Sample holder for measuring magnetic orientation and method for measuring magnetic orientation

Abstract

To provide a method for obtaining correct magnetic orientation information by tightly arranging specimens when using a specimen holder equipped with a magnet.SOLUTION: A specimen holder for magnetic orientation measurement is configured to hold a specimen when measuring a magnetic orientation of the specimen by X-ray diffraction. The specimen holder includes: a stage part in which a specimen is arranged on an upper side; a magnet arranged on a lower side of the stage part; and a specimen arrangement correction part having an opening and arranged so that a side face of the opening is housed within a region above the magnet. A related art thereof is also provided.SELECTED DRAWING: Figure 2

Description

[Technical field]

[0001] The present invention relates to a sample holder for measuring magnetic orientation and a method for measuring magnetic orientation. [Background technology]

[0002] Crystal orientation refers to the alignment of crystals in a specific direction due to the crystal structure. Rolled steel sheets and plating films often have crystals oriented in a certain direction. A known method for quantitatively evaluating the degree of crystal orientation in such materials is to determine it from the relative value of the X-ray diffraction peak intensity ratio of an oriented sample to that of a non-oriented sample.

[0003] In contrast, magnetic alignment rather than crystalline alignment is called magnetic orientation, and magnetic materials have a magnetic orientation in a specific direction.

[0004] When a material is in powder form, the individual crystal grains are randomly present and generally do not orient, but the crystal orientation may be oriented by applying force to the sample or by compacting it. The same is true for magnetic powder samples, which may become crystalline oriented by fixing them, but the direction of the crystalline orientation does not necessarily coincide with the direction of magnetic orientation. Therefore, by adopting the conventional fixing method and performing X-ray diffraction, the crystal orientation of magnetic material powders can be quantitatively evaluated, but the magnetic orientation cannot be evaluated.

[0005] Under such circumstances, Patent Document 1 discloses that it is effective to use a sample holder consisting of a stage portion (called a sample stage portion in Patent Document 1) and a base portion in order to evaluate the magnetic orientation of magnetic material powder by X-ray diffraction.

[0006] In Patent Document 1, a magnet (a lump of magnet in Patent Document 1) is placed in a container and fixed with an adhesive. This is attached to a base, and when a sample is sprinkled on the top surface of the container, the magnetic force of the magnet causes the sample to be oriented in the magnetic direction on the top surface of the container. Therefore, if an X-ray diffraction measurement is performed on a sample in a magnetically oriented state, an X-ray diffraction pattern reflecting the magnetic orientation can be observed. [Prior art documents] [Non-patent literature]

[0007] [Patent Document 1] JP 2003-98125 A Summary of the Invention [Problem to be solved by the invention]

[0008] Through intensive research by the present inventors, an improvement was found in the method described in Patent Document 1. In the method described in Patent Document 1, the sample on the stage is neatly oriented in the magnetic direction at the center of the magnet placed inside the container. On the other hand, when the sample moves away from the center of the magnet, the sample becomes dispersed (in other words, scattered) and oriented.

[0009] FIG. 1 is a schematic diagram of the sample holder described in Patent Document 1 when a sample is placed on it.

[0010] As shown in FIG. 1, the particles constituting the sample 5 tend to fall over as they move away from the center of the magnet 2.

[0011] In this state, the particles constituting the sample are dispersed on the stage 3, causing the inside of the sample 5 to become sparse. When the inside of the sample 5 becomes sparse, sufficient peak intensity cannot be obtained even when X-ray diffraction measurement is performed. As a result, there is a risk that correct magnetic orientation information cannot be obtained.

[0012] It is an object of the present invention to provide a method for obtaining accurate magnetic orientation information by packing the sample tightly when using a sample holder with a magnet. [Means for solving the problem]

[0013] The present inventors have thoroughly investigated the above-mentioned problems. As a result, in the configuration described in Patent Document 1, the inventors have come up with a new configuration in which the side of the opening is provided on the stage part and in the region directly above the magnet, and the side is used to prevent the particles constituting the sample from scattering, that is, the position of the sample is corrected so that the position of the sample is within the opening and therefore within the region directly above the magnet. A specific example of this configuration is as follows.

[0014] The first aspect of the present invention is A sample holder for holding a sample when measuring the magnetic orientation of the sample by X-ray diffraction, a stage portion on whose upper surface a sample is placed; A magnet disposed on the underside of the stage portion; A sample placement correction unit is arranged so that a side surface of an opening fits within the upper region of the magnet; A sample holder for magnetic orientation measurement comprising:

[0015] A second aspect of the present invention is the stage portion being formed by the outer surface of the bottom of the container; The magnet is fixed to the inner surface of the bottom of the container; The sample position correction unit is a ring-shaped sample holder for magnetic orientation measurement according to the first aspect, and is disposed above the magnet with the stage unit therebetween.

[0016] A third aspect of the present invention is A sample placement step of sprinkling a sample on the sample holder according to the first or second aspect to magnetically orient the sample on the upper surface of the stage and within the opening of the sample placement correction unit; a measuring step of performing X-ray diffraction measurement on the magnetically oriented sample and calculating the degree of magnetic orientation; The present invention relates to a method for measuring a magnetic azimuth orientation,

[0017] A fourth aspect of the present invention is The opening depth of the sample arrangement correction unit is smaller than the maximum vertical length of a particle aggregate in a state in which a plurality of particles constituting the sample are vertically connected due to magnetic orientation, The magnetic orientation measurement method according to the third aspect further includes a smoothing step between the sample placement step and the measurement step, in which particles protruding from the opening of the sample placement correction unit are smoothed to fit onto the upper surface of the sample placement correction unit. Effect of the Invention

[0018] According to the present invention, when using a sample holder with a magnet, the sample is packed tightly to obtain correct magnetic orientation information. [Brief description of the drawings]

[0019] [Figure 1] FIG. 1 is a schematic diagram of the sample holder described in Patent Document 1 when a sample is placed on it. [Diagram 2] FIG. 2(a) is a schematic perspective view showing the sample holder of this embodiment, and FIG. 2(b) is a schematic perspective view showing how a sample is sprinkled onto the sample holder. [Diagram 3] FIG. 3 is a schematic cross-sectional view of the sample holder of this embodiment after a sample placement step and a smoothing step have been carried out in that order. [Figure 4] FIG. 4 is a schematic plan view of the sample holder of this embodiment after a sample placement step and a smoothing step have been carried out in that order. [Diagram 5] FIG. 5(a) is a schematic cross-sectional view showing the state before the smoothing step, and FIG. 5(b) is a schematic cross-sectional view showing the state after the smoothing step. [Figure 6] FIG. 6 is a schematic perspective view showing a state in which the container of the sample holder of this embodiment is fixed to the base portion. [Figure 7] FIG. 7 is a schematic cross-sectional view of the modified sample holder after a sample placement step and a smoothing step have been carried out in that order. [Figure 8]Fig. 8(a) is a schematic cross-sectional view of a modified sample holder provided with a magnet holder after a sample placement step and a leveling step are performed in order, and Fig. 8(b) is a schematic bottom view of the modified sample holder provided with a magnet holder. [Figure 9] FIG. 9 is a graph showing the results of X-ray diffraction measurement for Example 1 and Comparative Example 1 (no magnet was used). [Figure 10] 10 is a graph showing the results of X-ray diffraction measurement of Example 1 and Comparative Example 2 (without using the sample position correction unit (ring)). Note that the graph of Example 1 in FIG. 10 is the same as the graph of Example 1 in FIG. [Figure 11] FIG. 11 is a graph showing the results of calculation of the degree of orientation (vertical axis) using eight arbitrary diffraction peaks (arranged on the horizontal axis) obtained from the measurement results of FIG. 9 for Example 1 and Comparative Example 1. [Figure 12] FIG. 12 is a graph showing the results of calculation of the degree of orientation (vertical axis) using eight arbitrary diffraction peaks (arranged on the horizontal axis) obtained from the measurement results of FIG. 10 for Example 1 and Comparative Example 2. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0020] The present embodiment will be described below. The suffix "-" indicates a value greater than or equal to a predetermined value and less than or equal to a predetermined value. The contents not described in this specification are incorporated by reference in the contents of Patent Document 1. In addition, the up-down direction in this specification refers to the top-bottom direction.

[0021] FIG. 2(a) is a schematic perspective view showing the sample holder 1 of this embodiment, and FIG. 2(b) is a schematic perspective view showing how a sample is sprinkled onto the sample holder 1. As shown in FIG.

[0022] The sample used in this embodiment is not limited as long as it has magnetism, but a powder composed of particles is preferable because it is easy to work with when carrying out the measurement method according to this embodiment.

[0023] This embodiment is a sample holder 1 for holding a sample when measuring the magnetic orientation of the sample by X-ray diffraction. The sample holder 1 has the following configuration. A stage portion 3 on whose upper surface 3a a sample is placed The magnet 2 arranged on the lower surface 3b of the stage portion 3 A sample placement correction unit 4 having an opening 4h and arranged so that the side surface of the opening 4h fits within the upper region of the magnet 2.

[0024] The stage part 3 is not limited in material or shape as long as the sample can be placed on the upper surface 3a and the magnet 2 can be fixed to the lower surface 3b. However, in order to perform X-ray diffraction measurement, it is preferable to configure the stage part 3 with a material that does not have crystallinity. In addition, if the stage part 3 does not have magnetic properties, it is possible to remove the magnet 2 without using force. As an example, the stage part 3 corresponds to the stage part 3 described in Patent Document 1, more specifically, to a container that does not have crystallinity. The stage part 3 is preferably made of the outer surface of the bottom of the container. In this case, in order to prevent the container from being soiled, an antifouling sheet may be provided on the container as part of the configuration of the stage part 3, and the container and the antifouling sheet may be sandwiched between them, and the sample may be magnetically oriented by a magnet.

[0025] There are no limitations on the material or shape of the magnet 2, so long as it is configured to be able to magnetically orient the sample across the stage section 3. For example, a cylindrical shape can be used as the shape. If it is cylindrical, a circular area (e.g., 10 to 15 mm in diameter) on the upper surface 3a of the stage section 3 directly above the magnet 2 can be effectively used as the X-ray beam irradiation area. However, even a rectangular prism-shaped magnet 2 can be used without problems as long as the area directly above the magnet 2 can sufficiently encompass the X-ray beam irradiation area. As an example, the magnet 2 corresponds to the "magnet block" described in Patent Document 1.

[0026] During irradiation with the X-ray beam, it is preferable that the magnet 2 is fixed to the inner surface of the bottom of the container. There is no limitation on the manner of fixing, and the magnet 2 may be fixed with an adhesive (glue, adhesive tape), or a structure that engages the bottom of the container and the magnet 2 may be formed on both. The magnet 2 may be fixed in a non-contact state with the inner surface of the bottom of the container, but in consideration of stably orienting the sample in magnetic orientation, it is preferable to have the two in contact with each other.

[0027] It is preferable to remove the magnet 2 after the irradiation of the X-ray beam is completed, that is, after the measurement is completed. In other words, it is preferable that the magnet 2 is detachably attached to the inner surface of the bottom of the container. By removing the magnet 2 after the measurement is completed, the force that draws the sample closer to the magnet 2 is released, and the sample can be easily removed from the stage part 3.

[0028] There are no limitations on the material or shape of the sample arrangement correction unit 4, so long as it has an opening 4h and is positioned so that the side of the opening 4h fits within the upper region of the magnet 2. However, considering the possibility that the sample may be oriented by the sample arrangement correction unit 4 rather than the magnet 2, a non-magnetic material (such as stainless steel or plastic (resin)) can be used for the sample arrangement correction unit 4.

[0029] During irradiation with the X-ray beam, the specimen position correction unit 4 is preferably fixed to the outer surface of the bottom of the container, i.e., the upper surface 3a of the stage unit 3. There is no limitation on the manner of fixing, and double-sided tape or adhesive may be used. After the irradiation with the X-ray beam is completed, i.e., after the measurement is completed, the specimen position correction unit 4 may be removed from the stage unit 3 in the same manner as the magnet 2, or may remain fixed therein.

[0030] The upper region of magnet 2 refers to the entire portion directly above magnet 2, and is the region that falls within the outline of magnet 2 when viewed in a plan view.

[0031] As its name suggests, the sample position correction unit 4 corrects the position of the sample so that the sample is located within the opening 4h and therefore within the area directly above the magnet 2. The side of the opening 4h can prevent the particles that make up the sample from scattering. In other words, the sample is only placed within the limited area of ​​the opening 4h. In addition, even if the particles try to scatter in this state, the particles that make up the sample will eventually come into contact with the side of the opening, and the sample position is corrected to the particle orientation at the center of the magnet in plan view (upright in this case) or a posture close to that. As a result of the above, the sample can be held tightly while maintaining the orientation of the sample in a specific direction (vertical in this embodiment) compared to the conventional method.

[0032] Regarding the opening 4h of the sample placement correction unit 4, the sample placement correction unit 4 is positioned on the upper surface 3a of the stage unit 3 so that when viewed in a plan view through the sample holder while leaving the outline, the outline of the opening 4h is contained within the outline of the magnet 2 fixed to the lower surface 3b of the stage unit 3.

[0033] The term "encompassing" here also includes the case where the two contours coincide (Example 1 described below). However, if the contour of the opening 4h is enclosed so that the two contours are only partially in contact, this is preferable because it is possible to partially eliminate the outermost edge of the magnet, which increases the inclination of the attitude of the particles that make up the sample, in the portion where the sample is placed. Furthermore, if the contour of the opening 4h is enclosed so as not to come into contact with the contour of the magnet 2, this is preferable because it is possible to completely eliminate the outermost edge of the magnet in the portion where the sample is placed.

[0034] As an example of this inclusion, the outline of the opening 4h of the sample arrangement and correction unit 4 may be located within a range of 0 to 2.0 mm from the outermost edge of the magnet toward the center in a plan view.

[0035] There is no limitation on the shape and size of the opening 4h of the sample arrangement correction unit 4. If the shape of the opening 4h is circular in a plan view, the X-ray beam irradiation area can be efficiently contained within the opening 4h. However, the shape of the opening 4h in a plan view may be rectangular or the like as long as the X-ray beam irradiation area can be contained within the opening 4h. In this case, it is preferable to contain the X-ray beam irradiation area within the opening 4h so that the outline of the opening 4h in a plan view does not come into contact with the X-ray beam irradiation area.

[0036] In plan view, the opening 4h, the magnet 2, and the X-ray beam irradiation area are preferably arranged concentrically. However, they do not need to be completely concentric, and a deviation of about 0.2 mm from each other is permissible.

[0037] It is preferable that the shapes of the upper and lower surfaces of the opening 4h are the same, but differences to the extent that they can be accommodated within the region above the magnet 2 are permissible.

[0038] The upper surface 4a of the sample arrangement correction unit 4 surrounding the opening 4h needs to be at the same height (so-called flush). This makes it possible to carry out a smoothing process in which the particles protruding from the opening 4h of the sample arrangement correction unit 4 are smoothed to the upper surface 4a of the sample arrangement correction unit 4. Furthermore, since the X-ray irradiation height is adjusted to match the upper surface 4a of the sample arrangement correction unit 4, accurate measurement of the angular position is possible.

[0039] FIG. 3 is a schematic cross-sectional view of the sample holder 1 of this embodiment after a sample placement step and a smoothing step have been carried out in that order.

[0040] FIG. 4 is a schematic plan view of the sample holder 1 of this embodiment after a sample placement step and a smoothing step have been carried out in that order.

[0041] FIG. 5(a) is a schematic cross-sectional view showing the state before the smoothing step, and FIG. 5(b) is a schematic cross-sectional view showing the state after the smoothing step.

[0042] As a result of the smoothing process, the height of the measurement surface becomes constant, and the peak position (diffraction angle) of the X-ray diffraction pattern does not shift. Furthermore, as shown in FIG. 5(a) to FIG. 5(b), by smoothing the particles protruding from the opening 4h, the protruding particles can be contained within the opening 4h (i.e., the area surrounded by the side surface of the opening 4h and the upper surface 4a of the sample arrangement correction unit 4), and the sample in the opening 4h becomes even denser. To ensure these effects, the depth of the opening 4h of the sample arrangement correction unit 4 is preferably set to a value smaller than the maximum vertical length of the particle aggregate 5a in which a plurality of particles constituting the sample are vertically connected by magnetic orientation. The depth of the opening 4h may be 1.0 to 3.0 mm, and is preferably 1.5 to 2.0 mm.

[0043] The sample position correction unit 4 is preferably ring-shaped and disposed above the magnet 2 across the stage unit 3. If this configuration is adopted, the present embodiment can be realized by simply disposing the ring-shaped sample position correction unit 4 (ring) on ​​the stage unit 3 for the existing sample holder 1 described in Patent Document 1. Furthermore, when the sample position correction unit 4 (ring) is adopted, the upper surface 4a of the ring-shaped frame can be used as an index for adjusting the sample height, which is the measurement surface, during the above-mentioned leveling step.

[0044] When the sample arrangement correction unit 4 is a ring, the diameter of the outermost edge is not limited, and may be larger or smaller than the outer diameter of the magnet in a plan view. In addition, the shape of the outermost edge of the ring is not limited, and may be circular, rectangular, or another shape in a plan view. In addition, there is no limit to the shape and size of the opening 4h of the ring, as described for the opening 4h of the sample arrangement correction unit 4.

[0045] In addition, the specific work content of the smoothing process may be to make the upper surface 4a of the sample placement correction section 4 flush (dashed line in Figure 5(a)) and repeat the process of smoothing to fit this upper surface 4a (Figure 5(a) → (b)).

[0046] The method for measuring the magnetic orientation using the sample holder 1 of this embodiment is as follows.

[0047] FIG. 6 is a schematic perspective view showing a state in which the container of the sample holder 1 of this embodiment is placed on the base portion 6. As shown in FIG.

[0048] The container of the sample holder 1 is placed on the base part 6. The placement must be such that the center of the X-ray irradiation part is at the center of the upper surface of the sample. The base part 6 may be a part of the X-ray diffraction measurement device.

[0049] a sample arrangement step of sprinkling a sample on the sample holder 1 of this embodiment and magnetically orienting the sample on the upper surface 3a of the stage portion 3 and within the opening 4h of the sample arrangement correction portion 4; a measuring step of performing X-ray diffraction measurement on the magnetically oriented sample and calculating the degree of magnetic orientation; has. Preferably, the method further includes the above-mentioned leveling step of leveling the particles protruding from the opening 4h of the sample positioning correction unit 4 to the upper surface 4a of the sample positioning correction unit 4 between the sample positioning step and the measurement step.

[0050] According to the magnetic orientation measuring method using the sample holder 1 of this embodiment, the magnetic orientation of a magnetic material powder can be evaluated by X-ray diffraction with high accuracy and high reproducibility.

[0051] The technical scope of the present invention is not limited to the present embodiment, but includes various modifications and improvements within the scope of the specific effects that can be obtained by the constituent elements of the invention and their combinations.

[0052] FIG. 7 is a schematic cross-sectional view of the modified sample holder after a sample placement step and a smoothing step have been carried out in that order.

[0053] In this embodiment, the sample arrangement correction unit 4 is a ring, but as shown in Fig. 7, a recess may be formed on the upper surface 3a of the stage unit 3 as the opening 4h of the sample arrangement correction unit 4, and a sample may be placed in this recess. That is, the opening 4h of the sample arrangement correction unit 4 may be formed by the upper surface 3a of the stage unit 3. Then, a magnet 2 may be placed on the lower surface 3b of the stage unit 3 in this recess, and the recessed portion of the stage unit 3 may be sandwiched between the magnet 2 to magnetically orient the sample. That is, the opening 4h in this specification includes both a through hole and a non-through hole.

[0054] FIG. 8(a) is a schematic cross-sectional view of a modified sample holder provided with a magnet holding portion 7 after a sample placement step and a leveling step have been carried out in that order. FIG. 8(b) is a schematic bottom view of a modified sample holder provided with a magnet holding portion 7. The white arrows in FIG. 8 indicate the directions in which magnet 2 is inserted and removed.

[0055] As shown in FIG. 8, as another example of a mode in which the magnet 2 is fixed to the inner surface of the bottom of the container, a magnet holder 7 may be provided on the inner surface of the bottom of the container.

[0056] In the modification shown in Fig. 8, a magnet holder 7 is provided so as to protrude downward from the inner surface of the bottom of the container. The magnet holder 7 may be separately attached to the inner surface of the bottom of the container. If the container is made of resin, the magnet holder 7 may be integrally molded with the container. The magnet holder 7 has an opening in the horizontal direction. By inserting the magnet 2 horizontally into the magnet holder 7 from the opening 71, the magnet 2 can be positioned on the inner surface of the bottom of the container. EXAMPLES

[0057] The present invention will be specifically described below using examples, but the present invention is not limited to the following examples in any way.

[0058] [Example 1] A powder sample A having magnetic properties was placed in the sample holder 1. The amount of powder sample A was 1 g. In the sample holder 1 of Example 1, the sample placement correction part 4 was a stainless steel ring. The inner diameter of the ring was 18 mm, the outer diameter was 30 mm, the width of the ring was 6 mm, and the height (thickness) of the ring was 1.5 mm. The magnet 2 was cylindrical with a height of 15 mm. The diameter of the cylinder of the magnet 2 was 20 mm, which was set larger than the inner diameter of the ring. Then, the magnet 2 and the ring were placed concentrically. After the smoothing process, an X-ray diffraction measurement result reflecting the magnetic orientation was obtained by an X-ray diffraction measurement device.

[0059] [Comparative Example 1] The sample holder 1 of this embodiment was not used, and a sample was placed on a simple glass sample holder 1 (without the magnet 2). Then, the X-ray diffraction measurement results were obtained in the same manner as in Example 1.

[0060] [Comparative Example 2] The sample holder 1 of this embodiment was used without the sample position correction unit 4 (that is, the one described in Patent Document 1). Then, the X-ray diffraction measurement results were obtained in the same manner as in Example 1.

[0061] [result] FIG. 9 is a graph showing the results of X-ray diffraction measurement for Example 1 and Comparative Example 1 (without using magnet 2).

[0062] 9, it was confirmed that there was no deviation in the 2θ direction between the diffraction peak positions of the X-ray diffraction measurement results of Comparative Example 1 and Example 1. The reason for this is that in Example 1, the sample placement correction unit 4 (ring) was present, suppressing the variation in the particles that constitute the powder sample A. In addition, the leveling process was performed, which allowed sufficient adjustment of the height alignment of the sample surface.

[0063] From the measurement results of FIG. 9 relating to Example 1 and Comparative Example 1, the results of calculating the degree of orientation were obtained using eight arbitrary diffraction peaks (FIG. 11).

[0064] Here, the degree of orientation was calculated as follows.

[0065] If the magnetic orientation degree of an arbitrary peak is K, the peak intensity of the arbitrary peak in the real sample is IPO(real sample), the sum of the peak intensities of all selected peaks in the real sample is IPS(real sample), the peak intensity of an arbitrary peak in a non-oriented state is IPO(non-oriented), and the sum of the peak intensities of all selected peaks in a non-oriented state is IPS(non-oriented), then the magnetic orientation degree K can be obtained by the following formula. K = {IPO (real sample) / IPS (real sample)} / {IPO (non-oriented) / IPS (non-oriented)}

[0066] In the case of Comparative Example 1, no magnetic orientation was confirmed. On the other hand, in the case of Example 1, X-ray diffraction measurement was possible in a state where powder sample A was magnetically oriented in a specific direction (C-axis direction). In addition, in the case of Example 1, the K value at the (006) peak was calculated to be high, and C-axis orientation was clearly indicated (FIG. 11).

[0067] 10 is a graph showing the results of X-ray diffraction measurement of Example 1 and Comparative Example 2 (without using the sample position correction unit 4 (ring)). Note that the graph of Example 1 in FIG. 10 is the same as the graph of Example 1 in FIG.

[0068] From the measurement results of FIG. 10 relating to Example 1 and Comparative Example 2, the results of calculating the degree of orientation were obtained using eight arbitrary diffraction peaks (FIG. 12).

[0069] There was a difference in the 2θ direction between the diffraction peak positions of the X-ray diffraction measurement results of Comparative Example 2 and Example 1. The reason for this is that the particles constituting Powder Sample A in Comparative Example 2 were varied.

[0070] The K value at the (006) peak was calculated to be higher in Example 1 than in Comparative Example 2. This is because the magnetic orientation of powder sample A in aperture 4h in Example 1 was more uniformly aligned, allowing the magnetic orientation to be measured correctly (FIG. 12). [Explanation of symbols]

[0071] 1. Sample holder 2. Magnets 3 Stage part (container) 3a (Top surface of stage) 3b (Stage) Bottom 4. Sample placement correction section (ring) 4a (Sample placement correction part) top surface 5. Sample 5a Particle aggregate in which multiple particles are connected vertically due to magnetic orientation 6 Base 7 Magnet holder 71 (Magnet holder) opening

Claims

1. A sample holder for holding a sample when measuring the magnetic orientation of the sample by X-ray diffraction. hand, a stage portion on whose upper surface a sample is placed; A magnet disposed on the underside of the stage portion; A test piece having an opening and arranged so that the side of the opening fits within the upper region of the magnet. A material placement correction unit, In plan view, the outline of the magnet is aligned with the opening so as not to come into contact with the outline of the magnet. It encompasses the area, In a plan view, the outline of the opening of the sample arrangement correction unit is disposed within a range of 0 to 2.0 mm from the outermost edge of the magnet toward the center, The opening depth of the sample arrangement correction unit is smaller than the maximum vertical length of a particle aggregate in a state in which a plurality of particles constituting the sample are vertically connected due to magnetic orientation associated with the arrangement of the magnets, The upper surface of the sample placement correction portion surrounding the opening is flush with the same height. Sample holder for magnetic orientation measurements.

2. the stage portion being formed by the outer surface of the bottom of the container; The magnet is fixed to the inner surface of the bottom of the container; The sample arrangement correction unit is ring-shaped and is disposed above the magnet with the stage unit interposed therebetween.

2. A sample holder for magnetic orientation measurement according to claim 1 .

3. a sample placement step of sprinkling a sample on the sample holder according to claim 1 or 2 to magnetically orient the sample on the upper surface of the stage portion and within the opening of the sample placement correction portion; and a measuring step of performing X-ray diffraction measurement on the magnetically oriented sample to calculate the degree of magnetic orientation.

4. The opening depth of the sample placement correction section is set so that the plurality of particles constituting the sample are aligned upwards due to their magnetic orientation. This is smaller than the maximum vertical length of the cluster of particles connected below. Between the sample placement step and the measurement step, particles protruding from the opening of the sample placement correction unit 4. The method for measuring magnetic orientation according to claim 3, further comprising a step of leveling the sample by aligning the probe with an upper surface of the sample arrangement correction portion.

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