JP2003098125A - Sample holder for evaluating magnetic orientation properties and magnetic orientation measuring method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample holder capable of evaluating the magnetic orienta tion properties of a material powder having magnetism by X-ray diffraction and to provide a magnetic orientation measuring method for measuring the magnetic orientation properties of the material powder having magnetism. SOLUTION: As the constitution of the sample holder for evaluating magnetic orientation properties, a magnet lump having a surface on which a sample to be inspected can be placed, a container having no crystallinity for fixing the magnet lump therein and a base part for fixing the container are provided. Further, as the magnetic orientation measuring method, a sample holder having a sample stage part having the magnet lump fixed therein is prepared and the sample to be inspected is sprinkled over the magnet lump of the sample holder to magnetically orient the sample to be inspected and the magnetically oriented sample to be inspected is subjected to X-ray diffraction and a degree of magnetic orientation is calculated from the measured result of X-ray diffraction.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample holder used for X-ray diffraction measurement for evaluating the magnetic orientation of a material powder having magnetism and a magnetic orientation measuring method using the sample holder.

[0002]

2. Description of the Related Art Alignment of crystals in a specific direction due to the crystal structure is called crystal orientation, and rolled steel sheets, plating films, etc. are often oriented in some direction. In order to quantitatively evaluate the crystal orientation degree of such a material, it can be obtained from the relative value of the X-ray diffraction peak intensity ratio of the oriented sample and the X-ray diffraction peak intensity ratio of the non-oriented sample. On the other hand, magnetic alignment, not crystal structure, is called magnetic orientation, and a magnetic material is magnetically oriented in a specific direction.

[0003]

When the material is a powder, it does not generally orient because the individual crystal grains are randomly present, but the crystal orientation is orientated by pressing or hardening the sample by applying force. I have something to do. The same applies to a powder sample having magnetism, and the crystal orientation may occur by fixing, but the orientation of the crystal orientation does not necessarily correspond to the orientation of the magnetic orientation. for that reason,
By performing X-ray diffraction using the conventional fixing method, the crystal orientation of the magnetic material powder can be quantitatively evaluated, but the magnetic orientation cannot be evaluated.

Therefore, it is an object of the present invention to provide a sample holder for making it possible to evaluate the magnetic azimuth orientation of a material powder having magnetism by X-ray diffraction.

It is an object of the present invention to provide a magnetic azimuth orientation measuring method for measuring the magnetic azimuth orientation of a magnetic material powder.

[0006]

The present inventor uses a sample holder composed of a sample stage section and a base section in order to evaluate the magnetic azimuth orientation of a magnetic material powder by X-ray diffraction. Have been found to be effective. The sample stage part is a container made of a material having no crystallinity,
It is composed of a magnet block and an adhesive, and the magnet block is put in a container and fixed with an adhesive. When this is mounted on the base part and the test sample is sprinkled on the upper surface of the sample stage part, the test sample is oriented in the magnetic direction by the magnetic force of the magnet mass of the sample stage part. An X-ray diffraction pattern reflecting the azimuthal orientation can be observed. For the test sample after the measurement, the adhesive agent on the sample stage portion is removed and the magnet block is removed to easily collect the entire amount of the test sample.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The structure of a sample holder of the present invention and steps of a measuring method are shown in FIG. As shown in FIGS. 1a and 1b, the sample stage unit 3 includes a container 1 having no crystallinity.
And the magnet mass 2 and the adhesive agent, and the magnet mass 2 is placed in the container 1 and fixed with the adhesive agent to form the sample stage section 3.

Next, as shown in FIGS. 1b and 1c, the sample stage portion 3 having the fixing agent 5 placed on the base portion 4 is mounted on the base portion 4 to form the sample holder 6 of the present invention. The sample 7 to be inspected is sprinkled on the upper surface of the sample stage part 3 while adjusting so as to match the height of the guide part of the sample holder 6 (dotted line in the figure).

As shown in FIG. 1d, the test sample 7 sprinkled is fixed by the magnetic force of the magnet mass 2 so as to be stacked in the height direction while being magnetically oriented in a specific direction. By mounting this on an X-ray diffractometer and performing X-ray diffraction measurement, an X-ray diffraction pattern reflecting the magnetic orientation can be obtained.

The features of the sample holder will be described below in Examples. (Example) For low Sm ₂ Fe17N ₃ samples B of the sample A and the magnetic properties of high Sm ₂ Fe ₁₇ N ₃ magnetic properties, FIG fixed to the X-ray diffraction measurements were performed on the sample holder 2
Shown in. In addition, from the measurement results in Fig. 2, an arbitrary diffraction peak 9
The results of calculating the degree of orientation using a book are shown in FIG. Here, the degree of orientation was calculated by the following method.

The magnetic orientation degree of an arbitrary peak is K, the peak intensity of an arbitrary peak in an actual sample is I _PO (actual sample), and the sum of the peak intensities of all selected peaks in the actual sample is I _PS ( (Actual sample), the peak intensity in the non-oriented state of any peak is I _PO (non-oriented), and the sum of the peak intensities of all selected peaks in the non-oriented state is I _PS (non-oriented)
Then, K = {I _PO (actual sample) / I _PS (actual sample)} / {I _PO (non-oriented) / I _PS (non-oriented)}

It can be seen from FIG. 3 that the K value at the (006) peak of sample A is calculated to be high, and the higher the characteristic, the more the C-axis orientation is remarkable.

Comparative Example Sm ₂ Fe ₁₇ N ₃ Sample A of the Example
FIG. 4 shows the X-ray diffraction measurement results for the sample, which was fixed with the sample holder and when it was fixed with the glass sample holder by the pressing method. Further, FIG. 5 shows the calculation result of the orientation degree using the arbitrary nine diffraction peaks from the measurement result of FIG. From FIG. 5, it can be seen that no particular orientation was observed in the case of the glass sample holder, but when the sample holder was fixed, X-ray diffraction measurement could be performed in a state of being magnetically oriented in a specific direction (C-axis direction). .

Table 1 shows the results of comparison of the sample recovery rates when measured with the sample holder and the glass sample holder.

[Table 1]

According to the sample holder, almost all of the sample used for the measurement can be collected.

[0016]

According to the sample holder of the present invention, it is possible to evaluate the magnetic orientation of the magnetic material powder by X-ray diffraction. In addition, the total amount of the sample after the measurement can be easily collected.

[Brief description of drawings]

FIG. 1 is a diagram showing a structure of a sample holder of the present invention and steps of a measuring method.

FIG. 2 is a graph showing the X-ray diffraction measurement results of two samples of SmFeN powder having different magnetic properties.

FIG. 3 is a graph showing the degree of orientation calculated based on the result of FIG. 2.

FIG. 4 is a graph showing an X-ray diffraction measurement result of the same —SmFeN powder measured using the sample holder and a glass sample holder.

5 is a graph showing the degree of orientation calculated based on the result of FIG. 4.

[Explanation of symbols]

1 Containers that do not have crystallinity 2 magnet mass 3 Sample stage section 4 base 5 fixative 6 Sample holder 7 Test sample

   ─────────────────────────────────────────────────── ─── Continued front page    F-term (reference) 2G001 AA01 BA18 CA01 GA01 GA10                       GA13 HA01 JA07 JA20 KA20                       LA02 MA04 QA01 QA03

Claims (5)

[Claims] 1. A sample holder for evaluating magnetic azimuth orientation, comprising a sample stage portion and a base portion capable of evaluating the magnetic azimuth orientation property by X-ray diffraction. 2. The sample holder according to claim 1, wherein the sample stage portion has a structure in which a magnet mass is fixed by using a fixing agent in a container made of a material having no crystallinity. 3. The sample holder according to claim 1, wherein the base unit has a structure capable of fixing the sample stage unit. 4. A magnet mass having a surface on which a sample to be tested can be mounted, a container having no crystallinity for fixing the magnet mass inside, and a base portion for fixing the container. A sample holder for evaluating magnetic orientation, which is characterized in that 5. A sample holder having a sample stage part in which a magnet block is fixed is prepared, and the sample sample is sprinkled on the magnet block of the sample holder to magnetically orient the sample sample. A magnetic azimuth orientation measuring method, which comprises subjecting an oriented test sample to X-ray diffraction, and calculating a magnetic orientation degree from a measurement result of X-ray diffraction.