage unit 50 are read into the computing unit 40 (step 21).

  The computing unit 40 divides the “diffracted X-ray intensity ratio of the target sample” by the “diffracted X-ray intensity ratio of the reference sample” to calculate a “standardized diffraction X-ray intensity ratio” (step 22).

  From the magnitude of the “normalized diffraction X-ray intensity ratio”, the crystallographic integrity of the target sample 22 and the degree of structural deterioration are determined (step 23).

  In each of the above embodiments, the analysis is performed on the peak value of the profile, but the same effect can be obtained even on the target reflecting the diffracted X-ray intensity, such as the integral value of the profile. .

Therefore, in Example 3, the crystal structure analysis apparatus 100 shown in FIGS. 6A and 6B is used, and the integral value of the profile is used to reflect the intensity of the diffracted X-rays. An example of structural analysis will be described.
Since the configuration is the same as that shown in FIGS. 6 (a) and 6 (b), refer to FIGS. 6 (a), 6 (b) and FIGS. 8 (a) to 8 (c). The X-ray diffraction measurement operation in Example 3 will be described.

  As shown in FIG. 6A, the target sample 21 to be analyzed is set in the sample holder 32 in an arrangement state that satisfies a wide light receiving system aperture angle condition (step 101).

  In a state where the analyzer crystal 35 is not set in the light receiving system and a wide light receiving system aperture angle condition is set, the intensity of diffracted X-rays radiated from the target sample 21 is scanned while irradiating the target sample 21 with X-rays ( (Diffraction X-ray intensity) is measured by the X-ray detector 33. The measurement condition at this time is defined as “first measurement condition” (step 102).

  The computing unit 40 integrates the measurement profile indicating the diffracted X-ray intensity obtained under the “first measurement condition” to obtain an integral value. This integrated value is defined as “diffracted X-ray intensity of the target sample at a wide aperture angle” (step 103).

  The above-mentioned “diffracted X-ray intensity of the target sample at a wide aperture angle” is stored in the storage unit 50 (step 104).

  As shown in FIG. 6B, in a state where the analyzer crystal 35 is set in the light receiving system and the light receiving system has a narrow opening angle condition, scanning is performed while irradiating the target sample 21 with X-rays. The intensity of the diffracted X-ray that has been radiated and transmitted through a narrow aperture angle (diffracted X-ray intensity) is measured by the X-ray detector 34. The measurement condition at this time is a “second measurement condition” that is different from the “first measurement condition” in that the aperture angle of the light receiving system is different and other measurement conditions are maintained (step 105).

  The computing unit 40 integrates the measurement profile indicating the diffracted X-ray intensity obtained under the “second measurement condition” to obtain an integral value. This integrated value is defined as “diffracted X-ray intensity of the target sample at a narrow aperture angle” (step 106).

  The “diffracted X-ray intensity of the target sample at a narrow aperture angle” is stored in the storage unit 50 (step 107).

  The “diffracted X-ray intensity of the target sample at a wide aperture angle” and “diffracted X-ray intensity of the target sample at a narrow aperture angle” stored in the storage unit 50 are read into the arithmetic unit 40 (step 108).

  The calculation unit 40 divides “diffracted X-ray intensity of the target sample at a narrow aperture angle” by “diffracted X-ray intensity of the target sample at a wide aperture angle” to obtain “diffracted X-ray intensity ratio of the target sample”. Calculate (step 109).

  The above-mentioned “diffracted X-ray intensity ratio of the target sample” is stored in the storage unit 50 (step 110).

  Next, as shown in FIG. 6A, the reference sample 22 in which the crystal integrity is ensured is set in the sample holder 32 in an arrangement state that satisfies a wide light receiving system aperture angle condition (step 111). .

  In a state where the analyzer crystal 35 is not set in the light receiving system and the light receiving system has a wide opening angle condition, the reference sample 22 is scanned while being irradiated with X-rays, and the intensity of diffracted X-rays emitted from the reference sample 22 ( (Diffraction X-ray intensity) is measured by the X-ray detector 33. The measurement conditions (“third measurement condition”) at this time are the reflection index selected independently of the above-mentioned “first measurement condition”, but the other measurement conditions are the same (step 112). .

  The computing unit 40 obtains an integrated value by integrating the measurement profile indicating the diffracted X-ray intensity obtained under the “third measurement condition”. This integrated value is defined as “diffracted X-ray intensity of the reference sample at a wide aperture angle” (step 113).

  The above-mentioned “diffracted X-ray intensity of the reference sample at a wide aperture angle” is stored in the storage unit 50 (step 114).

  As shown in FIG. 6B, in a state where the analyzer crystal 35 is set in the light receiving system and the light receiving system has a narrow opening angle condition, scanning is performed while irradiating the reference sample 22 with X-rays. The intensity of the diffracted X-ray that has been radiated and transmitted through a narrow aperture angle (diffracted X-ray intensity) is measured by the X-ray detector 34. The measurement condition (“fourth measurement condition”) at this time is the reflection index selected in “third measurement condition” with respect to the “second measurement condition” described above, but the other measurement conditions are the same. Yes (step 115).

  The computing unit 40 obtains an integrated value by integrating the measurement profile indicating the diffracted X-ray intensity obtained under the “fourth measurement condition”. This integrated value is defined as “diffracted X-ray intensity of the reference sample at a narrow aperture angle” (step 116).

  The above-mentioned “diffracted X-ray intensity of the reference sample at a narrow aperture angle” is stored in the storage unit 50 (step 117).

  The “diffracted X-ray intensity of the reference sample at a wide aperture angle” and the “diffracted X-ray intensity of the reference sample at a narrow aperture angle” stored in the storage unit 50 are read into the computing unit 40 (step 118).

  The calculation unit 40 divides the “diffracted X-ray intensity of the reference sample at a narrow aperture angle” by the “diffracted X-ray intensity of the reference sample at a wide aperture angle” to obtain the “diffracted X-ray intensity ratio of the reference sample”. Calculate (step 119).

  The “diffracted X-ray intensity ratio of the reference sample” is stored in the storage unit 50 (step 120).

  The “diffracted X-ray intensity ratio of the target sample” and the “diffracted X-ray intensity ratio of the reference sample” stored in the storage unit 50 are read into the computing unit 40 (step 121).

  The computing unit 40 calculates the “standardized diffraction X-ray intensity ratio” by dividing the “diffracted X-ray intensity ratio of the target sample” by the “diffracted X-ray intensity ratio of the reference sample” (step 122).

  From the magnitude of the “normalized diffraction X-ray intensity ratio”, the crystallographic integrity of the target sample 22 and the degree of structural deterioration are determined (step 123).

The characteristic view which shows the 0006 reflection X-ray-diffraction measurement profile of the GaN sample (sample A) measured on two types of light receiving system aperture angle conditions. The characteristic view which shows the 0006 reflection X-ray-diffraction measurement profile of the GaN sample (sample B) measured on two types of light receiving system aperture angle conditions. 1 is a schematic configuration diagram showing an X-ray analysis apparatus. 1 is a schematic configuration diagram showing an X-ray analysis apparatus. The characteristic view which shows the 006 reflection X-ray-diffraction measurement profile measured on two types of light receiving system aperture angle conditions with respect to the sample GaAs substrate crystal peak for a comparative reference. FIG. 3 is a configuration diagram showing a crystal structure analysis apparatus according to a second embodiment. FIG. 3 is a configuration diagram showing a crystal structure analysis apparatus according to a second embodiment. FIG. 6 is a flowchart showing an operation state of the second embodiment. FIG. 6 is a flowchart showing an operation state of the second embodiment. FIG. 6 is a flowchart showing an operation state of the second embodiment. FIG. 9 is a flowchart showing an operation state of the third embodiment. FIG. 9 is a flowchart showing an operation state of the third embodiment. FIG. 9 is a flowchart showing an operation state of the third embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 X-ray source 11 Sample holding part 12 X-ray detector 13 Slit 14 Analyzer crystal 20 Sample 100 Crystal structure analysis apparatus 30 X-ray diffractometer 31 X-ray source 32 Sample holding part 33, 34 X-ray detector 35 Analyzer crystal

Claims (8)

A method of analyzing the crystal structure of the sample by detecting the intensity of diffracted X-rays diffracted by the sample with an X-ray detector when the sample is irradiated with X-rays;
Using a target sample to be analyzed as a sample and irradiating the target sample with X-rays under a first measurement condition in which no aperture stop means is disposed between the target sample and the X-ray detector, Detecting the intensity of the diffracted X-ray diffracted by the target sample with the X-ray detector, and setting the detected intensity as the diffracted X-ray intensity of the target sample at a wide aperture angle;
An aperture stop means is disposed between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the target sample is irradiated with X-rays. The intensity of the diffracted X-ray diffracted by the target sample and passing through the aperture stop means is detected by the X-ray detector, and this detected intensity is set as the diffracted X-ray intensity of the target sample at a narrow aperture angle. Process,
Obtaining a relative ratio between the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle, and setting this relative ratio as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample is detected by the X-ray detector, and the detected intensity is set as the diffracted X-ray intensity of the reference sample at a wide aperture angle. Process,
The reference sample is irradiated with X-rays under the fourth measurement condition in which the reflection index is the reflection index selected in the third measurement condition but the other measurement conditions are the same with respect to the second measurement condition. Detecting the intensity of the diffracted X-rays diffracted at the aperture stop means by the X-ray detector and setting the detected intensity as the diffracted X-ray intensity of the reference sample at a narrow aperture angle; ,
Obtaining a relative ratio between the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle, and setting this relative ratio as the diffraction X-ray intensity ratio of the reference sample;
The relative ratio between the diffracted X-ray intensity ratio of the target sample and the diffracted X-ray intensity ratio of the reference sample is obtained, and this relative ratio is defined as a normalized diffracted X-ray intensity ratio. A crystal structure analysis method characterized by determining a crystal structure state of a target sample. A method of analyzing the crystal structure of the sample by detecting the intensity of diffracted X-rays diffracted by the sample with an X-ray detector when the sample is irradiated with X-rays;
A target sample to be analyzed is used as a sample, and the target sample is gradually changed under the first measurement condition in which an aperture stop means is not disposed between the target sample and the X-ray detector. The X-ray detector detects the intensity of the diffracted X-ray diffracted by the target sample, and the peak intensity among the detected intensities of the target sample at a wide aperture angle is detected. A step of diffracted X-ray intensity;
An aperture stop means is arranged between the target sample and the X-ray detector, but other measurement conditions are the same as the first measurement conditions, and the target sample is gradually changed while changing the incident angle. The X-ray detector detects the intensity of the diffracted X-ray that has been diffracted by the target sample and diffracted by the target sample and passed through the aperture stop means, and the peak intensity is detected from the detected intensities. A step of setting the diffraction X-ray intensity of the target sample at a narrow aperture angle;
Dividing the X-ray intensity of the target sample at a narrow aperture angle by the X-ray intensity of the target sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays while gradually changing the angle, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and the peak intensity is detected from the detected intensities. The step of setting the diffracted X-ray intensity of the reference sample at a wide aperture angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but the other measurement conditions are the same. The X-ray detector detects the intensity of diffracted X-rays that are irradiated with a line, diffracted by the reference sample, and passed through the aperture stop means, and the peak intensity is narrowed from the detected intensity. A step of setting the diffraction X-ray intensity of the reference sample at the opening angle;
Dividing the X-ray intensity of the reference sample at a narrow aperture angle by the X-ray intensity of the reference sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the reference sample;
Divide the diffracted X-ray intensity ratio of the target sample by the diffracted X-ray intensity ratio of the reference sample, and use this divided value as the normalized diffracted X-ray intensity ratio. A crystal structure analysis method comprising: determining a crystal structure state of a crystal. A method of analyzing the crystal structure of the sample by detecting the intensity of diffracted X-rays diffracted by the sample with an X-ray detector when the sample is irradiated with X-rays;
A target sample to be analyzed is used as a sample, and the target sample is gradually changed under the first measurement condition in which an aperture stop means is not disposed between the target sample and the X-ray detector. The X-ray detector detects the intensity of the diffracted X-ray diffracted by the target sample, and the integrated value obtained by integrating the detected intensity is used as the diffraction X of the target sample at a wide aperture angle. The step of making the line strength;
An aperture stop means is arranged between the target sample and the X-ray detector, but other measurement conditions are the same as the first measurement conditions, and the target sample is gradually changed while changing the incident angle. The X-ray detector detects the intensity of the diffracted X-ray that has been diffracted by the target sample and diffracted by the target sample and passed through the aperture stop means, and the integrated value obtained by integrating the detected intensity is narrowed. A step of setting the diffraction X-ray intensity of the target sample at the opening angle;
Dividing the X-ray intensity of the target sample at a narrow aperture angle by the X-ray intensity of the target sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the target sample;
A reference sample with guaranteed crystal integrity is used as the sample, and the reflection index is independently selected with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays while gradually changing the angle, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and an integrated value obtained by integrating the detected intensity is widened. A step of setting the diffraction X-ray intensity of the reference sample at the opening angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but the other measurement conditions are the same. The X-ray detector detects the intensity of diffracted X-rays that are irradiated with a line, diffracted by the reference sample, and passed through the aperture stop means, and the integrated value obtained by integrating the detected intensity is a narrow aperture angle. The step of setting the diffraction X-ray intensity of the reference sample at
Dividing the X-ray intensity of the reference sample at a narrow aperture angle by the X-ray intensity of the reference sample at a wide aperture angle, and setting this divided value as the diffraction X-ray intensity ratio of the reference sample;
Divide the diffracted X-ray intensity ratio of the target sample by the diffracted X-ray intensity ratio of the reference sample, and use this divided value as the normalized diffracted X-ray intensity ratio. A crystal structure analysis method comprising: determining a crystal structure state of a crystal. In any one of Claims 1 thru | or 3,
The crystal structure analysis method, wherein the reference sample is a Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal, which is a complete crystal substrate. A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition in which the target sample to be analyzed is held in the sample holding unit, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector, The target sample is irradiated with X-rays from an X-ray source, the intensity of diffracted X-rays diffracted by the target sample is detected by the X-ray detector, and the calculation unit calculates the detected intensity at a wide aperture angle. Memorize | stored in the said memory | storage part as the diffraction X-ray intensity of an object sample,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the second measurement conditions are used. The target sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means is detected by the X-ray detector, and the calculation unit calculates the detected intensity. Memorize | stored in the said memory | storage part as the diffraction X-ray intensity of the object sample in a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and the X-ray intensity and wide aperture angle of the target sample at a narrow aperture angle. The relative ratio with the X-ray intensity of the target sample is stored in the storage unit as the diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The reference sample is irradiated with X-rays from the X-ray source under the conditions, the intensity of the diffracted X-ray diffracted by the reference sample is detected by the X-ray detector, and the arithmetic unit widens the detected intensity. Storing in the storage unit as the diffracted X-ray intensity of the reference sample at the aperture angle;
With respect to the second measurement condition, the reflection index is the reflection index selected in the third measurement condition, but other measurement conditions are the same. In the fourth measurement condition, X-rays are emitted from the X-ray source to the reference sample. The X-ray detector detects the intensity of the diffracted X-ray that has been irradiated, diffracted by the reference sample, and passed through the aperture stop means, and the arithmetic unit detects the detected intensity at a reference angle at a narrow aperture angle. Is stored in the storage unit as the diffracted X-ray intensity of
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and the X-ray intensity and wide aperture angle of the reference sample at a narrow aperture angle. The relative ratio with the X-ray intensity of the reference sample is stored in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and the relative ratio between the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample A crystal structure analysis apparatus characterized in that the relative ratio is obtained as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the value of the normalized diffraction X-ray intensity ratio. A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition, a target sample to be analyzed is held in the sample holder, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector. The X-ray source irradiates the target sample with X-rays while gradually changing the angle, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample. Stored in the storage unit as the diffracted X-ray intensity of the target sample at a wide aperture angle,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the incident angle is gradually increased. The X-ray source irradiates the target sample with X-rays while changing the intensity, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means, The calculation unit stores the peak intensity from the detected intensity in the storage unit as the diffraction X-ray intensity of the target sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the target sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the target sample in the storage unit as a diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The X-ray source irradiates the reference sample with X-rays while gradually changing the incident angle under conditions, and the X-ray detector detects the intensity of the diffracted X-ray diffracted by the reference sample, and the calculation The unit stores the peak intensity from the detected intensity in the storage unit as the diffracted X-ray intensity of the reference sample at a wide aperture angle,
The X-ray source while gradually changing the incident angle under the fourth measurement condition in which the reflection index is set to the reflection index selected in the third measurement condition with respect to the second measurement condition but the other measurement conditions are the same. The reference sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample and passed through the aperture stop means is detected by the X-ray detector, and the calculation unit detects the detected intensity Storing the intensity of the peak from the above as the diffracted X-ray intensity of the reference sample at a narrow aperture angle in the storage unit,
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the reference sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the reference sample in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and divides the diffraction X-ray intensity ratio of the target sample by the diffraction X-ray intensity ratio of the reference sample. A crystal structure analysis apparatus characterized in that the division value is used as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the normalized diffraction X-ray intensity ratio value. A sample holder for holding the sample, an X-ray source for irradiating the sample held by the sample holder with X-rays, and an X-ray detector for detecting the intensity of the diffracted X-rays diffracted by the sample; X-ray diffraction having aperture stop means disposed between the sample holder and the X-ray detector and disposed in a light-receiving system where diffracted X-rays travel or disposed away from the light-receiving system Equipment,
An arithmetic unit;
A crystal structure analysis apparatus comprising a storage unit,
In the first measurement condition, a target sample to be analyzed is held in the sample holder, and the aperture stop means is not arranged in the light receiving system between the target sample and the X-ray detector. The X-ray source irradiates the target sample with X-rays while gradually changing the angle, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample. The integrated value obtained by integrating the intensity is stored in the storage unit as the diffraction X-ray intensity of the target sample at a wide aperture angle,
The aperture stop means is arranged in the light receiving system between the target sample and the X-ray detector, but the other measurement conditions are the same as the first measurement conditions, and the incident angle is gradually increased. The X-ray source irradiates the target sample with X-rays while changing the intensity, and the X-ray detector detects the intensity of the diffracted X-rays diffracted by the target sample and passing through the aperture stop means, The calculation unit stores the integrated value obtained by integrating the detected intensity in the storage unit as the diffracted X-ray intensity of the target sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the target sample at a narrow aperture angle and the X-ray intensity of the target sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the target sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the target sample in the storage unit as a diffracted X-ray intensity ratio of the target sample,
A reference sample in which the integrity of the crystal is guaranteed is held in the sample holder, and the reflection index is an independently selected reflection index with respect to the first measurement condition, but the other measurement conditions are the same. The X-ray source irradiates the reference sample with X-rays while gradually changing the incident angle under conditions, and the X-ray detector detects the intensity of the diffracted X-ray diffracted by the reference sample, and the calculation The unit stores an integrated value obtained by integrating the detected intensity as the diffracted X-ray intensity of the reference sample at a wide aperture angle in the storage unit,
The X-ray source while gradually changing the incident angle under the fourth measurement condition in which the reflection index is set to the reflection index selected in the third measurement condition with respect to the second measurement condition but the other measurement conditions are the same. The reference sample is irradiated with X-rays, the intensity of the diffracted X-rays diffracted by the reference sample and passed through the aperture stop means is detected by the X-ray detector, and the calculation unit detects the detected intensity Is stored in the storage unit as the diffracted X-ray intensity of the reference sample at a narrow aperture angle,
The calculation unit reads the X-ray intensity of the reference sample at a narrow aperture angle and the X-ray intensity of the reference sample at a wide aperture angle from the storage unit, and calculates the X-ray intensity of the reference sample at a narrow aperture angle as a wide aperture angle. And dividing the divided value by the X-ray intensity of the reference sample in the storage unit as the diffracted X-ray intensity ratio of the reference sample,
The calculation unit reads the diffraction X-ray intensity ratio of the target sample and the diffraction X-ray intensity ratio of the reference sample from the storage unit, and divides the diffraction X-ray intensity ratio of the target sample by the diffraction X-ray intensity ratio of the reference sample. A crystal structure analysis apparatus characterized in that the division value is used as a normalized diffraction X-ray intensity ratio, and the crystal structure state of the target sample is determined from the normalized diffraction X-ray intensity ratio value. In any one of Claims 5 thru | or 7,
The crystal structure analysis apparatus, wherein the reference sample is a Si substrate crystal, a Ge substrate crystal, a GaAs substrate crystal, or an InP substrate crystal, which is a complete crystal substrate.

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