JP2000314708A - X-ray topography device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray topography device capable of making an X-ray topography measurement of a sample under a special condition. SOLUTION: A sample S is irradiated with an X-ray from an x-ray source F being regulated by incident side slits 22a, 22b so that the X-ray diffracted by the sample S is detected by an X-ray film 7a or a CCD sensor 7b. An X-ray incident angle ω is adjusted relative to the sample S by rotating an ω movable carriage 11 about an ω axis Xω in the directions of arrows C-C', and a slit 9 and the ω movable carriage 11 are translationally moved by translationally moving a base 2 in the directions of arrows A-A', so that a diffracted X-ray image corresponding to the whole surface of the sample S is detected by the x-ray film 7a or the CCD sensor 7b. Since the sample S is held static during measurement, a special condition can be ensured by attaching accessory equipment, such as a sample formation growth furnace 8, to the sample S.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray topography apparatus for recording a diffracted X-ray from a sample on an X-ray plate or the like with a one-to-one geometric correspondence with the sample.

[0002]

2. Description of the Related Art A lattice defect or the like inside a crystal of a single crystal material is represented by X.
It is conventionally known that there is an X-ray topography as a method for directly observing using a line. The X-ray topography includes a single crystal method such as a Lang method and a Berg Barrett method, and a different two crystal method. The Lang method is generally known as a representative of a single crystal method in a transmission configuration, and the Berg Barrett method is generally known as a representative of a single crystal method of surface reflection.

In the single crystal method, a primary X-ray generated from an X-ray source is used.
X-rays are directly incident on the sample crystal and diffracted by the sample.
An image is formed by a line on a two-dimensional X-ray detecting means such as an X-ray dry plate. On the other hand, in the two-crystal method, primary X-rays generated from an X-ray source are incident on a first crystal, X-rays diffracted by the first crystal are incident on a sample crystal, and X-rays diffracted by the sample crystal are used. An image is formed on the two-dimensional X-ray detection means.

In the one-crystal method, the degree of satisfying the diffraction condition changes due to a partial shift of the crystal orientation, and a black-and-white contrast corresponding to a lattice defect occurs due to a diffraction effect such as an extinction effect and a Borman effect. In contrast, in the two-crystal method, the first crystal and the second crystal (that is,
By diffracting the X-ray twice in the sample), the angle range satisfying the diffraction condition is several tenths of that in the first crystallization method.
To several hundredths. Therefore, according to the two-crystal method, it is possible to detect minute lattice defects and minute strains that cannot be detected by the one-crystal method.

Now, considering the X-ray topography apparatus of the Lang method, the present applicant has disclosed in Japanese Patent Application Laid-Open No. Hei 7-14096 that the sample is arranged horizontally, and the X-ray is advanced in the vertical direction and transmitted through the sample. A so-called vertical X-ray topography apparatus having a structure to make it possible has been proposed.

[0006]

However, in the above-mentioned conventional X-ray topography apparatus, a one-to-one geometric correspondence is given to the sample, and the sample is sent to the two-dimensional X-ray detecting means such as an X-ray dry plate from the sample. When recording the diffracted X-rays, the sample must be translated in a horizontal plane, so that it is difficult to attach ancillary equipment such as a high-temperature container to the sample.

However, recently, there is a demand for measuring the behavior of a single crystal sample or the like to be measured by X-ray topography under special conditions, for example, in a low-temperature atmosphere, a high-temperature atmosphere, or during the growth process of the single crystal sample. Is getting stronger. In the above-described conventional liquid crystal device, it is difficult to attach necessary auxiliary equipment to the sample, and thus, such a demand cannot be met.

The present invention has been made in view of the above problems, and provides an X-ray topography apparatus capable of performing X-ray topography measurement on a sample placed under special conditions. With the goal.

[0009]

(1) In order to achieve the above object, an X-ray topography apparatus according to the present invention comprises:
An X-ray source for emitting X-rays, sample support means for holding the sample stationary during measurement, two-dimensional X-ray detection means for detecting X-rays from the sample in a plane, and an output from the X-ray source. At least one entrance slit for restricting X-rays traveling toward the sample, an exit slit disposed between the sample and the two-dimensional X-ray detection means, the X-ray source and the entrance slit And a base that supports the emission side slit and the ω movement table and that can move in parallel with the sample, and the base passes through the sample during the parallel movement. The ω moving table is rotatable about the ω axis.

According to the X-ray topography apparatus having the above configuration, the X-ray source and the incident side slit are rotated relative to the sample by the movement of the ω moving table, so-called ω rotation. Can be set to a value.

During the measurement, each element of the X-ray source, the entrance side slit and the exit side slit moves in parallel with respect to the sample and the two-dimensional X-ray detecting means in accordance with the movement of the base. A diffraction X-ray image with a one-to-one geometric correspondence can be detected by the two-dimensional X-ray detection means.

In addition, since the sample is kept stationary during the measurement, appropriate auxiliary equipment, around or near the sample,
For example, even when a high-temperature container, a low-temperature container, a sample generation / growth container, and the like are provided, X-ray measurement can be performed on the sample without any trouble. It is needless to say that such an accessory device is provided with an X-ray passing window for passing X-rays that pass through or reflect the sample.

In the above configuration, the "two-dimensional X-ray detecting means" is an X-ray detecting means having a structure capable of receiving X-rays in a plane area and detecting X-rays at each point in the plane area. For example, X-ray dry plate, X-ray film, stimulable phosphor,
It can be constituted by a planar CCD (Charge Coupled Device) sensor or the like.

The above-mentioned X-ray dry plate is a flat X-ray plate formed by providing an emulsion mainly composed of silver halide on one or both surfaces of a base substrate which is relatively hard and has an appropriate area.
Line detection element. The above-mentioned X-ray film is a planar X-ray film formed by providing an emulsion containing silver halide as a main component on one or both surfaces of a plastic film, for example, a thin and flexible plastic film. Line detection element.

X-rays expose photographic emulsions as well as visible light. When X-rays enter the emulsion, silver halide is ionized to form development nuclei. When this is developed, the silver particles are released and the portion is blackened. By measuring the blackening point and the degree of blackening, a two-dimensional X-ray distribution can be detected.

The stimulable phosphor is an energy storage type radiation detector, and is a stimulable phosphor such as BaFB.
r: A film formed by applying microcrystals of Er ^{2+ on} the surface of a flexible film, a flat film, or another member by coating or the like. This stimulable phosphor is an object having the property of being able to accumulate energy in the form of X-rays and the like and emitting the energy as light to the outside upon irradiation with stimulating light such as laser light.

That is, when the stimulable phosphor is irradiated with X-rays or the like, energy is accumulated as a latent image inside the stimulable phosphor corresponding to the irradiated portion, and the stimulable phosphor is further applied to the stimulable phosphor. When a stimulable phosphor such as a laser beam is irradiated, the latent image energy is emitted as light to the outside. By detecting the emitted light using a photoelectric tube or the like, the diffraction angle and intensity of X-rays that have contributed to the formation of a latent image can be measured. This stimulable phosphor has sensitivity 10 to 60 times that of a conventional X-ray film, and has a wide dynamic range of 10 ⁵ to 10 ⁶ .

The above-mentioned planar CCD sensor is an X-ray detecting element formed by arranging a CCD, which is a well-known electronic element, that is, a charge-coupled device in a plane. CCD
For example, a planar CCD sensor having an electrode array having a structure in which a plurality of electrodes are arranged on a silicon substrate with an oxide insulating film interposed therebetween, and the electrode array is arranged in a plane corresponding to the X-ray intake port. It is.

(2) In the X-ray topography apparatus having the above configuration, the X-ray source may be a point-shaped X-ray source. Thereby, the X-ray topography and the rocking curve can be accurately measured.

(3) In the X-ray topography apparatus having the above-mentioned configuration, the two-dimensional X-ray detecting means can be arranged at a position for receiving X-rays transmitted through the sample. This structure is a structure of an X-ray topography apparatus in a so-called transmission arrangement.

(4) In the X-ray topography apparatus having the above-mentioned structure, the ω-moving stage supporting the X-ray source and the incident side slit may be arranged at a position below a sample supported by the sample supporting means. it can. For an X-ray source, its weight can be quite large. If the ω moving table supporting the X-ray source is arranged below the sample as in the above configuration, even if the weight of the X-ray source becomes extremely large, the mechanism for supporting the X-ray source is relatively simple. Can be configured.

(5) In the X-ray topography apparatus according to any one of (1) to (3), the ω moving table that supports the X-ray source and the incident side slit is located above the sample supported by the sample supporting means. It can also be located at a location.

In an X-ray topography apparatus, it is required to extract a diffracted X-ray having a desired diffraction angle from a crystal or a sample. Therefore, regarding an incident side slit for limiting the X-ray incident on the crystal or the sample, an X-ray is required. The distance from the source to its entrance slit may have to be set quite long. In this case, if the ω carriage supporting the X-ray source is disposed below the sample as in (4), the length of the ω carriage becomes too long, and the arrangement position of the sample becomes extremely high. In addition, there is a problem that a hole for accommodating the ω moving table must be dug in the ground when the position of the sample is to be kept low. In contrast, the above (5)
If the ω carriage is placed above the sample as described,
No matter how long the distance from the X-ray source to the entrance slit is, the position of the sample can be kept low.

(6) In the X-ray topography apparatus having the above configuration, an auxiliary device can be provided near the sample. Here, the auxiliary device is a device capable of exerting some action on the sample. As the incidental device, for example, a container that can place a sample under some conditions other than the atmospheric atmosphere is considered. As such a container, for example, a high-temperature container that places a sample under high-temperature conditions, Various types of containers such as a low-temperature container placed under the conditions and a crystal growth furnace for generating and growing a single crystal sample or the like can be considered.

In the X-ray topography apparatus according to the present invention,
Since the sample is kept stationary during the measurement, the X-ray measurement can be performed on the sample without hindrance even if the above-described auxiliary device is provided around or near the sample.

(7) In the X-ray topography apparatus having the above-mentioned structure, the ω moving table may include a channel cut monochromator, and the channel cut monochromator may further include an X-ray path from the X-ray source to the sample. Can be movably provided between an operation position for blocking the X-ray and a retreat position for retreating from the X-ray passage.

A channel cut monochromator is formed by cutting a groove in a crystal block such as germanium or silicon to form walls on both sides of the groove, and reflecting X-rays on each of the walls to convert the X-rays into a single color. This is a monochromator having a structure to be converted.

According to the X-ray topography apparatus described in (7), the X-ray radiated from the X-ray source is made monochromatic, that is, the X-ray having only one specific wavelength is taken out of the sample. The light can be incident, and a so-called two-crystal method topography measurement can be performed. This makes it possible to detect minute lattice defects, minute distortions, and the like with respect to the sample.

(8) In the X-ray topography apparatus having the above structure, a 2θ movable table rotatable around a sample axis passing through the sample and a 0-dimensional X-ray detecting means supported by the 2θ movable table are provided. You can also. The "0-dimensional X-ray detecting means" referred to herein is an X-ray detecting means having a structure having no positional resolution, and is, for example, an SC (scint).
illation Counter: scintillation counter), PC
(Proportional Counter: proportional counter) or the like.

When a topography measurement is performed, diffracted X-rays generated from a sample are received by a two-dimensional X-ray detecting means such as an X-ray dry plate or a planar CCD camera. Does not contribute to the topography measurement. This zero-dimensional X-ray detection means is used at the time of an initial setting operation for setting various X-ray optical elements such as an X-ray source and a slit constituting the X-ray topography apparatus to a predetermined initial state, or Is used when a rocking curve is measured on a sample. Note that when performing the rocking curve measurement, X-ray detection by the two-dimensional X-ray detection unit is not performed.

The rocking curve measurement is mainly used as a measurement for evaluating the crystal integrity of a single crystal sample or the like, in which a single crystal sample is irradiated with X-rays and then diffracted by the sample. Diffracted X-rays or scattered X-rays for several tens to several hundreds of seconds near the X-ray intensity peak position
Intensity distribution for the line (ie rocking curve)
And evaluates the integrity and the like of the sample based on the rocking curve.

In the rocking curve measurement, usually, X-rays monochromatized by the first crystal (that is, taking out only X-rays of one specific kind of wavelength) are irradiated to a specific point of the sample. , And a rocking curve at one point is measured.

(9) In the X-ray topography apparatus described in (8) above, a planar CCD sensor is supported by the 2θ movable table in addition to the 0-dimensional X-ray detector, and the planar CD sensor is
The D sensor can be used as the two-dimensional X-ray detecting means. When an X-ray film is used as the two-dimensional X-ray detection means, after forming a diffracted X-ray image from the sample on the X-ray film, post-processing such as development processing must be performed.

On the other hand, when a planar CCD sensor is used as the two-dimensional X-ray detecting means, diffracted X-rays from the sample can be sequentially obtained as output signals of the planar CCD sensor, so that the operator is troublesome. This eliminates the need for post-processing, thereby enabling quick measurement.

Further, by providing both a zero-dimensional X-ray detecting means such as an SC and a planar CCD sensor as a two-dimensional X-ray detecting means on a 2θ movable stage, measurement using the two-dimensional X-ray detecting means and zero-dimensional X-ray detecting means can be performed. The measurement using the X-ray detection means can be freely switched and executed as desired by the operator.

[0036]

(First Embodiment) FIG. 1 shows one embodiment of an X-ray topography apparatus according to the present invention. This X-ray topography apparatus has respective components of a base 2, a 2θ movable base 3, and a sample support frame 4, each of which is supported by a machine frame 1.

Although the sample support frame 4 is schematically shown in FIG. 1, any structure can be used as long as the sample S can be detachably mounted and can be held stationary during the measurement. Is also good. Although the sample support frame 4 can directly support the sample S, in the present embodiment, the sample generation and growth furnace 8 as an auxiliary device is attached to the sample support frame 4.
The sample S is held in a stationary state by the sample production and growth furnace 8.

The sample generation and growth furnace 8 includes a sample, for example, SiC.
(Silicon carbide) A furnace for generating and further growing crystals, specifically, a heater for heating the inside to a high temperature, a vacuum exhaust system for evacuating the inside, and an inert inside. This is a furnace equipped with a gas transfer system for introducing gas. Each of the X-ray incident side and the diffracted X-ray emission side of the sample generation and growth furnace 8 is made of a material that can allow X-rays to pass therethrough and can isolate the internal atmosphere from the external atmosphere, such as beryllium. An X-ray passage window 6 is provided.

The sample S is provided with a φ rotation / tilt moving device 20. The φ rotation / tilt moving device 20 includes a φ axis Xφ extending in a direction perpendicular to the sample axis X0 passing through the sample in a direction perpendicular to the paper (that is, in a direction parallel to the paper).
, The sample S can be rotated, that is, rotated in a plane, and the sample S can be tilted, that is, tilted about the sample axis X0. These in-plane rotation and tilt movement with respect to the sample S are not performed during the measurement for obtaining the X-ray topography, but are performed during the initial setting for setting the sample S to the optimum measurement conditions. Is what is done.

The φ rotation / tilt moving device 20 has a structure in which, for example, a pulse motor is used as a power source and the power is transmitted to the sample S via an appropriate power transmission system.
The φ rotation / tilt moving device 20 can be installed between the sample generation and growth furnace 8 and the sample S to directly drive the sample S, or the sample support frame 4 and the sample generation and growth furnace 8, the sample S can be driven through the sample production and growth furnace 8.

A support member 14 is provided on the 2θ movable base 3, and the film support frame 15 is supported by the support member 14. A rotation support portion 29 is interposed between the support member 14 and the film support frame 15, and the rotation of the rotation support portion 29 causes the film support frame 15 to tilt and move as shown by the arrow D to adjust the angle. Can be held stationary in a later position.

An X-ray film 7a as two-dimensional X-ray detection means is detachably mounted on the film support frame 15.
The X-ray film 7a is a film that receives a diffracted X-ray emitted from the sample S in a plane region and forms an image.

On the surface of the 2.theta. Moving table 3, a two-dimensional CCD sensor 7b as two-dimensional X-ray detecting means and a SC (Scintillation Counter) 16 as zero-dimensional X-ray detecting means are provided.
Two X-ray detectors are fixedly installed. These detectors are
An axis passing through the sample S in a direction perpendicular to the paper surface, that is, the sample axis X
It is disposed at a predetermined angle α centered on 0. Reference numeral 28 denotes a light receiving slit disposed in front of the X-ray receiving surface of the SC 16.

The 2θ moving table 3 is provided with a 2θ moving device 13 which is driven by the 2θ moving device 13 to move the 2θ moving table 3 at a predetermined angle about the sample axis X0 as shown by an arrow BB '. You can rotate and move within the range. The 2θ moving device 13 has a structure in which, for example, a pulse motor is used as a power source and the power is transmitted to the 2θ moving base 3 via an appropriate power transmission system. The 2θ moving device 13 is disposed so as to mechanically connect the machine frame 1 and the 2θ moving base 3, for example.

A base moving device 12 is attached to the base 2,
The base 2 is driven by the base moving device 12 and relatively parallel moves with respect to the sample S, the film support frame 15 and the CCD sensor 7b as shown by arrows AA '. The base moving device 12 can be constituted by a driving device having an arbitrary structure as long as the base 2 can be moved in parallel. For example, a pulse motor is used as a driving source and its power is transmitted to the base 2 via an appropriate power transmission system. It can be configured by the structure of transmission. The base moving device 12 is provided so as to mechanically connect the machine frame 1 and the base 2, for example.

In FIG. 1, the base 2 is provided with an emission-side slit 9 and a ω-movement table 11. Exit slit 9
Has a groove-shaped space through which X-rays pass, that is, a slit 9a, and a slit position / width adjusting device 19 is attached to the emission side slit 9. The slit position / width adjusting device 19 adjusts the width of the slit 9a to narrow or widen, and further adjusts the entire position of the exit side slit 19 in the horizontal direction parallel to the film support frame 15 and the CCD sensor 7b. Adjust. The slit position / width adjusting device 19 can be configured by any structure as long as the above-described operation can be achieved, and is disposed on the base 2, for example.

The ω moving table 11 has an arrow CC ′ around an ω axis Xω set on the base 2 in a direction perpendicular to the paper surface.
Is supported by the base 2 so as to be rotatable in the direction of. ω
The axis Xω moves in the horizontal direction in FIG. 1 in accordance with the parallel movement of the base 2 in the direction of arrows AA ′.
5 shows a state where the ω axis Xω coincides with the sample axis X0.

The ω moving table 11 has an X-ray source F that emits X-rays, a pair of entrance-side slits 22 a and 22 b that regulate the divergence of the X-rays emitted from the X-ray source F, and a monochromator unit 23. Various X-ray optical elements such as are provided. The monochromator unit 23 is disposed on the surface of the monochromic base 18 together with one of the incident side slits 22b, and a monochromator slit 22c is disposed on the surface of the monochromic base 18 in addition to these elements.
The monochromator slit 22c regulates the X-ray emitted from the X-ray source F so as to be incident on the monochromator 23.

The X-ray source F is constituted by, for example, a point-shaped X-ray source. In addition, the pair of incidence-side slits 22a and 22b regulate the incident angle of the X-ray incident on the sample S to an extremely narrow angle range, and as a result, diffracted X-rays of a specific wavelength that are separated with high precision. It has a role of taking out from the sample S, and therefore, the distance L between the slits is relatively long, for example, about 1 to 2 meters. In some cases, only one incident side slit 22b on the side close to the sample S is provided, and the other incident side slit 22a may be omitted.

The monochromator 23 has a channel cut monochromator 24, for example, as shown in FIG. This channel cut monochromator 24 has a structure in which walls are formed on both sides of a groove by cutting a groove, that is, a channel, in a crystal block such as germanium or silicon, and X-rays are reflected on each of the walls 26. Meter. In this channel cut monochromator 23, the incident X-ray R0 is diffracted twice by the wall 26 to be monochromatic, and the output X-ray R1 having a specific wavelength is obtained.
To form

Returning to FIG. 1, the monochrome substrate 18 has a retracted position Pt retracted from the X-ray path R2 as shown by a solid line.
And the action position Ps that blocks the X-ray passage as shown by the dashed line. A monochrome switching device 25 is attached to the monochrome base 18, and the monochrome switching device 25 drives the monochrome base 18 to move it between the retracted position Pt and the operation position Ps. The monochrome base 18
Is not limited to being automatically performed using the monochrome switching device 25, but can also be performed manually.

An ω moving device 21 is attached to the ω moving table 11, and is driven by the ω moving device 21 to
1 can rotate around a ω axis Xω in a predetermined angle range as shown by an arrow CC ′. By this rotational movement, as shown in FIG. 4, the incident angle ω of the X-rays coming out of the X-ray source F and entering the sample S can be changed. Note that FIG. 4 shows a state in which the ω axis Xω and the sample axis X0 passing through the sample S are coincident with each other, so that the ω moving table 11 consequently rotates around the sample axis X0. Have been.

In FIG. 1, the output terminals of the planar CCD sensor 7b and SC16 are connected to an X-ray intensity calculation circuit 31. The X-ray intensity calculation circuit 31 calculates the X-ray intensity based on the X-ray count signal output from the CCD sensor 7b and SC16, and outputs a signal corresponding to the intensity. In particular, when an output signal is generated in the planar CCD sensor 7b, the X-ray intensity calculation circuit 31 also outputs a position signal corresponding to the X-ray receiving position in the light receiving surface.

FIG. 2 shows an embodiment of a control device used in the X-ray topography apparatus of the present embodiment. The control device 33 shown here has a CPU (Central Processing).
Unit) 34, a memory 36 attached thereto, and an input / output interface 37. The memory 36 is a ROM
(Read Only Memory), RAM (Random Access Memor)
y), a concept including an external storage medium such as a hard disk, and other various storage media.

The input / output interface 3 of the control device 33
7 has a CRT (Cathode Ray Tube) display 38
And an image forming apparatus such as a printer 39 are connected. Further, the following elements shown in FIG. 1, that is, the X-ray intensity calculation circuit 31 and the 2θ moving device 1
3, each element of the slit position / width adjusting device 19, the φ rotation / tilt moving device 20, the monochrome switching device 25, the ω moving device 21, and the base moving device 12, as shown in FIG. Connected to CPU34.

The X-ray topography apparatus having the above configuration can perform at least two types of measurements, that is, topography measurement and rocking curve measurement. Hereinafter, each of them will be described.

(Topography Measurement) There are two types of topography measurement: a case where an X-ray film 7a is used as a two-dimensional X-ray detecting means and a case where a planar CCD sensor 7b is used in FIG. A description will be given of a case where the measurement is performed by using.

In this topography measurement, X-rays generated from the X-ray source F are made incident on the sample S, and the X-ray diffracted by the sample S causes the X-ray film 7a to have a one-to-one geometric relationship with the sample S. An image is formed with a proper correspondence. Also,
In the X-ray topography apparatus according to the present embodiment, the topography measurement is performed on the sample S while generating and growing the crystal sample S of SiC by the sample generation and growth furnace 8.

At the time of this topography measurement, first,
X-ray source F, incident side slits 22a and 22b, sample axis X0 passing through sample S, ω axis Xω passing through base 2, output side slit 9, film support frame 1 supporting X-ray film 7a
The optical axis is adjusted so that various X-ray optical elements such as 5 are accurately placed on the X-ray optical axis. At the time of the optical axis adjustment, the X-rays generated from the X-ray source F using the SC 16 while rotating the 2θ-movement table 3 by 2θ by the 2θ-movement device 13 as necessary.
Detect lines.

After the optical axis adjustment, the sample production and growth furnace 8 is operated to produce and grow the sample S. When the timing for performing the topography measurement on the sample S comes, the X-ray film 7 a is mounted on the film support frame 15. Further, the ω moving table 11 is rotated around the ω axis Xω to adjust the X-ray incident angle ω with respect to the sample S, as shown in FIG. The X-ray incident angle ω is set to a value that satisfies the diffraction condition, that is, the so-called Bragg diffraction condition. Further, if necessary, SC16 is set to a diffraction angle 2θ0 corresponding to the crystal structure of sample S, and X-rays generated from X-ray source F and diffracted by sample S are detected.

Next, at a predetermined position of the film support frame 15, X
The base film 2 is moved to the initial position with respect to the X-ray film 7a by mounting the line film 7a and further operating the base moving device 12. At this time, in the normal case, the sample axis X0 and ω
The position with respect to the axis Xω is shifted. afterwards,
Arrow A- moves the base 2 at a constant speed by the base moving device 12.
X-rays are emitted from the X-ray source F while being sent and moved in the direction A '. The emitted X-rays pass through a pair of entrance side slits 22.
Due to the functions of a and 22b, the light enters the sample S at an incident angle regulated within a narrow angle range near the incident angle ω.

Since the incident angle ω of the X-ray to the sample S is set in advance so as to satisfy the diffraction condition, the sample S
Is normal, the X-rays incident on the sample S are diffracted by the sample S. This diffracted X-ray passes through the exit-side slit 9 and passes through the X-ray film 7 a in the film support frame 15.
And an image corresponding to the width and length of the slit 9a of the emission side slit 9 is formed on the X-ray film 7a.

Since the incident point of the X-rays incident on the sample S, that is, the ω axis line Xω moves in the horizontal direction along with the movement of the base 2 in the direction of the arrow AA ′, the sample is placed on the X-ray film 7a. The diffraction X-ray image from the entire surface of S is
Is formed by the geometric relationship of Then, X-ray film 7
By removing a from the film support frame 15 and performing a predetermined developing process, an X-ray topography relating to the sample S is obtained on the X-ray film 7a. According to the X-ray topography, the degree of satisfying the diffraction condition is changed by a partial shift of the crystal orientation, and the black-and-white contrast corresponding to the lattice defect in the sample S is reduced by X due to diffraction effects such as an extinction effect and a Borman effect. Observed on line film 7a.

Prior to exposing the X-ray film 7a with diffracted X-rays from the sample S, as shown in FIG. The X-ray film 7a may be set parallel to the sample S by rotating the X-ray film 15 by an appropriate angle manually or automatically about the rotation support section 29 as indicated by an arrow D.

(Topography Measurement Using Planar CCD Sensor) The above description is for the case where the X-ray film 7a is used as the two-dimensional X-ray detecting means. The sensor 7b can also be used. In this case, after detecting the diffraction angle 2θ0 with respect to the sample S in FIG. 4 by SC16, the 2θ moving device 13 is operated in FIG. 6 to move the 2θ moving table 3 to an appropriate angle around the sample axis X0, specifically, Rotates the X-ray receiving surface of the CCD sensor 7b on the X-ray optical path by rotating the detector 16 by an angle α between the detectors between the SC 16 and the CCD sensor 7b.

Then, the base 2 is moved by the base moving device 12.
While moving in the direction of the arrow AA 'at a constant speed,
The X-ray source F emits X-rays. The emitted X-rays enter the sample S at an incident angle regulated within a narrow angle range near the incident angle ω by the function of the pair of incident-side slits 22a and 22b.

Since the incident angle ω of the X-rays with respect to the sample S is set in advance so as to satisfy the diffraction condition,
Is normal, the X-rays incident on the sample S are diffracted by the sample S. The diffracted X-rays pass through the exit slit 9 to expose the light receiving surface of the CCD sensor 7b, and an image corresponding to the width and length of the slit 9a of the exit slit 9 is received by the light receiving surface.

The point of incidence of the X-rays incident on the sample S, that is, the ω axis line Xω scans in the horizontal direction along with the movement of the base 2 in the direction of the arrows AA ′, so that the light is incident on the light receiving surface of the CCD sensor 7b. A diffraction X-ray image from the entire surface of the sample S is formed in a one-to-one geometric relationship with the sample S. CCD sensor 7
b outputs an X-ray count signal for each coordinate point on the X-ray receiving surface, and based on the output signal, an X-ray intensity calculation circuit 3
1 calculates the diffraction X-ray intensity distribution in the plane of the sample S.

The result of this operation is shown in the display 38 of FIG.
The image is displayed as an image as an X-ray topography, or printed as an X-ray topography on a printing material such as paper by the printer 39. With these X-ray topographies, the degree of satisfying the diffraction condition changes due to a partial shift of the crystal orientation, and the black-and-white contrast corresponding to the lattice defect in the sample S is caused by the diffraction effects such as the extinction effect and the Borman effect. To be observed.

(Rocking Curve Measurement) Rocking curve measurement is performed by diffracting X-rays or scattered X-rays in the vicinity of the intensity peak position of the X-ray diffracted by the sample when the X-ray is incident on the sample for several tens to several hundreds of seconds This is a measurement to evaluate the integrity of the sample by examining the strength of the sample.

In performing the rocking curve measurement, the monochrome base 18 is moved to the operating position P as shown in FIG.
Place on S. At this time, as shown in FIG. 3, between the incident X-rays R0 and the outgoing X-rays R1 for the channel cut monochromator 24, the traveling directions are the same, that is, parallel, but there is an optical path difference G. In FIG. 7, the base 2 is moved in parallel by the base moving device 12 in FIG.
Is adjusted so that the outgoing X-ray R1 from the sample goes to the sample axis X0 in FIG.

Next, as shown in FIG. 8, the X-ray incident angle ω with respect to the sample S was adjusted to a desired angle, and
Is adjusted to an X-ray diffraction angle 2θ0 specific to the sample S. Then, the X-ray source F emits point-like X-rays in a state where X-rays can freely pass through the portion without mounting the X-ray film on the film support member 15. Among the emitted X-rays, those that have passed through the first incident side slit 22a and the monochromator slit 22c of the pair of incident side slits 22a and 22b are incident on the channel cut monochromator 24 to be monochromatic, Only a specific wavelength component, for example, a Kα ray is extracted.

The extracted monochromatic X-rays enter the sample S, where they are diffracted or scattered, and the intensity of the diffracted or scattered X-rays is measured by the SC 16. At this time, the operation of the ω moving device 21 causes the ω moving table 11 to move the ω moving table 11 to an extremely small angle range around the ω axis Xω, for example,
Rotating intermittently every minute step angle, for example, every 0.5 seconds, over an angle range of 0 seconds to several 100 seconds,
Thereby, the X-ray incident angle ω with respect to the sample S is changed.

In the rocking curve measurement, the sample S
The change range of the X-ray incident angle ω with respect to is very narrow, and the capture angle of the SC is sufficiently wide in comparison with the change range.
SC16 can be held stationary.

As described above, when the X-ray source F or the like moves by ω,
The intensity information of the diffracted X-ray or the scattered X-ray from the sample S at each ω angle position is obtained by the SC 16, and as a result, a so-called rocking curve as shown in FIG. 9 is obtained. Each incident X appearing in this rocking curve
Based on the X-ray intensity information with respect to the line angle position, the integrity, composition, and the like of the crystal of the sample S are evaluated.

The above rocking curve is for a specific point of the sample S. In rocking curve measurement, such a measurement result at one specific point may be sufficient, or measurement at several points must be performed, that is, mapping measurement must be performed. There is also.

When such a mapping measurement is performed, in FIG. 8, after a rocking curve measurement is performed on one point of the sample S, the X-ray incidence optical system including the X-ray source F and the X-ray including the SC16 and the like are measured. The X-ray receiving system is moved integrally and relatively to the sample S, and the X-ray incident position on the sample S and the expected X-ray position of the SC 16 are carried to different points of the sample S, and the new position is obtained. Perform rocking curve measurements on points.

When such a mapping measurement is performed, the base 2 and the SC 16 are not limited to being translated in a direction parallel to the plane of the paper, but are preferably translated in a direction perpendicular to the plane, that is, in a direction perpendicular to the plane of the paper. .

(Other Embodiments) The present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and various modifications may be made within the scope of the invention described in the claims. Can be modified.

For example, in the apparatus shown in FIG.
The X-ray incident optical system associated therewith is disposed below the sample S, and the X-ray receiving optical system such as the CCD sensor 7b is disposed above the sample S, but these positional relationships are reversed. That is, the X-ray source F and the like are disposed at the upper position, and C
An X-ray receiving optical system such as the CD sensor 7b may be provided at a lower position.

The sample production and growth furnace 8 as an accessory provided near the sample includes a high-temperature vessel, a low-temperature vessel,
It can be replaced with various devices according to measurement requirements.

In the apparatus shown in FIG. 1, the X-ray source F and the first
The entrance-side slit 22a was placed on the ω moving table 11 and rotated, but when the distance L between the slits is long, the X-ray source F
In addition, even if the first incident side slit 22a is linearly moved in the direction of the arrow AA 'in place of the rotational movement, the X-ray incident angle ω can be moved with respect to the sample S at an approximately constant angular velocity. There is no problem on the top.

In the description of FIG. 1 and the like, it is supposed that the reflection at the crystal sample is performed based on the symmetric reflection in the normal topography measurement as shown in FIG. However, when SiC is used as a crystal sample or the like, there is no symmetry plane with good conditions.
It is also conceivable to use an asymmetric surface as shown in FIG.
In such a case, it is necessary to determine the setting of each optical system element from the X-ray source to the X-ray detecting means in consideration of such asymmetric reflection.

[0084]

According to the X-ray topography apparatus of the present invention, the X-ray source and the incident side slit are rotated by the movement of the ω moving table with respect to the sample held stationary during the measurement.
Because of the so-called ω rotation, the incident angle of the X-rays on the sample can be set to a desired value.

Further, since the X-ray source, the entrance slit, and the exit slit move in parallel with respect to the sample and the two-dimensional X-ray detecting means by the movement of the base, a one-to-one geometric correspondence with the sample. Can be formed on the two-dimensional X-ray detection means.

Further, since the sample is kept stationary during the measurement, appropriate auxiliary equipment,
For example, even when a high-temperature container, a low-temperature container, a sample generation / growth container, and the like are provided, the X-ray measurement can be performed on the sample without any trouble.

[Brief description of the drawings]

FIG. 1 is a front view showing an embodiment of an X-ray topography apparatus according to the present invention.

FIG. 2 is a block diagram showing one embodiment of an electric control system used in the apparatus of FIG.

FIG. 3 is a front view showing an example of a monochromator used in the apparatus of FIG.

FIG. 4 is a front view showing an example of a use form of the apparatus of FIG. 1;

FIG. 5 is a front view showing a main part of another example of a use form of the apparatus of FIG. 1;

FIG. 6 is a front view showing still another example of the usage mode of the device of FIG. 1;

FIG. 7 is a front view showing still another example of a usage form of the device of FIG. 1;

FIG. 8 is a front view showing still another example of a usage form of the device of FIG. 1;

FIG. 9 is a graph showing an example of a result of an X-ray measurement performed using the apparatus of FIG.

FIG. 10 is a diagram schematically showing the type of an X-ray reflection surface of a crystal sample.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 Machine frame 2 Base 3 2θ moving stand 4 Sample support frame (sample support means) 7a X-ray film (two-dimensional X-ray detection means) 7b Planar CCD sensor (two-dimensional X-ray detection means) 8 Sample generation and growth furnace (Auxiliary equipment) 9 Emission-side slit 11 ω moving table 14 Film support member 15 Film support frame 16 SC (0-dimensional X-ray detection means) 18 Monochrome base 22a, 22b Incident-side slit 23 Monochromator unit 24 Channel cut monochromator 26 Wall 29 Rotation support part F X-ray source G Optical path difference L Distance between slits Pt Retreat position Ps Working position R0, R1, R2 X-ray path S Sample X0 Sample axis Xω ω axis Xφ φ axis α Distance between detectors ω X-ray incidence angle

 ────────────────────────────────────────────────── ─── Continued on the front page F term (reference) 2G001 AA01 BA11 BA26 CA01 DA01 DA02 DA06 DA09 EA09 FA06 GA13 HA12 HA13 JA01 JA05 JA06 JA11 JA20 KA01 KA03 KA20 LA11 RA03 SA10 SA29

Claims (9)

[Claims] 1. An X-ray source for emitting X-rays, a sample supporting means for holding a sample stationary during a measurement, and a two-dimensional X-ray capable of detecting X-rays from the sample in a plane area
X-ray detection means, at least one entrance slit for restricting X-rays emitted from the X-ray source toward the sample, and an emission slit disposed between the sample and the two-dimensional X-ray detection means And a base that supports the X-ray source and the entrance slit, and a base that supports the emission slit and the base and that can move parallel to the sample. Is the ω that passes through the sample during the translation.
An X-ray topography apparatus, comprising an axis, wherein the ω-movement stage is rotatable about the ω-axis. 2. The X-ray topography apparatus according to claim 1, wherein the X-ray source is a point-shaped X-ray source. 3. The method according to claim 1, wherein
An X-ray topography apparatus, wherein the dimensional X-ray detection means is arranged at a position for receiving X-rays transmitted through the sample. 4. The apparatus according to claim 1, wherein the ω moving table supporting the X-ray source and the incident side slit is positioned below a sample supported by the sample supporting means. X characterized by being arranged
Line topography equipment. 5. The apparatus according to claim 1, wherein the ω moving table supporting the X-ray source and the incident side slit is located above a sample supported by the sample supporting means. X characterized by being arranged
Line topography equipment. 6. The X-ray topography apparatus according to claim 1, further comprising an auxiliary device provided near the sample. 7. The apparatus according to claim 1, wherein the ω moving table includes a channel cut monochromator, and the channel cut monochromator is an X-ray path from the X-ray source to the sample. An X-ray topography apparatus capable of being moved between an operation position for blocking an X-ray and a retreat position for retreating from the X-ray passage. 8. The at least one of claims 1 to 7, wherein the 2θ movable table is rotatable about a sample axis passing through the sample, and 0-dimensional X-ray detection is supported by the 2θ movable table. X-ray topography apparatus comprising: 9. An X-ray topography apparatus according to claim 8, wherein said two-dimensional X-ray detection means is a planar CCD sensor supported by said 2θ movable table.