JP2003194741A - X-ray diffraction apparatus, reflected X-ray measurement method, and reciprocal lattice space map creation method - Google Patents

Abstract

(57) [Problem] To quickly and efficiently evaluate the crystallinity of a crystalline material, particularly a thin film crystalline material. An XRD includes a detector having a plurality of light receiving elements arranged in a predetermined pattern, so that a reciprocal lattice space map can be created at high speed. Further, by moving the detector 51 by a distance smaller than the interval at which the light receiving elements are arranged and performing scanning a plurality of times, the resolution in scanning can be increased. Further, by changing the distance between the detector 51 and the stage 40, the resolution of the simultaneous detection width can be adjusted. Further, the resolution of the simultaneous detection width can also be adjusted by changing the angle of the detector 51 with respect to the light receiving axis.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray diffractometer, a reflection X-ray measuring method and a reciprocal lattice space map creating method for evaluating crystallinity of a crystalline material.

[0002]

2. Description of the Related Art Conventionally, in order to evaluate the crystal structure of a crystalline material, XRD (X-ray diffractomet) utilizing X-ray diffraction has been used.
er) is used. The XRD is a device for evaluating crystallinity of a crystalline material by irradiating a sample with X-rays and measuring reflected X-rays due to Bragg reflection from a crystal plane.
Hereinafter, a method of evaluating a crystalline material using XRD will be specifically described.

A crystal has a structure in which atoms are arranged in a three-dimensional order. The atomic array structure is formed by repeating a certain unit structure (unit lattice). The unit lattice is a parallelepiped formed by lattice points, and is defined by the lengths a, b, and c of three sides that are not parallel to each other in the unit lattice and the angles α, β, and γ formed by these sides. The structure of is determined. Then, from the structure of the unit cell, the crystal plane (direction of crystal plane or spacing)
Is specified. That is, by analyzing the crystal plane,
It is possible to evaluate the crystal structure.

FIG. 9 is a diagram showing a parallelepiped ABCD-EFGH which is an example of the structure of a unit lattice. In FIG. 9, the vertices A to H of the parallelepiped ABCD-EFGH are lattice points, and among the vertices A to H, three points that are not on the same line are arbitrarily selected to specify a predetermined crystal plane. . That is, a crystal structure having a parallelepiped ABCD-EFGH as a unit lattice includes a plurality of crystal planes, and each of these crystal planes Bragg-reflects an incident X-ray.

Therefore, in the evaluation of the crystalline material using XRD, the sample is irradiated with X-rays from various angles,
The reflected X-ray that satisfies the Bragg reflection condition is detected. Then, the crystal plane is specified based on the detected distribution characteristic of the reflected X-rays, and further the crystal structure of the crystal material to be evaluated is evaluated. Here, the concept of the reciprocal lattice space, which is generally used to easily evaluate the crystal structure, is introduced.

In a real space, the crystal plane spacing of the sample is d,
The incident angle of X-rays on the target crystal plane is θ, and the wavelength is λ
Then, the condition that the incident X-ray reflects Bragg is 2dsinθ
= Nλ (n is an arbitrary integer). At this time, if the above equation is modified by matching the dimension with the wave number 1 / λ detected by XRD, 2 (1 / λ) sin θ = n (1 / d).
Here, if wave number 1 / λ = k and 1 / d = q, then 2 ksi
It can be written that nθ = nq. Note that n = 1 may be set here in view of the crystal plane spacing and the scale of the wavelength of X-rays. That is, q =
An equation of 2 ksin θ is derived.

This expression is an expression representing the Bragg reflection condition in a coordinate system having a wave number dimension, and such a coordinate space is called a reciprocal lattice space. Next, in the reciprocal lattice space, assume that a wave number vector of incident X-rays, ki and a wave number vector of reflected X-rays, and a triangle OLM having kf as two sides. It should be noted that | vector ki | = | vector kf | = k. FIG. 10 is a diagram showing a triangle OLM.

In the triangle OLM, the vector ki and the vector kf start from the vertex L and the angle between them is ∠OLM = 2θ. At this time, the length of the side connecting the end point of the vector ki (vertex O) and the end point of the vector kf (vertex M) is 2ksin θ = q. When the vertex O is the origin, the vertex M is Points (reciprocal lattice points) that satisfy the reflection condition are shown. Further, θ indicates the incident angle of the incident X-ray with respect to the target crystal plane in the real space, as described above. Of the reciprocal lattice point group distributed in the reciprocal lattice space, a plan view in which a specific lattice point is focused and an area in the vicinity thereof is enlarged is called a reciprocal lattice space map.

By introducing such a concept of the reciprocal lattice space, when evaluating a crystal material by XRD, the incident direction of X-rays is variously changed and the Bragg reflected light is measured to obtain the reciprocal lattice space. It is possible to detect the lattice points and easily evaluate the crystal structure of the crystal material from the distribution characteristic (reciprocal lattice space map). Next, the spread of reciprocal lattice points in an actual crystal material will be described. This is due to the deviation from the ideal perfect periodic structure. The crystal material to be evaluated has variations in the crystal plane spacing or crystal plane orientation of the sample itself. In the reciprocal lattice space map, the reciprocal lattice spacing spreads in the direction of the distance from the origin of the reciprocal lattice space due to the variation of the crystal plane spacing, and the rotation direction around the origin of the reciprocal lattice space due to the variation of the crystal plane direction. Spreads over.

There are various crystal materials, such as single crystal materials, polycrystal materials, and materials having an intermediate crystal structure such as an epitaxial film on a substrate. Then, for a sample such as a polycrystalline material in which a plurality of crystal grains are uniformly mixed in the crystal material, the reciprocal lattice points of the respective crystal grains are continuously annularly distributed in the reciprocal lattice space map. It will be. This distribution of reciprocal lattice points in a ring is called a Debye ring. On the other hand, in a sample in which the periodic structure is orderly present, such as an ideal single crystal, the reciprocal lattice points are distributed in discrete point shapes in the reciprocal lattice space map.

Here, a conventional XRD used for evaluating the crystal structure of a crystal material will be described. FIG. 11 is a schematic diagram showing the configuration of a conventional XRD 100. In FIG. 11, the XRD 100 includes a main body 110 and an X-ray irradiation unit 120.
An incident X-ray arm 130 having a tip is provided, a stage 140 for mounting a sample, and a reflection X-ray arm 160 having a light receiving section 150 for receiving the X-ray reflected by the sample at the tip.

In the XRD 100, the incident X-ray arm 1
30 is rotatably installed on the main body 110. And
By rotating the incident X-ray arm 130 within a predetermined plane, it is possible to irradiate the sample installed on the stage 140 with X-rays emitted from the X-ray irradiator 120 from an arbitrary angle. The reflective X-ray arm 160 is also rotatably installed on the main body 110. Then, the reflection X-ray arm 160
By rotating and changing the position of the light receiving unit 150, it is possible to measure the Bragg reflected light at various positions of the X-ray reflected on the sample.

Therefore, the crystal structure of the sample can be examined by scanning while changing the positions of the incident X-ray arm 130 and the reflective X-ray arm 160 in various ways. In addition,
The XRD100 has a slightly different configuration depending on the type of sample to be evaluated, and is an XRD for evaluating polycrystalline materials.
Let 100 be the angle of the incident X-ray arm 130 with respect to the stage 140 (incident angle of X-ray to the sample),
The reflection X-ray arm 160 is also changed so that the light receiving unit 150 always captures the X-ray reflected from the sample at the reflection angle of θ. That is, the XRD 100 for evaluating a polycrystalline material measures the distribution of reciprocal lattice points along a straight line parallel to the normal direction of the surface of the stage 140 in the reciprocal lattice space.

On the other hand, the XRD 100 for evaluating a sample having an orientation or lattice distortion such as a thin film crystal material formed on a substrate needs to examine a wide distribution of reciprocal lattice points in a reciprocal lattice space. Therefore, in addition to the above configuration,
The incident X-ray arm 130 and the reflective X-ray arm 160 can change their positions independently of each other, and the stage 140 can change its posture with respect to the main body 110.

[0015]

However, the conventional XRD for evaluating the orientation and the lattice distortion of the thin film crystal material is used.
In the above, since the light receiving section was provided with only one light receiving element, in order to obtain the reciprocal lattice space map, it was necessary to sequentially scan the vicinity of the reciprocal lattice point with the one light receiving element. That is, to create a reciprocal lattice space map,
It was supposed to spend a huge amount of time.

Here, there is known a conventional XRD for evaluating a polycrystalline material, in which a light receiving portion is provided with a sensor in which a plurality of light receiving elements are arranged in a line. However, since this XRD assumes only the evaluation of the crystallinity of the polycrystalline material, the movement of the arm and stage is limited as described above, and the distribution of a wide range of reciprocal lattice points in the reciprocal lattice space is limited. Was something I couldn't look into. Also,
When evaluating the orientation and lattice strain distribution of thin film crystal materials, 1
Since it is necessary to expand the vicinity of one lattice point and create a more precise reciprocal lattice space map, it is important to properly adjust the measurement accuracy (resolution) compared to when evaluating polycrystalline materials. Become.

An object of the present invention is to quickly and efficiently evaluate crystallinity such as orientation and lattice distortion peculiar to crystalline materials, especially thin film crystalline materials.

[0018]

The present invention is capable of irradiating an X-ray in a predetermined irradiation axis direction with a stage on which a sample is placed (for example, the stage 40 in FIG. 1), and the irradiation axis is set on the stage. The irradiation unit (for example, the X-ray irradiation unit 20 and the incident X-ray arm 30 in FIG. 1) installed toward the reception unit can receive reflected X-rays from a predetermined light-receiving axis direction, and the light-receiving axis is set on the stage. A light-receiving unit (for example, the light-receiving unit 50 and the reflection X-ray arm 60 in FIG. 1) installed to face each other, and independently adjusts the angle of the irradiation axis with respect to the stage and the angle of the light-receiving axis with respect to the stage. It is a possible X-ray diffractometer, characterized in that the light receiving unit includes a detector (for example, the detector 51 in FIG. 1) including a plurality of light receiving elements arranged in a predetermined pattern.

Further, it is characterized in that the detector can be continuously moved in the light receiving axis direction. Further, the detector is characterized in that the installation angle with respect to the light receiving axis can be continuously changed. Also,
The plurality of light receiving elements are arranged in a row at a predetermined interval.

Further, the plurality of light receiving elements are characterized in that the light receiving elements arranged in one row at predetermined intervals are arranged in a plurality of rows. Further, each of the columns forming the plurality of columns is arranged so as to be offset from other adjacent columns by a distance smaller than the predetermined interval. The stage is characterized in that the orientation (tilt angle) of the installation surface on which the sample is installed can be adjusted.

The stage is characterized in that the rotational angle position within the installation surface on which the sample is installed can be adjusted. The irradiating section is capable of irradiating white light as the X-ray. It is possible to irradiate X-rays in a predetermined irradiation axis direction with the stage on which the sample is installed, and it is possible to receive reflected X-rays from a predetermined light-receiving axis direction with the irradiation unit installed with the irradiation axis facing the stage Is provided with a light receiving portion installed with the light receiving axis facing the stage, the angle of the irradiation axis with respect to the stage,
The angle of the light-receiving axis with respect to the stage can be adjusted independently, and the plurality of light-receiving elements are used by using an X-ray diffractometer having a detector including a plurality of light-receiving elements arranged in a predetermined pattern in the light-receiving section. It is characterized in that the reflected X-rays are measured in a single measurement process for the entire space within a predetermined range based on the respective detection signals.

The resolution in reflection X-ray measurement is arbitrarily adjusted by moving the detector in the light receiving axis direction. The resolution in reflected X-ray measurement is arbitrarily adjusted by changing the installation angle of the detector with respect to the light receiving axis.
By the operation of changing the angle of the irradiation axis with respect to the stage while maintaining the angle (for example, 2π−2θ in FIG. 3) formed by the irradiation axis of the irradiation section and the light reception axis of the light receiving section,
Reflection X in one measurement process for the entire space within a predetermined range
The feature is that the line is measured.

The plurality of light receiving elements are arranged at a predetermined interval, and the reflected X-ray is measured at an arbitrary resolution by measuring the reflected X-ray by moving the detector by a movement amount smaller than the predetermined interval. It is characterized by that. It is a method of creating a reciprocal lattice space map using the X-ray diffractometer. The X
Using a line diffractometer, by performing In-Plane measurement on the sample, the in-plane rotation angle of the crystal contained in the sample,
Characteristics based on the angle formed by the wave vector of the incident X-rays and the wave vector of the reflected X-rays (for example, φ-2θ characteristic in FIG. 8)
It is characterized by getting.

According to the present invention, the reciprocal lattice space map can be created at high speed because the detector including the plurality of light receiving elements arranged in the predetermined pattern is provided. In addition, the resolution in scanning can be improved by moving the detector by a distance smaller than the interval in which the light receiving elements are arranged and scanning a plurality of times. Further, by providing a mechanism for continuously changing the distance between the detector and the stage, the resolution in scanning can be adjusted arbitrarily. Further, by providing a mechanism for continuously changing the installation angle of the detector with respect to the light receiving axis, the resolution in scanning can be arbitrarily adjusted.

Further, according to the present invention, the In-Plane measurement can be performed at high speed. Further, by using a white light source as the X-ray source, the rocking curve measurement (measurement of the distribution characteristic of the reflected X-ray intensity in the vicinity of the direction in which the Bragg reflected light of the crystal is measured) of the detector is extremely short. Can be done in time.

[0026]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of an XRD according to the present invention will be described in detail below with reference to the drawings. First, the configuration will be described. FIG. 1 is a schematic diagram showing the configuration of an XRD 1 according to this embodiment. In FIG. 1, XRD1 is a main body 1
0, and an incident X-ray arm 30 including the X-ray irradiation unit 20,
It is configured to include a stage 40 on which a sample is placed and a reflective X-ray arm 60 including a light receiving unit 50 that receives the X-ray reflected by the sample.

In FIG. 1, the main body 10 includes a control unit for controlling the entire XRD 1 and an interface for outputting measurement data. The X-ray irradiation unit 20 generates X-rays and irradiates the generated X-rays in a predetermined irradiation axis direction. The X-ray irradiator 20 is installed on the incident X-ray arm 30 with its irradiation axis facing the stage 40, and as will be described later, even if the incident X-ray arm 30 rotates, the X-ray irradiator is always provided. The irradiation axis of 20 is directed to the stage 40.

The incident X-ray arm 30 is rotatably installed on the main body 10 and its angular position with respect to the stage 40 can be changed. In addition, the incident X-ray arm 30
An X-ray irradiation unit 20 is provided at the tip. That is, the incident angle of the irradiation axis of the X-ray irradiation unit 20 with respect to the stage 40 can be adjusted by rotating the incident X-ray arm 30.
The stage 40 can be installed with the sample to be evaluated fixed at a predetermined sample installation position, and the posture (tilt angle) with respect to the main body 10 can be freely changed within a predetermined range. That is, the stage 40 changes from the reference posture to
It is equipped with a mechanism capable of adjusting the normal direction of the surface on which the sample is installed (installation surface) vertically and horizontally in FIG. In addition, the stage 40 can rotate in the installation surface direction and adjust the height of the installation surface in a reference posture.

The sample placed on the stage 40 is a thin film crystal material or the like formed substantially parallel to the substrate surface, and is placed so that the sample surface and the installation surface of the stage 40 are substantially parallel to each other. The light receiving section 50 includes a detector 51 in which a plurality of light receiving elements are arranged in a predetermined pattern (for example, one row or a matrix), and the detector 51 detects X-rays incident from a predetermined light receiving axis direction. To be done. The light-receiving unit 50 has a light-receiving axis that always faces the stage 40, like the X-ray irradiation unit 20.

Here, the detector 51 will be further described. The detector 51 includes a plurality of light receiving elements that can output detection signals by receiving X-rays. The plurality of light receiving elements are arranged in a predetermined pattern. FIG. 2 is a diagram showing an example of a pattern in which the light receiving elements of the detector 51 are arranged. In FIG. 2, the light receiving elements of the detector 51 are, for example, (a) arranged in a line at a predetermined interval on a straight line, (b) arranged on a curved line such as an arc, or (c). ) It is possible to arrange in multiple columns.

The distance between these adjacent light receiving elements is
It is a factor that determines the resolution in X-ray detection. Therefore, when arranging the light receiving elements in a plurality of rows, by arranging the adjacent rows so as to be displaced by a distance smaller than the distance between the light receiving elements, an effect of improving the resolution can be obtained. In addition, when performing the measurement process of the reflected X-rays, after one measurement process, the detector 51 is displaced by a distance less than the distance between the light receiving elements, and the measurement process is further performed, which is the same effect as enhancing the resolution. Can be obtained.

Further, the detector 51 can change the installation angle with respect to the light receiving axis, which changes the density of the light receiving elements viewed from the sample (stage 40),
The same effect as increasing the resolution can be obtained.
The reflective X-ray arm 60 is rotatably installed on the main body 10 and can change its angular position with respect to the stage 40. The rotation axis of the reflection X-ray arm 60 is the same as the rotation axis of the incident X-ray arm 30.

Further, the reflection X-ray arm 60 includes the light receiving section 50.
Is movably provided at an arbitrary position in the radial direction of rotation. That is, by rotating the reflection X-ray arm 60, the angle (reflection angle) of the light-receiving axis of the light-receiving unit 50 with respect to the stage 40 can be adjusted, and the light-receiving unit 50 can be rotated by the radius of rotation of the reflection X-ray arm 60. By moving in the direction, the distance between the stage 40 and the light receiving unit 50 can be continuously adjusted. Under such a configuration, it is possible to irradiate the sample installed on the stage 40 with X-rays from the X-ray irradiator 20 and measure the reflected X-rays by the light receiver 50. That is, the Bragg reflected light can be detected by the light receiving unit 50.

Further, since the light receiving section 50 is provided with the detector 51, it is possible to detect the Bragg reflected light by performing the measurement processing once for the reciprocal lattice space within a certain range. Furthermore, since the incident X-ray arm 30 and the reflection X-ray arm 60 can independently adjust the angular position with respect to the stage 40, it is possible to detect Bragg reflected light in an arbitrary reciprocal lattice space. Next, a measuring method when creating a reciprocal lattice space map using XRD1 will be described.

FIG. 3 is a conceptual diagram showing the principle of evaluating a sample using XRD1. In FIG. 3, the X-ray irradiation unit 2
The incident X-rays irradiated by 0 impinge on the sample at an incident angle ω with respect to the sample surface placed parallel to the stage 40.
At this time, the incident X-ray and the specific crystal plane of the sample are
Bragg reflection occurs when the reflection condition of is satisfied. Then, when the angular position of the light receiving unit 50 with respect to the sample is the angular position at which the reflected light that satisfies the Bragg reflection condition reaches on the specific crystal plane, the light receiving unit 50 detects the Bragg reflected light. Here, the light receiving unit 50 detects the reflected X-rays by the detector 51 including a plurality of light receiving elements.

Therefore, the angle between the wave vector of the incident X-ray (hereinafter referred to as "incident vector") ki and the wave vector of the reflected X-ray (hereinafter referred to as "reflection vector") kf (2π-2θ). ) And variously changing the incident angle ω of the incident X-ray with respect to the sample, and examining the angular position of the light receiving section 50 where the Bragg reflected light is measured, the crystal structure of the sample can be evaluated. It is possible to simultaneously measure the space in which each of the light receiving elements is located.

Although the concept of crystal structure evaluation in the real space is shown in FIG. 3, the evaluation of the crystal structure in the reciprocal lattice space will be considered. FIG. 4 is a diagram showing an incident vector ki and a reflection vector kf in the reciprocal lattice space. In FIG. 4, at the tip of the reflection vector kf,
A range in which a plurality of light receiving elements of the detector 51 can simultaneously detect reflected X-rays (hereinafter, referred to as “simultaneous detection width”) is shown.

In FIG. 4, when an ideal single crystal material is evaluated as a sample, the reciprocal lattice points have a dot shape. However, in reality, each reciprocal lattice point has a certain spread due to the variation in the crystal structure. Hereinafter, a method of operating the XRD 1 in order to obtain the reciprocal lattice point distribution (reciprocal lattice space map) including the constant spread will be described. Figure 3
As shown in FIG. 6, the detection position of the reflected X-ray is specified by using the incident angle ω of the X-ray with respect to the sample (stage 40) and the angle between the incident vector ki and the reflection vector kf (2π-2θ) as parameters. .

Therefore, in the reciprocal lattice space, the XRD 1 is operated to appropriately measure the reflected X-ray distribution near the reciprocal lattice point. First, an operation for a method (first method) for creating a reciprocal lattice space map at high speed will be described. In order to create the reciprocal lattice space map at high speed, considering the effective use of the simultaneous detection width of the detector 51, the detector 51 is moved in a direction more perpendicular to the simultaneous detection width direction.

That is, in the reciprocal lattice space, the angle between the incident vector ki and the reflection vector kf is fixed, and the incident angle ω is scanned in the vicinity of the reciprocal lattice point over the range of δω (see FIG. 5). This is stage 4 of XRD1 in real space.
This corresponds to the operation of changing the angular position of the incident X-ray arm 30 with respect to the stage 40 while fixing the relative angular position of the incident X-ray arm 30 and the reflective X-ray arm 60 with 0 fixed.

By this method, a reciprocal lattice space map in a certain range can be created at high speed with the resolution of the detector 51 (the resolution based on the arrangement of a plurality of light receiving elements). Next, the operation for the method (second method) for accurately producing the reciprocal lattice space map will be described. When creating a reciprocal lattice space map, it is desired to measure the vicinity of the reciprocal lattice point in more detail, particularly when evaluating a thin film crystal material containing a minute orientation distribution or lattice distortion. On the other hand, the detector 51
The resolution in one scan is determined by the arrangement of the light receiving elements of.

Therefore, in the reciprocal lattice space, after scanning near the reciprocal lattice point with an arbitrary incident angle ω as a reference, the angle between the incident vector ki and the reflection vector kf is set to a small amount δθ (for example, the interval between a plurality of light receiving elements) Less than) and again scan around the reciprocal lattice point with reference to the incident angle ω (see FIG. 6). This is stage 4 of XRD1 in real space.
With 0 fixed, the relative angular position between the incident X-ray arm 30 and the reflective X-ray arm 60 is fixed, and the angular position of the incident X-ray arm 30 with respect to the stage 40 is changed from a specific position by a predetermined amount. Then, the relative angular position between the incident X-ray arm 30 and the reflective X-ray arm 60 is slightly changed, and the angular position of the incident X-ray arm 30 with respect to the stage 40 is again changed by a predetermined amount from the specific position. It corresponds to the operation.

By this method, the distance between the light receiving elements of the detector 51 is complemented, and it becomes possible to perform scanning with higher resolution, that is, to create a more accurate reciprocal lattice space map. In addition, a method of changing the distance between the light receiving unit 50 and the stage 40 for adjusting the resolution in the measurement of the reciprocal lattice points (third method)
The method) will be described. In the reciprocal lattice space, a plurality of light receiving elements included in the detector 51 are discretely arranged in a predetermined pattern in the simultaneous detection width. That is, the number of points at which the reflected X-rays are detected in the simultaneous detection width is determined by the configuration of the detector 51, and thereby the resolution in scanning is determined.

Therefore, in the reciprocal lattice space, the resolution of the detector 51 is relatively changed by changing the simultaneous detection width. The operation of reducing the simultaneous detection width in the reciprocal lattice space corresponds to the operation of moving the detector 51 away from the sample (stage 40) in the real space, and the operation of expanding the simultaneous detection width in the reciprocal lattice space is the real space. In, it corresponds to the operation of bringing the detector 51 close to the sample. Specifically, in the XRD 1, when reducing the simultaneous detection width, the light receiving unit 50 installed in the reflection X-ray arm 60.
Corresponds to the operation of increasing the distance between the sample and the sample (stage 40), and in the case of enlarging the simultaneous detection width, it corresponds to the operation of reducing the distance between the light receiving unit 50 installed in the reflective X-ray arm 60 and the sample.

By this method, the same detector 51 can be used to realize scanning with a desired resolution. In order to obtain a desired resolution, the length of the reflective X-ray arm 60 needs to be continuously changed and the distance between the light receiving unit 50 and the sample (stage 40) needs to be arbitrarily adjusted. Further, by increasing the density of the light receiving elements, the S / N (Signal /
Noise) ratio can be improved. As with the third method, a method (fourth method) of adjusting the angle of the detector 51 with respect to the light receiving axis is possible as a method of adjusting the resolution in the measurement of the reciprocal lattice points. The operation for performing will be described.

In the real space, changing the installation angle of the detector 51 of the XRD 1 with respect to the light receiving axis corresponds to changing the simultaneous detection width located at the tip of the reflection vector kf in the reciprocal lattice space. , This is the third
It has the same effect as the method. Therefore, the resolution in scanning can be easily adjusted by this method.

Next, a method for evaluating the in-plane orientation of crystals using XRD1 will be described. In addition, by using XRD1 in the present embodiment, in-plane
It is also possible to perform the measurement at high speed. The in-plane measurement is the following crystallinity evaluation method. As shown in FIG. 7, by irradiating the sample with X-rays at an incident angle (eg, less than 1 °) in the vicinity of a critical angle at which total reflection occurs, X-rays having a component parallel to the sample surface are generated. And that X
Regarding the line component Br on the crystal plane perpendicular to the sample surface
Agg reflection occurs, and the reflected X-ray is detected from the surface of the sample with a small angle of reflection. As a result, in a sample for which crystallinity evaluation is difficult by ordinary X-ray diffraction, such as an ultra-thin film crystal material that does not have many continuous crystal planes in the thickness direction, the spread in the area direction of the sample is used ( It is possible to evaluate the crystallinity by considering the thickness).

In-Plan using XRD1 according to the present invention
In the e measurement, the reciprocal lattice space map can be created as in the first to fourth methods. However, since the sample is irradiated with X-rays at a small incident angle ω (for example, ω << 1 °), it is necessary to control the tilt angle of the stage 40 and the rotation angle in the installation plane direction. . Specifically, in FIG. 7, by adjusting the angular position of the incident X-ray arm 30 with respect to the stage 40, the height of the stage 40, and the tilt angle, the incident angle δ of the X-ray is set to a predetermined minute angle.

Then, the reflected X-rays are measured while changing the angular position (2π-2θ) of the reflective X-ray arm 60 and the rotation angle φ of the stage 40 in the in-plane direction. this is,
In the first to fourth methods, an operation of measuring reflected X-rays while changing an incident angle ω of the X-ray with respect to the sample and a relative angular position between the incident X-ray arm 30 and the reflected X-ray arm 60. It is the same operation. Therefore, also in the In-Plane measurement, the same effects as those of the first to fourth methods are performed, so that the above-described effects are obtained.

As described above, by performing the in-plane measurement, it is possible to evaluate the variation in the rotation direction with respect to the substrate surface of the sample (in-plane orientation). Further, as shown in FIG. 8, the measured in-plane orientation is represented on the φ-2θ plane by using the rotation angle φ and the angle 2θ formed by the incident vector ki and the reflection vector kf as parameters, and It is possible to separately evaluate the rotation distribution and the distribution of the intervals of the crystal planes perpendicular to the substrate surface.

As described above, the XRD according to the present embodiment
Since No. 1 includes the detector 51, the reciprocal lattice space map can be created at high speed. Further, by moving the detector 51 by a distance smaller than the interval in which the light receiving elements are arranged and scanning a plurality of times, the resolution in scanning can be improved. Further, the resolution of the simultaneous detection width can be adjusted by changing the distance between the detector 51 and the stage 40. Further, the resolution of the simultaneous detection width can be adjusted by changing the angle of the detector 51 with respect to the light receiving axis.

Further, in-plane measurement can be performed using XRD1. In the present embodiment, by using a white light source as the X-ray source, each of the plurality of light receiving elements constituting the detector 51 has a Bragg plane from a plane having the same crystal plane spacing but different orientations.
Since the reflected light is detected at the same time, the rocking curve measurement (the measurement of the distribution characteristic of the reflected X-ray intensity in the vicinity of the direction in which the Bragg reflected light of the crystal is measured) can be performed in an extremely short time.

That is, within the range of the azimuth width determined from the simultaneous detection width, the rocking curve can be measured without any scanning.

[0054]

As described above, according to the present invention, the reciprocal lattice space map can be created at high speed because the detector including the plurality of light receiving elements arranged in the predetermined pattern is provided. In addition, the resolution in scanning can be improved by moving the detector by a distance smaller than the interval in which the light receiving elements are arranged and scanning a plurality of times. Further, the resolution in scanning can be adjusted by changing the distance between the detector and the stage. Further, the scanning resolution can be adjusted by changing the installation angle of the detector with respect to the light receiving axis.

Further, according to the present invention, it is possible to perform In-Plane measurement. Further, by using a white light source as the X-ray source, the rocking curve measurement (measurement of the distribution characteristic of the reflected X-ray intensity in the vicinity of the direction in which the Bragg reflected light of the crystal is measured) of the detector is extremely short. Can be done in time.

[Brief description of drawings]

FIG. 1 is a schematic diagram showing a configuration of an XRD 1 according to the present embodiment.

FIG. 2 is a diagram showing an example of a pattern in which light receiving elements of a detector 51 are arranged.

FIG. 3 is a conceptual diagram showing the principle of evaluating a sample using XRD1.

FIG. 4 is a diagram showing an incident vector ki and a reflection vector kf in a reciprocal lattice space.

FIG. 5 is a diagram showing a measurement operation in which the angle between the incident vector ki and the reflection vector kf is fixed, and the incident angle ω is scanned in the vicinity of the reciprocal lattice point over the range of δω.

FIG. 6 is a diagram showing a measurement operation for scanning near the reciprocal lattice point while slightly changing the angle between the incident vector ki and the reflection vector kf by δθ.

FIG. 7 is a conceptual diagram showing In-Plane measurement.

FIG. 8 is a view in which the in-plane orientation of the crystal material and the distribution of the crystal plane intervals are separated and represented on the φ-2θ plane.

FIG. 9 is a parallelepiped ABC that is an example of the structure of a unit lattice.
It is a figure which shows D-EFGH.

FIG. 10 is a diagram showing a triangle OLM.

FIG. 11 is a schematic diagram showing a configuration of a conventional XRD 100.

[Explanation of symbols]

1,100 XRD 10,110 body 20,120 X-ray irradiation unit 30,130 Incident X-ray arm 40,140 stages 50,150 Light receiving part 51 detector 60,160 Reflective X-ray arm

Claims (16)

[Claims] 1. A stage on which a sample is installed, X-rays can be irradiated in a predetermined irradiation axis direction, and an irradiation unit installed with the irradiation axis facing the stage, and reflection from a predetermined light receiving axis direction. It is possible to receive X-rays, and a light receiving section is installed with the light receiving axis facing the stage, and the angle of the irradiation axis with respect to the stage and the angle of the light receiving axis with respect to the stage can be adjusted independently. The X-ray diffractometer, wherein the light receiving unit includes a detector including a plurality of light receiving elements arranged in a predetermined pattern. 2. The X-ray diffraction apparatus according to claim 1, wherein the detector can be continuously moved in the light receiving axis direction. 3. The X-ray diffraction apparatus according to claim 1, wherein the detector is capable of continuously changing an installation angle with respect to the light receiving axis. 4. The X-ray diffractometer according to claim 1, wherein the plurality of light receiving elements are arranged in a row at predetermined intervals. 5. The X-ray diffraction according to claim 1, wherein the plurality of light receiving elements are arranged in a plurality of rows at a predetermined interval. apparatus. 6. The X-ray diffractometer according to claim 5, wherein each of the plurality of columns is arranged so as to be offset from other columns adjacent to each other by a distance smaller than the predetermined interval. 7. The stage is capable of adjusting the orientation of an installation surface on which the sample is installed.
X-ray diffraction apparatus in any one of. 8. The X-ray diffractometer according to claim 1, wherein the stage is capable of adjusting a rotational angle position within an installation surface on which the sample is installed. 9. The X-ray diffractometer according to claim 1, wherein the irradiation section can emit white light as the X-ray. 10. A stage on which a sample is set, X-rays can be irradiated in a predetermined irradiation axis direction, and an irradiation unit installed with the irradiation axis facing the stage, and reflection from a predetermined light receiving axis direction. It is possible to receive X-rays, and a light receiving section is installed with the light receiving axis facing the stage, and the angle of the irradiation axis with respect to the stage and the angle of the light receiving axis with respect to the stage can be adjusted independently. Is, using an X-ray diffraction device having a detector composed of a plurality of light receiving elements arranged in a predetermined pattern in the light receiving section, based on the detection signals of each of the plurality of light receiving elements, for the entire space of a predetermined range A method for measuring reflected X-rays, wherein the reflected X-rays are measured in a single measurement process. 11. The reflected X-ray measurement method according to claim 10, wherein the resolution in the reflected X-ray measurement is arbitrarily adjusted by moving the detector in the light receiving axis direction. 12. The reflection X-ray measurement method according to claim 10, wherein the resolution in reflection X-ray measurement is arbitrarily adjusted by changing the installation angle of the detector with respect to the light receiving axis. 13. The operation of changing the angle of the irradiation axis with respect to the stage while maintaining the angle between the irradiation axis of the irradiation section and the light reception axis of the light receiving section is performed once for the entire space within a predetermined range. The reflected X-ray measurement method according to claim 10, wherein the reflected X-ray measurement is performed in the measurement process. 14. The reflected X-ray measurement is performed at an arbitrary resolution by arranging the plurality of light receiving elements at a predetermined interval and measuring the reflected X-ray by moving the detector by a movement amount smaller than the predetermined interval. 10. The method according to claim 10, wherein
The reflected X-ray measurement method according to any one of 3 above. 15. A reciprocal lattice space map creating method using the X-ray diffractometer according to claim 1. 16. An in-plane rotation angle distribution of crystals contained in the sample by performing In-Plane measurement on the sample using the X-ray diffraction apparatus according to claim 1. A reciprocal lattice space map creating method, characterized in that a characteristic based on an angle formed by a wave number vector of an incident X-ray and a wave number vector of a reflected X-ray is obtained.