JP2018066652A - Analytical method of powder sample - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a technique that improves the accuracy and correctness of X-ray diffraction measurement.SOLUTION: An analytical method of powder samples includes: filling a powder sample into a recess which is formed on one face of a flat plate-like sample container and of which a periphery is surrounded with a main surface of the sample container; using a measurement sample produced by shearing the powder sample by moving a flat plate-like jig while keeping a state of the main surface of the flat plane-like sample container in contact with a flat face of the flat plate-like jig; and conducting X-ray diffraction measurement for the powder sample of the measurement sample.SELECTED DRAWING: Figure 4

Description

  The present invention relates to a method for analyzing a powder sample. More specifically, the present invention relates to a powder sample analysis method for performing X-ray diffraction measurement using a measurement sample in which a powder sample is suitably prepared and adjusted in a sample container.

  X-ray diffractometry is a new material for research and development, such as inorganic and organic powders, polymer materials, proteins, metal parts, organic and inorganic thin-film semiconductors, and colloidal particles as a means of investigating the state and physical properties of substances. To various materials related to production. For example, in Patent Document 1, X-ray diffraction measurement is performed on a powder sample obtained by pulverizing minerals. This analysis method irradiates a sample with X-rays having a predetermined wavelength, observes the X-ray diffraction action by the crystal lattice, and performs qualitative, quantitative, and identification of various substances and materials.

As a method for producing a measurement sample used for X-ray diffraction measurement, it is described as a conventional example in Patent Document 2, but in the analysis of a powder sample in X-ray diffraction method, a powder sample is placed in a recess of a measurement sample holder. After filling, a method of filling the main surface of the sample container while rubbing with a slide glass or the like (hereinafter referred to as abrasion) is generally performed.
Further, according to JIS-K-0131: X-ray diffraction analysis general rules and JIS-R-7651: Carbon material lattice constant and crystallite size measurement method, in the preparation of a sample, a powder sample is worn into a sample container. There is a description that the powder sample must be filled uniformly and smoothly so as to coincide with the main surface of the sample container (conform to the same height).
As described above, in order to maintain the accuracy and accuracy of the X-ray diffraction method, the surface of the powder sample raised from the concave portion of the sample container is smoothed, and the main surface of the sample container and the powder sample are adjusted to the same height. Operation is required.

  However, when the powder sample is scraped into the sample container, in addition to the variation due to the particle size of the powder sample, variations due to personal experience and know-how are likely to occur. These variations are the peak positions of the X-ray diffraction measurement (diffraction angle: 2θ). ) And the half-value width are causes for deteriorating accuracy and accuracy (see Patent Document 2). In Patent Document 2, in order to solve this problem, a sample prepared by providing a fluororesin-based sheet, a resin surface-attached board to which the fluororesin-based sheet is attached, a resin surface-attached base to which the sheet is attached, and a thickness adjusting jig. A pedestal is used.

  On the other hand, Patent Document 3 discloses a special sample container for adjusting the main surface of the sample container and the powder sample to the same height. This special sample container is intended to smooth the surface of the powder sample. No mention at all. Moreover, in order to use the special sample container, if there is a need for modification of parts on the X-ray diffractometer main body side, such as a sample container mounting base, or automatic measurement using an autosampler, a sample changer, a transfer arm, Remodeling is required and it is not practical to apply.

JP-A-7-12760 JP 2006-118557 A JP-A-8-247969

Rigaku Corporation, “Sample Preparation for Powder X-ray Diffraction Measurement”, [online], Webinar (Online Seminar) [Rigaku] (pdxsample), [Search January 20, 2016], Internet <URL: http: // www . rigaku. co. jp / rigaku. com / weberar / getwebinar. php? getwebinar = pdxsample>

  The present invention has been made paying attention to the above problems, and in a powder sample analysis method for performing X-ray diffraction measurement on a powder sample filled in a recess formed in a sample container. An object of the present invention is to provide a technique for improving accuracy and accuracy in X-ray diffraction measurement using a measurement sample in which a powder sample is prepared and adjusted in a sample container.

As mentioned earlier, scraping of powder samples into sample containers is involved in the accuracy and accuracy of X-ray diffraction measurement, and depending on the type of sample, the required accuracy and accuracy may not be satisfied. Are known.
Hereinafter, a description will be given with reference to FIG. FIG. 1 is a schematic cross-sectional view showing how a powder sample overflowing from a concave portion of a sample container is scraped with a spatula in the prior art. Reference numeral 1 is a sample container, reference numeral 11 is its main surface, and reference numeral 12 is a concave portion. , 2 indicates a spatula, and P indicates a powder sample. Hereinafter, for convenience of explanation, reference numerals are omitted.

  When the powder sample overflowing from the concave portion of the sample container is scraped off with a spatula, as shown in FIG. 1, the operator holds the tip of the spatula against the main surface of the sample container, Lift the base end of the spatula upward from the main surface of the sample container and make an angle. The powder sample overflowing from the concave portion is usually scraped off by pulling the spatula forward. As another method, Non-Patent Document 1 introduces an operation of preparing another sample container as a scraping jig and scraping it using the back surface thereof. When scraping off, as in the above method, with respect to the main surface of the sample container, the scraping jig is lifted upward to make a certain angle (when tilted, between the main surface of the sample container, To the extent that another shaving jig can be inserted), it is pulling forward.

  However, minute irregularities may be formed at the tip of the spatula or scraping jig. When scraping is performed using this spatula or chafing jig, the unevenness at the tip of the spatula or chafing jig is reflected directly on the surface of the powder sample. This is shown in FIG. FIG. 2 shows a state in which minute unevenness present at the tip of the spatula reflects unevenness on the surface of the powder sample filled in the recess when the powder sample is scraped off. And (a) is an enlarged schematic view of the tip part where the spatula is scraped off, (b) is the powder sample surface filled in the recess when scraped by the conventional operation using the spatula of (a). FIG.

  The unevenness on the surface of the powder sample shown in FIG. 2 (b) is a reflection of the unevenness on the tip of the scraped spatula, and the unevenness on the surface of the powder sample can be made by each operator with the spatula in front. There are individual differences depending on the trajectory at the time of pulling, the angle at which the spatula is lifted, which spatula is used, etc., and it will change greatly. The same applies to the case of scraping using a glass plate or the like, including the method of Non-Patent Document 1. Even when using a glass plate, it is usual to lift the base end of the glass plate upward from the main surface of the sample container and to make an angle because of the need to grip the glass plate. The unevenness at the tip is reflected on the surface of the powder sample as it is.

  This is the reason why the accuracy and accuracy are reduced due to the variation of individual experience and know-how in smoothing the surface of the powder sample and adjusting the main surface of the sample container and the powder sample to the same height. Therefore, the present inventor has conceived.

  In addition, it is also known that the particle size of the powder sample has a great influence on the degree of accuracy and accuracy reduction in the X-ray diffraction measurement. JIS-K-0131: X-ray diffraction mentioned above. If the general rules of analysis are followed, a sample having a large particle size needs to be pulverized to a particle size of 10 μm or less using a mortar or the like, if necessary, manually or with a dedicated machine. However, a method for confirming the particle size, a method for determining the necessity of pulverization, and the like have not been disclosed.

  The present inventor has not only worn out the powder sample filled in the recess formed in the sample container, but also focused on checking the particle size of the powder sample and determining the necessity of pulverization. As a result, these problems have been solved.

The embodiments of the present invention made based on the above findings are as follows.
The first aspect of the present invention is:
A powder sample is filled in a concave portion surrounded by the main surface of the sample container, and the main surface of the flat sample container, the flat surface of the flat jig, The X-ray diffraction measurement was performed on the powder sample of the measurement sample using the measurement sample prepared by moving the flat jig while scraping the powder sample with the plate in contact. It is the analysis method of the powder sample characterized by performing.

According to a second aspect of the present invention, in the invention according to the first aspect,
Before scraping the powder sample,
Determining whether the maximum particle size of the powder sample is 10 μm or less,
When the maximum particle size of the powder sample exceeds 10 μm, the powder sample is pulverized until the maximum particle size is 10 μm or less,
When the maximum particle size of the powder sample is 10 μm or less, the powder sample is scraped off.

According to a third aspect of the present invention, in the invention according to the second aspect,
The method of analyzing a powder sample, wherein the particle size of the powder sample is measured before the determination.

According to a fourth aspect of the present invention, in the invention according to the third aspect,
The particle size measurement is a powder sample analysis method using a laser diffraction / scattering method.

  According to the present invention, accuracy and accuracy in X-ray diffraction measurement can be improved.

It is the cross-sectional schematic which shows a mode that the powder sample overflowed from the recessed part of the sample container is scraped off with a spatula by the conventional method. It is a figure which shows a mode that the deformation | transformation of the micro unevenness | corrugation which exists in the front-end | tip of a spatula reflects an unevenness | corrugation on the surface of the powder sample with which the recessed part was filled when scrubbing a powder sample by a conventional method, (a ) Is an enlarged view of the tip of the spatula, and (b) is a diagram showing a plan view of the surface of the powder sample filled in the recesses after scraping by a conventional method. It is a flowchart which shows the analysis method of the powder sample of this embodiment. It is a cross-sectional schematic diagram which shows the mode of abrasion in preparation of the sample for a measurement of this embodiment. In Example 1, it is a graph which shows the result of having measured the particle size of the powder sample before pulverization. In Example 1, it is a graph which shows the result of having measured the particle size of the powder sample after grinding | pulverization.

Hereinafter, embodiments of the present invention will be described in the following order.
1. 1. Analysis method of powder sample 1-1. Particle size measurement 1-2. Particle size determination 1-3. Grinding of powder sample 1-4. Preparation of measurement sample 1-5. 1. X-ray diffraction measurement 2. Effects of the embodiment Modifications etc. In this specification, “to” refers to a value not less than a predetermined value and not more than a predetermined value. In the present embodiment, preparation of a measurement sample and X-ray diffraction measurement are essential, but particle size measurement, particle size determination, and pulverization of a powder sample are suitable examples.

<1. Analysis method of powder sample>
In the present embodiment, the following operations are performed according to the flowchart shown in FIG. In addition, the powder sample in the present embodiment is not particularly limited in type, particle shape, or the like as long as a measurement result can be obtained when X-ray diffraction measurement is performed.

1-1. Particle size measurement In the particle size measurement, the particle size of a powder sample is measured. As a specific measuring method, a known method may be used. For example, particle size measurement methods include sieve method, natural sedimentation method, centrifugal sedimentation method, air permeation method, Coulter method, dynamic light scattering method, image analysis method, laser diffraction / scattering method, and the latest There are various methods such as ultracentrifugation. These methods have different advantages and disadvantages in addition to the measurement range of particle size and particle size distribution depending on the measurement principle, so it is important to use them properly depending on the particle size region and purpose.

  In the present embodiment, it is necessary to measure the maximum particle size of the powder sample, but among the above methods, it is preferable to employ the laser diffraction / scattering method. The laser diffraction / scattering method has better operability than the sieving method, each sedimentation method and the air permeation method. In view of the reproducibility of the particle size measurement, the measurement range (microns), etc., the laser diffraction / scattering method for obtaining the effective diameter is generally suitable in the present embodiment. Examples of the laser diffraction / scattering apparatus include Microtrack MT3300EXII (manufactured by Microtrack Bell Co., Ltd.), LA950V2 (manufactured by Horiba, Ltd.), SALD-3100 (manufactured by Shimadzu Corporation), and the like. However, it is not particularly limited.

1-2. Particle size determination In the particle size determination, it is determined whether or not the maximum particle size of the powder sample is 10 μm or less before the preparation of the measurement sample described later. In the determination, when the maximum particle size of the powder sample exceeds 10 μm, the powder sample is pulverized until the maximum particle size becomes 10 μm or less (pulverization of the powder sample described later). On the other hand, when the maximum particle size of the powder sample is 10 μm or less, the process proceeds to preparation of a measurement sample.

  As described above, the reason for determining the particle size is as follows.

  First, when X-ray diffraction measurement is performed on a powder sample, setting the particle size of the powder sample to an appropriate value leads to improvement in measurement accuracy and accuracy. Based on the pulverization of the sample described in JIS-K-0131: General rules for X-ray diffraction analysis, the present inventor has determined the particle size condition that the maximum particle size of the powder sample is 10 μm or less. Set.

  Another reason is largely related to the production of a measurement sample described later. In the particle size determination, it is determined whether or not the maximum particle size of the powder sample exceeds 10 μm. When the maximum particle size of the powder sample exceeds 10 μm, the above-mentioned is performed until the maximum particle size becomes 10 μm or less. There is a great significance to pulverize the powder sample to obtain an appropriate particle size. This is because the smaller the maximum particle size of the powder sample, the smaller the unevenness at the tip of the scraping jig, when the powder sample is scraped off at an angle with a scraping jig such as a spatula or glass plate. Deep traces will remain on the powder sample. Therefore, in the preparation of the measurement sample to be described later, it is necessary to use the scraping method of the present invention so as not to leave minute traces on the tip of the scraping jig on the powder sample.

1-3. Grinding of powder sample In the above particle size determination, if it is determined that the maximum particle size of the powder sample exceeds 10 μm, the powder sample is ground until the maximum particle size becomes 10 μm or less. It is preferable to carry out the treatment. As a specific method, a known method may be used. For example, an agate mortar, a vibration mill, or an airflow crusher. In addition, after performing the said grinding | pulverization process, the particle size measurement of a powder sample and a particle size determination are performed again, and the said powder sample is pulverized until the maximum particle size becomes 10 micrometers or less.

1-4. Production of measurement sample Production of a measurement sample is one of the major features of this embodiment. In the preparation of the measurement sample, a powder sample formed on one surface of a flat sample container and filled with a recess surrounded by the main surface of the sample container, a main surface of the flat sample container, The powder sample is scraped off by moving the flat jig while keeping the flat surface of the flat jig in contact. In the present embodiment, a glass plate is used as the flat jig. The procedure will be described below.

First, a flat sample container used for X-ray diffraction measurement is prepared. As the sample container, a publicly known one may be used, but a recess formed on one surface of a flat sample container, surrounded by the main surface of the sample container, for filling a powder sample, It is suitable to use a sample container having the same. In addition, the main surface said here refers to the part on the same plane other than the recessed part (the side surface and bottom face) in one surface of a flat sample container.
Then, a powder sample having a maximum particle size of 10 μm or less, which has been subjected to the particle size measurement, the particle size determination, and the pulverization of the powder sample, is filled in the concave portion of the sample container. At that time, it is preferable to fill the powder sample with an amount that slightly overflows from the recess.
Moreover, the thing provided with the opening part penetrated to the flat sample container center part back surface can also be used. In the case of using a flat sample container having the above-mentioned opening, it is placed on a flat substrate such as a flat glass plate, filled with a powder sample in a recess made by the flat substrate and the opening, and pressed to The powder sample should not be dropped.

  Then, scraping is performed. The scraping will be described with reference to FIG. FIG. 4 is a schematic cross-sectional view showing the state of scraping in the production of the measurement sample of the present embodiment. Reference numeral 3 denotes a flat jig, but the reference numeral is omitted hereinafter. As shown in FIG. 4, the powder sample is moved by moving the flat jig while keeping the flat surface of the flat jig and the main surface of the sample container (that is, the flat portion other than the concave portion) in contact with each other. Scrape off. More specifically, in the state where the plane of the flat jig and the main surface of the sample container are in surface contact, the flat jig is moved and the powder sample is moved while maintaining both planes in parallel. Scrape off. In this way, the main surface of the sample container and the surface of the powder sample filled in the recess can be made the same height. In addition, according to the above method, a flat plate that passes after the powder sample has been scraped off on the side surface of the flat jig without leaving traces of deep irregularities in the powder sample due to minute irregularities at the tip of the scraping jig. The surface of the powder sample in the recess is uniformly flattened by the flat portion of the jig. Therefore, the surface of the powder sample can be smoothed.

  In the above example, a glass plate is used as the flat jig, but the present invention is not limited to this, and the flat jig that can be scraped while being parallel to the main surface of the sample container. If it is a tool, there is no limitation in particular. For example, you may use the jig which attached the handle like the plastering board (trowel) board to the flat metal plate which can be frayed.

1-5. X-ray diffraction measurement The above-mentioned measurement sample in which the powder sample is filled in the concave portion of the sample container is attached to a sample holder for an X-ray diffractometer, and suitable X-ray diffraction according to the type and brand of the powder sample. Select measurement conditions and perform X-ray diffraction measurement. As the scanning condition, a continuous mode in which the measurement is performed while driving the shaft at a constant speed may be used, or a step mode in which the shaft is fed at a constant angle and measured in a stationary state may be used.

<2. Advantages of the embodiment>
According to the present embodiment, it is possible to improve accuracy and accuracy in X-ray diffraction measurement. More specifically, in the abrasion when the measurement sample is produced, the flat jig is in contact with the main surface of the flat specimen container and the flat surface of the flat jig on the surface of the specimen container. By moving the flat jig and scraping the powder sample, the main surface of the sample container and the sample surface can be adjusted to the same height and the sample surface can be smoothed. There are no irregularities on the surface of the powder sample, which caused variations in experience and know-how, and reduced accuracy and accuracy, and accuracy and accuracy can be achieved by X-ray diffraction measurement results.

  In particle size measurement, the laser diffraction / scattering method is used to perform highly reliable particle size measurement in just a few minutes compared to other methods, and the maximum particle size of the powder sample used for measurement can be easily obtained. If the maximum particle size is larger than the criterion, it is possible to move to pulverization of the powder sample at an early stage. By performing pulverization, it is possible to improve the accuracy and accuracy of measurement X-ray diffraction line misalignment and peak intensity reduction caused by non-uniformity of the sample, and reduce the frequency of reanalysis. .

<3. Modification>
The technical scope of the present invention is not limited to the above-described embodiment, and various modifications and improvements are added within the scope of deriving specific effects obtained by the constituent elements of the invention and combinations thereof. Including.

  For example, in the present embodiment, a flat sample container is used, but it may be a plate-like one as long as it has a main surface as a flat surface and a recess is surrounded by the main surface. For example, a block-shaped sample container having a certain thickness may be adopted. The same applies to the flat jig, and there is no particular limitation as long as there is a plane that can contact the main surface (plane) of the sample container.

  In preparation of a powder sample to be used for measurements other than X-ray diffraction measurement (for example, JIS-R-5201: physical test method for cement (“9. Freezing test” therein)), Put in a sample container and scrape off excess to smooth the surface. At this time, it is also possible to employ the above-described scraping method of the present invention. Therefore, in the above-described embodiment, “X-ray diffraction measurement” may be simply referred to as “measurement”.

  Hereinafter, this embodiment will be described. The technical scope of the present invention is not limited to the following examples.

Example 1
Using the powder sample (metal composite oxide powder A), the position and intensity of the strongest diffraction line in the crystal main phase detected from the X-ray diffraction profile were calculated and evaluated according to the following procedure. In addition to the lattice constant, the height deviation of the powder sample from the main surface of the sample container was calculated and evaluated by Rietveld analysis, which is a crystal structure analysis technique.

<Particle size measurement>
First, the particle size of the powder sample was measured with Microtrac MT3300EXII (manufactured by Microtrac Bell Co., Ltd.), which is a measuring apparatus using a laser diffraction / scattering method. The result is shown in FIG. The maximum particle size was about 40 μm. Various conditions in the particle size measurement are as described in Table 1.

<Determination of particle size>
Next, the necessity of pulverization was determined from the particle size measurement results. As described above, since the maximum particle diameter exceeded 10 μm, it was determined that pulverization was necessary.

<Pulverization of powder sample>
Since it was determined in the particle size determination that pulverization was necessary, manual pulverization using an agate mortar was performed for about 10 minutes. Thereafter, the particle size of the pulverized powder sample was measured again. As shown in FIG. 6, the maximum particle size was 10 μm or less (about 2.5 μm). Proceed to.

<Preparation of measurement sample>
In order to fill the powder sample after pulverization, a sample container formed on one surface of a flat sample container and having a recess surrounded by the main surface of the sample container is prepared. The recess was filled. At that time, an amount of powder sample was filled so as to slightly overflow from the concave portion.

  Then, as shown in FIG. 4, the flat jig is moved and the powder sample is rubbed while the surface of the glass plate and the main surface of the sample container (that is, the portion other than the concave portion) are in contact with each other. Chopped.

The prepared measurement sample was attached to a sample holder for an X-ray diffractometer, and X-ray diffraction measurement was performed under predetermined conditions shown in Table 2.
X'Pert-PRO / MPD (Spectris Co., Ltd.) was used for the X-ray diffractometer, and High Score Plus (Spectris Co., Ltd.) was used for the analysis software.
Thereafter, the diffraction line on the 003 plane, which is the strongest diffraction line of the powder sample, is separated from other diffraction lines, the position (2θ) and intensity (cps) of the diffraction line are obtained, and Rietveld analysis is performed. In addition to the lattice constant, the height deviation of the powder sample from the main surface of the sample container was calculated. The results are shown in Table 3.

Next, with regard to scraping of the powder sample into the sample container, scraping according to the present invention (moving the flat jig in contact with the main surface of the sample container) and scraping by the conventional method (main of the sample container) In order to compare the angle of the spatula with respect to the surface), the surface states of the powder samples were compared.
Therefore, the flatness (surface roughness) of the powder sample after the abrasion of Example 1 was examined using an optical profiler NewView 6200 (manufactured by Zygo-Corporation). The results are shown in Table 3.

  According to Example 1, in addition to the position and intensity of the diffraction line, the lattice constant, and the standard deviation with respect to the deviation of the height of the powder sample from the main surface of the sample container is small, and the analysis result is very reliable. Proven to be obtained. In addition, from the investigation results of flatness, it was proved that the flatness was improved by using the present invention, and the surface of the powder sample could be smoothed better. From these results, it was found that the fraying according to the present invention can cope with an analysis sample requiring high reliability rather than the fraying by the conventional method.

(Example 2)
Using the powder sample (metal composite oxide powder A), the particle size measurement to particle size determination is omitted, and the maximum particle size exceeds 10 μm. Diffraction measurement was performed. The results are shown in Table 3.
Further, in the same manner as in Example 1, the flatness (surface roughness) of the powder sample after the abrasion in Example 2 was examined using an optical profiler NewView 6200 (manufactured by Zygo- Corporation). The results are shown in Table 3.

  Compared with the average value of Example 1, when the particle size measurement to particle size determination are omitted, the height of the powder sample from the main surface of the sample container in addition to the position and intensity of the diffraction line, the lattice constant, and the like. There was a tendency for the difference to increase. Further, the flatness was the same. From these results, the effect of producing a sample for X-ray diffraction measurement using a scraping method of the present invention using a powder sample pulverized to a maximum particle size of 10 μm or less could be confirmed.

(Comparative Example 1)
When the powder sample (metal composite oxide powder A) that had been crushed in Example 1 was scraped off into the sample container, the same operation as that performed in the conventional method was performed. Specifically, in order to hold the glass plate while applying the tip of the glass plate to the main surface of the sample container, the base end of the glass plate is lifted upward from the main surface of the sample container, and an angle is formed. Then, by pulling the glass plate to the front, the powder sample overflowing from the recess was scraped off with the glass plate in an angled state with respect to the main surface of the sample container. Other than that was carried out similarly to Example 1, and performed the X-ray-diffraction measurement. The results are shown in Table 3. Further, in the same manner as in Example 1, the flatness (surface roughness) of the powder sample after the abrasion of Comparative Example 1 was examined using an optical profiler NewView 6200 (manufactured by Zygo-Corporation). The results are shown in Table 3.

  According to Comparative Example 1, compared to the case of Example 1 in Table 3, in addition to the position and intensity of the diffraction line, the standard deviation regarding the deviation of the height of the powder sample from the main surface of the sample container, in addition to the lattice constant, Was clearly inferior. Moreover, also about flatness, the flatness as Example 1 was not acquired in the comparative example 1, and it turned out that it is inferior also about smoothing the surface of a powder sample.

(Comparative Example 2)
Using the powder sample (metal composite oxide powder A), omitting the particle size measurement to particle size determination, and in a state where the maximum particle size exceeds 10 μm, it is worn by the conventional method (on the main surface of the sample container, Angled the spatula). Other than that was carried out similarly to Example 1, and performed the X-ray-diffraction measurement. The results are shown in Table 3. Further, in the same manner as in Example 1, the flatness (surface roughness) of the powder sample after abrasion of Comparative Example 2 was examined using an optical profiler NewView 6200 (manufactured by Zygo- Corporation). The results are shown in Table 3.

  Compared with the average value of Example 1, particle size measurement to particle size determination was omitted, and abrasion according to the present invention was not performed (the plate-shaped jig was moved while being in contact with the main surface of the sample container). In some cases, the difference tended to become larger with respect to the deviation of the height of the powder sample from the main surface of the sample container in addition to the position and intensity of the diffraction line, the lattice constant, and the like. Further, the flatness was the same. From these results, the effect of pulverizing the maximum particle size to 10 μm or less was further clarified.

DESCRIPTION OF SYMBOLS 1 ......... Sample container 11 ... Main surface 12 ... Concavity 2 ...... Spatula 3 ......... Plate-shaped jig | tool P ......... Powder sample

Claims (4)

  A powder sample is filled in a concave portion surrounded by the main surface of the sample container, and the main surface of the flat sample container, the flat surface of the flat jig, The X-ray diffraction measurement was performed on the powder sample of the measurement sample using the measurement sample prepared by moving the flat jig while scraping the powder sample with the plate in contact. A method for analyzing a powder sample, comprising: Before scraping the powder sample,
Determining whether the maximum particle size of the powder sample is 10 μm or less,
When the maximum particle size of the powder sample exceeds 10 μm, the powder sample is pulverized until the maximum particle size is 10 μm or less,
The method for analyzing a powder sample according to claim 1, wherein when the maximum particle size of the powder sample is 10 µm or less, the powder sample is scraped off.   The method for analyzing a powder sample according to claim 2, wherein the particle size of the powder sample is measured before the determination. 4. The method for analyzing a powder sample according to claim 3, wherein the particle size measurement uses a laser diffraction / scattering method.