JPH0714871Y2 - Thin sample holder for X-ray diffraction with restricted field stop - Google Patents

Description

[Detailed Description of the Invention] [Industrial field of application] The present invention adheres an X-ray limited irradiation field diaphragm under a microscope to a thin piece or a thin film fixed (hereinafter abbreviated as thin piece) surface at an arbitrary measurement position. The present invention relates to a thin-piece sample holder device for X-ray diffraction with a limited irradiation field diaphragm, which is capable of irradiating and diffracting X-rays on a thin piece substance which is fixed and is inside the diaphragm by an X-ray diffraction device.

[Prior Art] In X-ray diffraction, in conventional X-ray irradiation of a sample,
Usually, a metal cylindrical collimator or the like is used. In this method, a sample portion to be measured is aligned with the optical axis of the collimator, and X-rays are irradiated and diffracted. The area to be irradiated on the sample is determined by the size of the radiation source, the inner diameter and length of the cometer, and the length from the collimator tip to the sample position. This method is effective when the sample is completely bathed in X-rays like the single crystal method, but for a specific sample existing in a plane such as a thin piece, the smaller the measurement area becomes. Aligning the optical axis with the collimator is extremely difficult. Even if the microscope is installed in the X-ray diffractometer,
At high magnification, the working distance of the microscope (distance between the objective lens and the sample position) becomes short, and it is difficult to mount it in an actual device. In the case of vibrating and diffracting a substance, the accuracy of mechanical crossing of the vibration axis becomes a problem, and it is not possible to confirm whether the target position in the slice is actually irradiated with X-rays.

[Problems to be solved by the invention] The technical problem of the present invention is to perform measurement and positioning of a sample under a microscope independently of a diffractometer, and to determine the measurement position and area of the sample confirmed under the microscope with a limited X-ray irradiation field. Select and fix with iris X
It is to provide a sample holder device capable of irradiating and diffracting a line.

[Means for Solving the Problems] The sample holder device of the present invention for solving the above problems is
Equipped with a frame-shaped sample holder for X-ray diffraction that holds and fixes thin or thin film solid samples on the stage of a microscope. The X-ray limiting irradiation field diaphragm is moved to an arbitrary measurement position on the sample surface and attached so as to be in close contact with the diaphragm moving arm provided on the X-ray diffractometer. This enables X-ray diffraction.

[Operation] To use the sample holder device of the present invention, first, the thin sample is mounted on the sample holder and fixed, and in this state, the thin sample is observed with a microscope to determine the region to be measured. Next, by moving the diaphragm moving arm having the X-ray restricted irradiation field diaphragm at its tip, the diaphragm of the arm is fixed according to the position to be measured. If the diaphragm of the arm is closely fixed to the thin sample in this manner, only the substance exposed in the diaphragm can be irradiated and diffracted by X-rays.

Therefore, the measurement positioning of the sample is performed under the microscope independently of the diffractometer, and the measurement position and area of the sample confirmed under the microscope are selectively fixed by the X-ray limiting irradiation field diaphragm to irradiate the X-ray.
Can diffract.

[Advantages of the Invention] According to the sample holder device of the present invention as described above, the following two advantages can be obtained.

For one, the measurement positioning of the sample can be done under the microscope independently of the diffractometer. In this case, it is possible to confirm the sample position and the region while observing under the mirror, and move the diaphragm to the optimum measurement position according to it, and closely fix it. Second, when vibrating the thin piece on the X-ray diffractometer, the diaphragm is fixed on the thin piece, so if you use a collimator that is a little large to allow the deviation of vibration, only the substance inside the diaphragm will be However, the bath will always be completely exposed to X-rays, and diffraction will be obtained only in the region to be accurately measured. That is, compared with the conventional method, even if the optical axis alignment of the substance to be measured and the collimator and the fine adjustment of the vibration axis and the optical axis are not strictly performed, the collimator that completely bathes the diaphragm hole should be selected for measurement. There is a guarantee that the diffraction information of the material will be obtained.

[Embodiment] An embodiment of the thin sample holder device of the present invention will be described below with reference to the drawings.

In FIGS. 1 and 2, reference numeral 1 denotes a sample holder for X-ray diffraction, which is formed into a frame shape for holding and fixing a thin sample a so that it can be placed on a stage of a microscope, and an X-axis is attached to the tip of the sample holder 1. A diaphragm moving arm 2 having a line-limited irradiation field diaphragm 3 can be fixed by a screw 4. The X-ray limiting irradiation field diaphragm 3 is formed by providing a small-diameter hole in the X-ray shielding plate, and is preferably made of a metal such as lead or platinum that shields X-rays well. As shown, one X
It is possible to prepare several diaphragms with different diameters on the line shield. When the thin sample a is vibrated, the thickness of the shield plate is
It is better to make it as thin as possible so that the edge of the diaphragm cannot be shaded inside, but a thickness that can shield 90% or more of the X-rays used is desirable.

The diaphragm moving arm 2 is preferably made of a highly elastic material such as stainless steel. In this diaphragm moving arm 2, the X-ray restricted irradiation field diaphragm 3 is made to face the X-ray restricted irradiation field diaphragm 3 by facing the X-ray restricted irradiation field diaphragm 3 to the hole 5 provided at one end and inserting the screw 4 into the elongated hole 6 provided over substantially the entire length. The thin sample a is moved to an arbitrary measurement position and attached so as to be closely fixed. If the tightening position of the screw 4 is the inclined surface 7 of the peripheral portion of the sample holder 1 as shown in the figure, the X-ray limiting irradiation field diaphragm 3 is moved by the diaphragm moving arm 2.
Due to the elasticity of, it can be closely fixed to the thin sample a.

In the figure, 8 is a thin sample holder, and 9 is a cylindrical rod such as brass for fixing to a goniometer head for an X-ray diffractometer or an X-ray diffraction camera.

Next, a method of using the sample holder device will be described.

First, a thin piece sample a is prepared so as to fit the inner frame of the sample holder 1, and the shaped thin sample a is held in the inner frame of the sample holder 1 with the surface to be observed facing up,
Fix with.

In this state, the sample holder 1 is horizontally placed on the stage of the microscope for observation. When the position to be measured under the mirror is determined, the sample holder 1 is fixed by aligning it with the center of the microscope visual field. Next, after selecting the size of the diaphragm that fits the measurement area, the center of the selected diaphragm 3 is aligned with the center of the visual field by the diaphragm moving arm 2 and the diaphragm moving arm 2 is screwed.
Fix with. The diaphragm 3 is in contact with the surface of the thin sample a,
When the screw 4 is loosened, it can be moved while sliding on the surface of the thin sample. If the screw 4 is formed so as to be fixed to the inclined surface 7, when the diaphragm moving arm 2 is fixed by the screw 4, the diaphragm 3 can be closely fixed to the thin sample a by the elasticity of the diaphragm moving arm 2.

The movement of the diaphragm 3 by the diaphragm moving arm 2 can be freely performed by manually moving a portion of the arm 2 opposite to the diaphragm 3 by rotating around the screw 4 and moving along the long hole 6. With this method, the diaphragm 3 can be fixed with an accuracy of about 10 μm, but in the case of more precise adjustment, fine adjustment is possible.
The XY moving mechanism may be attached to the diaphragm moving arm 2.

The holder device in which the diaphragm 3 is closely fixed on the thin sample a as described above is fixed by inserting the cylindrical rod 9 into the cylindrical groove at the top of the goniometer head for an X-ray diffractometer or an X-ray diffraction camera. To do. The centering of the sample on the rotation axis of the diffracting device can be easily performed even with a telescope of about 10 times attached to the device by using the hole of the diaphragm 3 as a mark. Also, since the diameter of the collimator is sufficiently larger than the aperture diameter,
The flake material in the diaphragm is completely exposed to X-rays. Therefore, strict optical axis alignment is not necessary.

When the thin sample a is vibrated, the area actually irradiated is determined by the diameter and thickness of the diaphragm and the vibration angle. The thinner the shielding plate of the squeeze 3 and the smaller the vibration angle, the smaller the irradiation blind region. In order to reduce the vibration angle, X-rays of shorter wavelength may be selected. If an energy dispersive detector is used, it is possible to collect diffraction lines efficiently without vibrating the thin sample a too much.

[Brief description of drawings]

FIG. 1 is a front view of a thin sample holder device showing an embodiment of the present invention, and FIG. 2 is a side view of the center of FIG. 1 ... Sample holder, 2 ... Aperture moving arm, 3 ...
Restricted irradiation field diaphragm, a ... Thin sample.

Claims (1)

[Scope of utility model registration request] 1. A sample holder for X-ray diffraction, which is frame-shaped to hold and fix a thin sample or thin-film solid sample and can be mounted on a stage of a microscope.
Limiting field of the line A stop moving arm equipped with a stop
The X-ray restricted irradiation field diaphragm was moved to an arbitrary measurement position on the sample surface and attached so as to be able to be closely fixed, and X-ray diffraction was enabled on the flaky material in the diaphragm on the X-ray diffractometer. A thin-piece sample holder device for X-ray diffraction with a limited irradiation field stop.