JP2003149174A - Sample holder for x-ray diffraction measurement and sample fixing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample holder and a sample fixing method which can both prevent powder sample from being oriented and fix the height of a measurement face to a fixed height in X-ray diffraction measurement. SOLUTION: The sample holder comprises a plate having a through-hole, an organic film attached to one face of the plate by fixing agent so as to close the through-hole and a collodion thin film adhering to the inner surface of the organic film so as to fix the powder sample. The sample fixing method attaches the organic film to one face having the through-hole by the fixing agent, and fix the collodion thin film adhering to the inner surface of the organic film to the powder sample.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a sample holder used for X-ray diffraction measurement of a powder sample and a sample fixing method.

[0002]

2. Description of the Related Art When a material is a powder, it is generally not oriented because individual crystal grains are randomly present.
The sample may be oriented by pressing or hardening the sample by applying force. When the sample is oriented, the diffraction peak due to the crystal is detected differently from the theoretical peak intensity ratio, so the evaluation method using the peak intensity (quantitative analysis,
The measurement error when performing the crystal structure analysis) becomes large.

[0003]

In order to avoid orientation due to sample fixation, it is effective to apply a thin layer of petroleum jelly etc. on the sample plate and sprinkle the sample powder on the sample plate. Since the heights of the measurement planes are different, it is not possible to accurately determine the diffraction peak position used when performing the crystal structure analysis.

Therefore, an object of the present invention is to provide a sample holder and a sample fixing method which can achieve both the non-orientation of a powder sample and the constant height of the measurement surface in X-ray diffraction measurement.

[0005]

In order to achieve the above-mentioned object, the present invention provides a plate having a through hole, and an organic film attached to one surface of the plate by an adhesive agent so as to close the through hole. And a collodion thin film adhered to the inner surface of the organic film so as to fix the powder sample.
A sample holder for line diffraction measurement is adopted.

Further, the plate having the through-hole has an X-ray irradiation area in the X-ray diffraction measurement which is within the through-hole, and the through-hole secures at least 5 mm square and the surface to which the organic film is attached. It is characterized by being a solid material having a smooth (sample measurement surface). The organic film has a thickness of 10 μm or less and has a larger area than the through holes of the plate. The collodion thin film can be attached by dropping a few drops of a solvent containing collodion on the plate-side surface of the organic film and drying after a few minutes.

A powder sample for X-ray diffraction measurement is fixed by spraying an appropriate amount before the solvent is completely dried. In the X-ray diffraction measurement using the sample holder by this sample preparation method, the X-rays generated from the X-ray source are irradiated from the outer surface of the organic film of the sample holder, and most of them are transmitted to the powder sample attached to the inner surface, The X-ray diffracted by the sample is again detected by the X-ray detector through the organic film.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The sample fixing method and sample holder of the present invention will be described below with reference to FIG. In FIG. 1, 1 is a plate having through holes, 2 is an organic film, 3 is a fixing agent, 6 is a solvent containing collodion, and 7 is a powder sample.

The sample holder 5 of the present invention is completed by sticking the organic film 2 using the adhesive 3 so as to close the through hole of the plate 1. At this time, it is important to prevent unevenness and wrinkles on the organic film 2. Here, in the X-ray diffraction measurement, X-rays are applied to the surface indicated by 4.

A few drops of the solvent 6 containing collodion are dropped on the inner surface of the organic film 2 from the side opposite to the through hole to which the organic film 2 is attached, and an appropriate amount of the powder sample 7 is sprayed before the solvent 6 dries. When the solvent 6 is completely dried, the powder sample 7 is fixed near the inner surface of the organic film 2, so that the height of the sample surface can be kept constant at the correct position every time.

Examples of the present invention and comparative examples will be described below. (Example) FIG. 2 shows an X-ray diffraction pattern of LiCoO ₂ powder fixed using the sample holder of the present invention. As is clear from FIG. 2, according to the present invention, an X-ray diffraction pattern in a non-oriented state can be obtained for the powder sample.

(Comparative Example) FIG. 3 shows an X-ray diffraction pattern of LiCoO ₂ powder fixed by the pressing method of the conventional example.
As is apparent from FIG. 3, in the pressing method, the selective orientation (C-axis orientation) is remarkably recognized in the diffraction pattern.

The results of comparison of the reproducibility of the height of the sample surface are shown in Table 1 below. According to the present invention, the measurement reproducibility is very excellent, and it was confirmed that the height of the sample surface for each measurement is kept constant. You can see that it is inferior.

[0014]

[Table 1]

[0015]

According to the present invention, the powder sample can be evaluated by X-ray diffraction without being oriented. Further, since the sample height is constant for each measurement, it can be applied to crystal structure analysis.

[Brief description of drawings]

FIG. 1 is a diagram illustrating a structure of a sample holder of the present invention.

FIG. 2 shows L fixed using the sample holder of the present invention.
6 is a graph showing the X-ray diffraction measurement results of iCoO ₂ powder.

FIG. 3 is a LiC fixed by a pressing method of a conventional example.
oO is a graph showing the ₂ powder X-ray diffraction measurement results of the.

[Explanation of symbols]

1 Plate with through holes 2 Organic film 3 Adhesive 5 Sample holder 6 Solvents containing collodion 7 Powder sample

Claims (3)

[Claims] 1. A plate having a through hole, an organic film adhered to one surface of the plate by a fixing agent so as to close the through hole, and a powder sample fixed to an inner surface of the organic film so as to be fixed. X comprising a collodion thin film
Sample holder for line diffraction measurement. 2. The organic film has a thickness of 10 μm or less, has a larger area than a through hole of a plate, and has a composition that does not chemically react with collodion.
The sample holder described in 1. 3. A sample fixing in X-ray diffraction measurement, characterized in that an organic film is attached to one surface of a plate having a through hole with a fixing agent, and a powder sample is fixed to a collodion thin film attached to the inner surface of the organic film. Method.