JPH0786484B2 - Goniometer head - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention is used in an X-ray diffractometer, and has an X-ray diffraction pattern in a predetermined crystal orientation.
The present invention relates to a goniometer head for adjusting the supporting orientation (mounting angle) of a crystal so that a line is incident.

[Prior Art] As methods for evaluating single crystals of various substances, there are methods utilizing X-ray diffraction phenomena, such as the Laue method, the precession method, and the Weisenberg method. These methods fix a single crystal so that X-rays are incident on a specific crystal orientation, irradiate the single crystal with X-rays, record a diffraction spot by the single crystal on a photographic film, and analyze the diffraction spot. Then, the single crystal is evaluated. In these methods, it is necessary to adjust the angle of the single crystal so that a specific orientation of the single crystal becomes a predetermined direction with respect to the X-ray irradiation direction. For this reason, a holder with a crystal attachment angle correction mechanism called a goniometer head is used in the X-ray diffractometer.

In order to fix the specific crystal orientation of the sample crystal in a predetermined direction with respect to the X-ray radiation direction, after mounting the sample crystal on this goniometer head, an X-ray diffraction photograph was taken and this photograph was analyzed. It is necessary to adjust the crystal mounting angle to a predetermined angle. By repeating this operation a plurality of times, the attachment angle of the single crystal can be adjusted to a predetermined angle so that the X-rays are incident in the predetermined crystal orientation direction.

FIG. 2 is a schematic diagram showing the positional relationship between the sample mounting angle and the incident X-ray.

The X-ray diffractometer has three-axis coordinate axes consisting of an X-axis, a Y-axis and a Z-axis which are orthogonal to each other. Then, the X-rays emitted from the X-ray generator provided in the X-ray diffractometer enter the sample crystal 10 from the direction shown by the arrow in the figure. This X-ray incident direction is always at a constant angle with respect to the X axis, the Y axis, and the Z axis.

The sample crystal 10 is fixed to the tip of the crystal attachment shaft 11 and attached to the goniometer head. In this case, the direction of the specific orientation of the sample crystal 10 does not match the predetermined X-ray incident direction.
Generally, an angular deviation in a specific azimuth direction in the direction of rotation about the X axis is an α angle, an angular deviation in a particular azimuth direction in a direction of rotation about the Y axis is a β angle, and a direction of rotation about the Z axis is a direction. The deviation of the angle in the specific azimuth direction at is called D angle.

FIG. 3 is a front view showing a conventional goniometer head. A β angle adjusting mechanism unit 13 is attached on the X / Y direction moving mechanism unit 12 of the goniometer head, and the X / Y direction moving mechanism unit 12 moves the β angle adjusting mechanism unit 13 in the X axis direction and the Y axis direction. Can be moved individually. The β angle adjusting mechanism section 13 is a fixed section 13 fixed on the X / Y direction moving mechanism section 12.
and a movable portion 13b having a lower curved surface that comes into surface contact with the upper curved surface of the fixed portion 13a. Moving part 1
3b can be slid along the curved surface of the fixed portion 13a by a driving device (not shown). As a result, the movable portion 13b can rotate about the horizontal axis.

On the β angle adjusting mechanism section 13, an α angle adjusting mechanism section 14 which is similarly constituted by a fixed section 14a and a movable section 14b is provided. This fixed portion 14a is a movable portion 13b of the β angle adjusting mechanism portion 13.
It is fixed on. The movable portion 14b can be slid along the curved surface of the fixed portion 14a by a driving device (not shown) with the direction orthogonal to the rotation axis of the movable portion 13b of the β angle adjusting mechanism 13 as the rotation axis. ing.

A crystal mounting plate 15 is provided on the movable portion 14b of the α angle adjusting mechanism portion 14.

The sample crystal is fixed to the crystal mounting portion 15. At this time, since the specific orientation direction of the crystal is an arbitrary direction, the α angle adjusting mechanism unit 14 and the β angle adjusting mechanism unit 13 adjust the α angle and the β angle, and the entire goniometer head is rotated around the vertical axis. Therefore, it is necessary to adjust the D angle. To do this, take an X-ray diffraction photograph of the crystal, analyze it,
It is necessary to repeat the work of adjusting the D angle, the α angle and the β angle little by little.

When analyzing an X-ray diffraction photograph, it is easy to determine the angle deviation from any one of the X-axis, Y-axis, and Z-axis coordinate axes even if the specific orientation direction of the sample crystal does not match. Is. However, it is extremely difficult to determine the angle deviation from two or more axes at the same time. Therefore, the method of adjusting the angle for each axis is the most efficient method. Generally, the D angle, which is movable in the widest range in the structure of the goniometer head, is adjusted first, and then α
Angle and β angle are adjusted.

[Problems to be Solved by the Invention] However, as described above, in the conventional goniometer head, the α-angle and β-angle adjusting mechanism parts 14 and 13 are arranged closer to the crystal than the D-angle adjusting mechanism part. When the D angle is adjusted, the rotating shafts of the movable parts 14b and 13b of the α angle and β angle adjusting mechanism parts 14 and 13 also move, and deviate from the X axis and the Y axis, respectively. In this state, trying to adjust only one of the α angle and β angle, the α angle adjusting mechanism unit 14 or the β angle adjusting mechanism unit
When 13 is driven, the crystal typeface rotates about the X axis and Y
Since the rotation about the axis is performed at the same time, both the α angle and the β angle change. Therefore, in the conventional goniometer head, it is necessary to perform adjustment while simultaneously moving both the α-angle adjusting mechanism unit 14 and the β-angle adjusting mechanism unit 13, and it is necessary to match the specific orientation direction of the crystal with the predetermined direction. It is extremely complicated.

The present invention has been made in view of such problems,
For rotations about the first, second and third directions,
It is an object of the present invention to provide a goniometer head that can be individually adjusted and that can easily adjust a specific azimuth direction of a sample crystal to a predetermined direction.

[Means for Solving the Problems] A goniometer head according to the present invention is a goniometer head for X-ray diffraction, which adjusts a supporting orientation of a crystal to make X-rays incident on a specific crystal orientation, and a crystal mounting for supporting the crystal. And a first adjusting mechanism part for rotating the crystal mounting part with the first direction passing through the crystal mounting part as a central axis.
This first adjustment mechanism part is arranged in a second direction orthogonal to the first direction.
A second adjusting mechanism portion that rotates about the direction of
It has a 3rd adjustment mechanism part which rotates this 2nd adjustment mechanism part on the 3rd direction orthogonal to the said 1st and 2nd direction as a central axis.

[Operation] In the present invention, first, the crystal mounting portion that supports the crystal is rotated about the first direction passing through the crystal mounting portion by the first adjusting mechanism portion. As a result, the angle (D angle) of the direction of rotation about the first direction is adjusted. Next, the second and third adjusting mechanism sections rotate the first and second adjusting mechanism sections, respectively, around the second and third directions orthogonal to the first direction. As a result, the angles (α angle, β angle) of the directions of rotation about the second and third directions are adjusted.

In the present invention, since the crystal attachment portion is directly attached to the first adjusting mechanism portion for rotating the crystal attachment portion about the first direction passing through the crystal attachment portion, the D angle should be adjusted. However, the α and β angles do not change. For this reason, it becomes easy to adjust the support orientation for making X-rays incident on a specific orientation of the crystal.

[Embodiment] Next, an embodiment of the present invention will be described with reference to the accompanying drawings.

1 (a) is a left side view showing an embodiment of the present invention, and FIG. 1 (b) is a front view thereof.

An X / Y-direction moving mechanism unit 2 is provided below the goniometer head according to the present invention, and a β-angle adjusting mechanism unit 3 is mounted on the X / Y-direction moving mechanism unit 2. The X / Y direction moving mechanism unit 2 allows the β angle adjusting mechanism unit 3 to move within a limited range in the X direction and the Y direction of the X-ray diffraction device.

The β angle adjusting mechanism section 3 is a fixed section having a concavely curved upper surface.
3a and a moving portion 3b having a convexly curved lower surface, and the fixed portion 3a and the moving portion 3b are arranged with their curved surfaces in surface contact. The movable portion 3b can be slid along the curved surface of the fixed portion 3a by a driving device (not shown). The goniometer head of the present embodiment is arranged in the X-ray diffractometer so that the central axis of this curved surface is parallel to the Y-axis of the X-ray diffractometer.

On the β angle adjusting mechanism section 3, like the β angle adjusting mechanism section 3,
An α-angle adjusting mechanism section 4 including a fixed section 4a and a movable section 4b is provided. This fixing part 4a is a β angle adjusting mechanism part 3
The movable part 4b is fixed on the movable part 3b, and the movable part 4b can be slid along the curved surface of the fixed part 4a by a driving device (not shown). And the central axis of this curved surface is X
It is parallel to the X axis of the line diffractometer.

A D angle adjusting mechanism 5 is arranged on the α angle adjusting mechanism 4. The D-angle adjusting mechanism 5 is composed of a disk-shaped fixed part 5a and a disk-shaped rotating part 5b which are coaxially arranged and are in surface contact with each other. The fixed portion 5a is the α angle adjusting mechanism portion 4
Is fixed on the movable part 4b of the
A drive device (not shown) can rotate about 5a on its center axis. The rotation axis of the rotating portion 5b is orthogonal to the central axis of the arc surface of the α angle adjusting mechanism portion 4. A crystal attachment portion 6 is arranged in the center of the rotating portion 5b.

Next, a description will be given of the operation of aligning the specific azimuth direction of the sample crystal with a predetermined direction by the goniometer head configured as described above and taking a desired X-ray diffraction photograph.

First, by fixing the crystal attachment shaft to the crystal attachment portion 6, the sample crystal fixed on the crystal attachment shaft is attached to the goniometer head. Next, the position of the sample crystal is adjusted so that the X-ray is properly irradiated to the sample crystal by appropriately driving the X / Y direction moving mechanism unit 2.

Next, the sample crystal is irradiated with X-rays and an X-ray diffraction photograph is taken. Then, this photograph is analyzed by a predetermined method to obtain the deviation angle of the D angle. Based on this result, the D angle adjusting mechanism section 5 is driven to rotate the sample crystal by a desired angle. Then, the X-ray diffraction photograph of the sample crystal is taken again. Repeat this work until the deviation of the D angle disappears.

Next, the X-ray diffraction photograph is analyzed to obtain the shift angle of the α angle.
Then, based on this result, the α-angle adjusting mechanism unit 4 is drive-controlled to rotate the sample crystal by a desired angle. afterwards,
An X-ray diffraction photograph of the sample crystal is taken and the shift angle of the α angle is obtained. This α-angle adjustment work is repeated until the α-angle shift is eliminated.

Then, the X-ray diffraction photograph is analyzed to determine the deviation angle of the β angle. Then, based on this result, the β-angle adjusting mechanism section 3 rotates the sample crystal by a desired angle. Then, similarly to the method of adjusting the D angle and the α angle described above, an X-ray diffraction photograph is taken, and this operation is repeated until the β angle shift is eliminated. In this way, it is possible to obtain a desired X-ray diffraction photograph with the specific orientation of the sample crystal as the predetermined direction.

Next, the result of actually manufacturing the goniometer head of this embodiment shown in FIGS. 1A and 1B and comparing its operability with the conventional goniometer head shown in FIG. 3 will be described.

A Cu single crystal was used as a sample crystal, and this single crystal was attached to the goniometer heads of Examples and Conventional Examples. And
The D angle, α angle, and β angle were adjusted so that the X-rays were vertically incident on any one of the (100), (110), and (111) crystal planes of this single crystal, and Cu was applied by the precession method. An X-ray diffraction photograph of the single crystal was taken. Then, the number of X-ray diffraction photographs required until the deviation angle between the specific azimuth direction of the crystal and the X-axis, Y-axis and Z-axis of the X-ray diffractometer was 0.1 ° or less was examined. This operation was repeated 10 times for each of the example and the conventional example, and the average number of required X-ray diffraction photographs was calculated. The results are shown in Table 1 below.

As is clear from Table 1, the goniometer head of this embodiment required almost the same number of X-ray diffraction photographs as the conventional example when adjusting the D angle. However, in comparison with the number of X-ray diffraction photographs required at the time of adjusting the α angle and β angle thereafter, the example is about 1/3 the number of the conventional example, and the number required for adjusting the D angle is Even when compared with the total number of photographs, the number of examples was about two-thirds less than that of the conventional example.

[Effects of the Invention] As described above, the goniometer head according to the present invention includes the first adjusting mechanism portion that rotates the crystal about the first direction passing through the crystal mounting portion as the central axis, and the first adjusting mechanism portion that is orthogonal to the first direction. A second adjusting mechanism part for rotating the first adjusting mechanism part with the second direction as a central axis, and a second adjusting mechanism part with a third direction orthogonal to the second direction as a central axis. And a third adjusting mechanism for rotating the X-ray diffraction device, so that the angle of a specific orientation of the crystal is individually adjusted with respect to the direction of rotation around the X-axis and the Y-axis of the X-ray diffractometer. You can Therefore, it becomes easy to analyze the X-ray diffraction photograph for adjusting the crystal attachment angle, and the number of times of taking the X-ray diffraction photograph for adjustment is significantly reduced. Therefore,
The single crystal analysis by X-ray diffraction is completed in an extremely short time.

[Brief description of drawings]

FIG. 1 (a) is a left side view showing an embodiment of the present invention, FIG. 1 (b) is a front view of the same, and FIG. 2 is a schematic view showing a positional relationship between a sample mounting angle and an incident X-ray. FIG. 3 is a front view showing a conventional goniometer head. 2,12; X / Y direction moving mechanism section, 3,13; β angle adjusting mechanism section, 3a,
4a, 5a, 13a, 14a; fixed part, 3b, 4b, 13b, 14b; movable part, 4, 14;
α-angle adjusting mechanism section, 5; D-angle adjusting mechanism section, 5b; Rotating section, 6, 15;
Crystal mounting part, 10; Sample crystal, 11; Crystal mounting axis

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Mamoru Aoyagi 1-5-1 Kiba, Koto-ku, Tokyo Fujikura Electric Wire Co., Ltd. (56) Reference JP-A-1-260353 (JP, A) JP A 61-153552 (JP, A) Actual public Sho 43-6240 (JP, Y1)

Claims (1)

[Claims] 1. A goniometer head for X-ray diffraction, which adjusts a supporting orientation of a crystal to make X-rays incident on a specific crystal orientation, and a crystal mounting portion for supporting the crystal and a first mounting portion passing through the crystal mounting portion. A first adjusting mechanism part for rotating the crystal attachment part about a direction as a central axis, and a second adjusting part for rotating the first adjusting mechanism part about a second direction orthogonal to the first direction as a central axis. A goniometer, comprising: a mechanical section; and a third adjusting mechanism section that rotates the second adjusting mechanism section about a third direction orthogonal to the first direction and the second direction as a central axis. head.