JP2006071608A - Powder holder, measuring sample manufacturing method, and sample analysis method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a powder holder, measuring sample manufacturing method, and sample analysis method which can easily manufacture test samples, even for powder to achieve enhancement in the measuring efficiency, in the analysis requiring smoothness of sample surface. <P>SOLUTION: This powder holder comprises a base section and a powder-holding section provided to the base section, wherein the powder holding section has at least one powder storage hole for storing powder on the opposite side of its base section, and the hardness of the powder-holding section is smaller than the hardness of the base section. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a powder holder, a measurement sample manufacturing method, and a sample analysis method.

  In general, the analysis surface of a sample in EPMA (Electron Probe Microanalyzer, X-ray Microanalyzer) analysis or fluorescent X-ray analysis is required to be smooth. This is because if there are irregularities on the sample surface, the X-ray spectral conditions and the absorption process change, which affects the X-ray intensity.

  By the way, when the above analysis is performed on the powder, conventionally, the measurement sample is manufactured by pressing the powder using a predetermined jig in order to obtain the smoothness of the sample surface. For example, a powder sample was formed by a hand press or a hydraulic machine using a hard metal mold for forming tablets, and then the sample formed from the mold was taken out and used as a measurement sample. Further, as another method for producing a measurement sample from powder, there is also a method of polishing a cured product obtained by mixing a binder resin and powder and curing the mixture (for example, Non-Patent Document 1). reference).

Satoshi Uchiyama, Satoshi Watanabe, Shizuo Kimoto, "X-ray Microanalyzer 6th Edition", p. 95, Nikkan Kogyo Shimbun, August 30, 1975

  However, in the above-described conventional measurement sample manufacturing method, much labor and time are spent in manufacturing the measurement sample, and the measurement efficiency is not necessarily sufficient.

  The present invention provides a powder holder and a measurement sample manufacturing method capable of easily measuring a measurement sample even in the case of analysis requiring smoothness of the sample surface and improving measurement efficiency. It is another object of the present invention to provide a sample analysis method.

  In order to solve the above problems, a powder holder of the present invention includes a base part and a powder holding part provided on the base part, and the powder holding part is a powder holding part. It has at least one powder containing hole for containing powder on the side opposite to the base part, and the hardness of the powder holding part is smaller than the hardness of the base part.

  According to the powder holder of the present invention, after filling the powder containing hole with the powder, the base portion of the powder holding portion is deformed by pressing with a predetermined smooth surface on the side opposite to the base portion. Without changing the powder holding portion. As a result, the powder holding portion is deformed and the powder filled in the powder containing hole is also pressed with a smooth surface, so that a measurement sample having a smooth surface in the powder containing hole can be obtained. . The powder holder can be placed on the sample stage of the analyzer to perform measurement. Therefore, by using the powder holder, a measurement sample can be easily obtained from the powder, and measurement can be performed without taking out the measurement sample from the powder holder, so that the measurement efficiency can be improved. it can.

  In the powder holder of the present invention, it is preferable that the powder holding part has a plurality of powder containing holes for containing powder on the side opposite to the base part of the powder holding part. According to such a powder holder, after the powder is filled in each of the plurality of powder receiving holes, the opposite side of the powder holding portion from the base portion is pressed with a predetermined smooth surface, whereby the plurality of powders A measurement sample having a smooth surface in the accommodation hole can be obtained simultaneously. This can further improve the measurement efficiency when analyzing a large number of powders.

  Further, according to the above powder holder having a plurality of powder holding holes, after filling the powder holding holes with the powder, the side opposite to the base part of the powder holding part is smoothed. By applying pressure on the surface, the surface of the measurement sample obtained in the plurality of powder accommodating holes can be positioned on one surface. Thus, in an analyzer that needs to align the surface of the sample with the position of the predetermined three-dimensional coordinate, if the surface of one measurement sample is aligned with the position of the predetermined three-dimensional coordinate, The surface of the sample can be adjusted to the position of the predetermined three-dimensional coordinate only by movement in two dimensions. Accordingly, one-dimensional operation can be omitted in the operation for aligning the surface of the measurement sample with a predetermined coordinate position, and the measurement efficiency can be further improved.

  In addition, in the method of manufacturing a measurement sample using a conventional mold, since the powders are individually press-molded, it is not easy to make the thickness of a plurality of measurement samples constant. When arranging samples for use on a sample stage and sequentially measuring each sample, an operation for aligning the sample surface with a predetermined three-dimensional coordinate position is required for each measurement.

  Furthermore, in the powder holder of the present invention, the base portion has an annular marking surface that projects outward from the surface of the powder holding portion opposite to the base portion and surrounds the powder holding portion. The marking surface is preferably provided with at least one marking portion.

  Since the powder holder has a marking portion, the positional relationship between the marking portion and the powder accommodation hole can be obtained in advance. Therefore, after the powder holding hole is filled with powder, the side opposite to the base part of the powder holding part is pressed with a predetermined smooth surface, and the powder in which the measurement sample is obtained in the powder holding hole By confirming the marking part of the holder (hereinafter sometimes referred to as “sample holder for measurement”) in the analyzer and using this marking part as a reference point, Based on the positional relationship, the surface of each measurement sample can be adjusted to a predetermined coordinate position. Thereby, it becomes possible to further improve the measurement efficiency.

  Further, in the powder holder of the present invention, the base part and the powder holding part may be provided with alignment parts for aligning the powder accommodation holes at predetermined positions with respect to the marking part. preferable. By providing such an alignment portion, it is possible to more reliably obtain the positional relationship between the marking portion and the powder accommodating hole even when using a separately prepared base and powder holding portion. it can.

  Further, in the powder holder of the present invention, the base portion has a powder holding portion receiving recess for receiving the powder holding portion, and the powder holding portion is fitted into the powder holding portion receiving recess. It is preferable. According to such a powder holder, the powder holding part is firmly fixed to the base part. For this reason, after the powder holding hole is filled with powder, it is possible to suppress the powder holding portion from being displaced when pressurizing the side opposite to the base portion of the powder holding portion with a predetermined smooth surface. It becomes possible to more reliably obtain a measurement sample having a smooth surface in the powder containing hole.

  Moreover, it is preferable that the said powder holding | maintenance part accommodation recessed part provided in the said base part has the opening of the powder holding | maintenance part accommodation recessed part small toward the depth direction. If the powder holding portion receiving recess has such a shape, it becomes easy to extract the powder holding portion from the base portion, and the measurement sample holder after measurement is disassembled into the base portion and the powder holding portion. It will be easier to do. Thereby, when reusing a base part, the effort and time until a new powder holder is obtained combining with a new powder holding part can be reduced.

  Furthermore, it is preferable that the said base part has a through-hole connected with the said powder holding | maintenance part accommodation recessed part provided in the base part. By having such a through hole, in the measurement sample holder after the measurement, for example, a rod-shaped instrument can be inserted into the through hole and the powder holding part can be easily pushed out from the base part, It becomes easier to disassemble the measurement sample holder after the measurement into the base portion and the powder holding portion.

  Further, in the powder holder of the present invention, the base portion has a first slip prevention portion that prevents the base portion and the powder holding portion from slipping, and the powder holding portion is the first slip portion. It is preferable to have the 2nd slip prevention part which has a shape complementary to the prevention part. According to such a powder holder, when the powder holding hole is filled with powder, and the opposite side of the powder holding part to the base part is pressed with a predetermined smooth surface, the powder holding part becomes the base part. Therefore, it is possible to more reliably obtain a measurement sample having a smooth surface in the powder accommodation hole. Further, in the powder holder provided with the marking portion, the positional relationship between the marking portion and the powder containing hole can be determined more reliably.

  In addition, the measurement sample manufacturing method of the present invention includes a powder filling step of filling the powder holding hole of the powder holding portion with powder in the powder holder of the present invention, and a base of the powder holding portion. And a pressurizing step of obtaining a measurement sample in the powder accommodation hole by pressurizing the surface opposite to the portion with a smooth surface.

  According to the measurement sample manufacturing method of the present invention, it is possible to easily manufacture a measurement sample having a smooth surface from a powder as described above by using the powder holder of the present invention and passing through the above steps. it can. Thereby, the measurement efficiency of the analysis (especially elemental analysis using an EPMA analyzer) in which the smoothness of the sample surface is required can be improved.

  The first sample analysis method of the present invention is an X-ray generated from a measurement sample by irradiating the measurement sample obtained by the measurement sample manufacturing method of the present invention with an electron beam or X-ray as an incident ray. The sample for measurement is analyzed by detecting as an outgoing line. According to the sample analysis method of the present invention, since the measurement sample obtained by the measurement sample manufacturing method of the present invention has a smooth surface, the measurement obtained by the above-described conventional method by using this measurement sample. Compared to the case of using a sample for analysis, analysis with excellent measurement efficiency can be performed.

  Furthermore, in the first sample analysis method of the present invention, the measurement sample is analyzed by detecting the X-ray generated from the measurement sample with a spectroscopic crystal as an outgoing line. Is preferred. By separating X-rays with a spectral crystal, the energy resolution of the generated X-rays is improved, and the element identification accuracy is improved particularly when elemental analysis is performed. Even in such an analysis method, since the sample surface is required to be smooth, the measurement sample obtained by the above-described conventional method can be obtained by using the measurement sample obtained by the measurement sample production method of the present invention. Compared to the case of using, an analysis with further excellent measurement efficiency can be performed.

  In the second sample analysis method of the present invention, for each sample, the sample is irradiated with an electron beam or an X-ray as an incident line, and the X-ray generated from the sample is detected as an outgoing line. A sample analysis method for analyzing a plurality of samples, wherein, in the powder holder of the present invention described above, the powder holding part contains powder on the opposite side of the base part of the powder holding part A plurality of body-accommodating holes, and the base portion projects outwardly from the surface opposite to the base portion of the powder holding portion, and has an annular marking surface surrounding the powder holding portion, In the powder holder provided with at least one marking portion on the marking surface, a powder filling step for filling the powder holding hole of the powder holding portion with powder, and a base portion of the powder holding portion Pressurizing step to obtain a sample for measurement in the powder containing hole by pressurizing the opposite surface with a smooth surface An arrangement step of placing the measurement sample holder obtained by the including step on the sample stage, a reference point setting step for confirming the marking portion of the measurement sample holder as a reference point, and a reference point for each measurement sample Based on the predetermined positional relationship between the powder receiving hole and the marking portion, the surface of the measurement sample is aligned with the irradiation position of the electron beam or X-ray, and the electron beam or X-ray is irradiated as the incident beam. And a sample analysis step of detecting X-rays generated from the measurement sample as an outgoing line.

  According to the sample analysis method described above, the operation for aligning the surface of the measurement sample with a predetermined coordinate position as described above by using the powder holder of the present invention having a plurality of powder receiving holes. In this case, one-dimensional operation can be omitted. Furthermore, by using the powder holder of the present invention having a marking portion, if the marking portion is used as a reference point, each measurement sample is obtained on the basis of the positional relationship between the marking portion and the powder containing hole obtained in advance. It is possible to easily adjust the surface of the film to a predetermined coordinate position. Accordingly, the position of the marking portion is first confirmed, and then the surface of one measurement sample is aligned with the focus position (predetermined three-dimensional coordinate position) of the electron beam or X-ray to obtain another measurement sample. It is possible to adjust the surface of the material to the position of the predetermined three-dimensional coordinate by only two-dimensional movement based on the positional relationship between the marking portion and the powder accommodation hole obtained in advance. Thereby, the measurement efficiency for a plurality of samples can be greatly improved.

  According to the present invention, in the analysis where the smoothness of the sample surface is required, a measurement sample can be easily manufactured even if it is a powder, and a powder holder capable of improving the measurement efficiency, and the measurement sample manufacturing Methods and sample analysis methods can be provided.

  Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the description of the drawings, the same or corresponding elements are denoted by the same reference numerals, and redundant description is omitted. In addition, the dimensional ratio in each drawing does not necessarily match the actual dimensional ratio.

[Measurement sample manufacturing method]
First, an embodiment of the measurement sample manufacturing method of the present invention will be described.

  In the powder sample holder of the present invention, the measurement sample manufacturing method of the present embodiment is opposite to the powder filling step of filling powder in the powder holding hole of the powder holding portion and the base portion of the powder holding portion. And a pressing step of obtaining a measurement sample in the powder receiving hole by pressing the side surface with a smooth surface.

  Here, a first embodiment of the powder holder of the present invention used in the above-described measurement sample manufacturing method will be described.

  1-3 is a figure which shows 1st Embodiment of the powder holder of this invention. FIG. 1 is a schematic plan view showing a first embodiment of the powder holder of the present invention. 2 is a cross-sectional view taken along the line II-II in FIG. FIG. 3 is an exploded perspective view showing the first embodiment of the powder holder of the present invention. The powder holder 100 shown in FIGS. 1 to 3 includes a base portion 10 and a powder holding portion 20. The base unit 10 has a powder holding unit receiving recess 11 for storing the powder holding unit 20, and the powder holding unit receiving recess 11 is formed on one surface of the base unit 10. Here, both the base part 10 and the powder holding | maintenance part 20 are cylindrical. Further, the base portion 10 has an annular wall so as to protrude outward from the surface 20 a opposite to the base portion 10 of the powder holding portion 20 and to surround the powder holding portion receiving recess 11. . And the annular wall has the annular marking surface 12a so that the powder holding | maintenance part accommodation recessed part 11 may be surrounded. And the marking part 50 is provided on this marking surface 12a. Further, the powder holding unit 20 has powder accommodating holes 30 a to 30 i on the surface 20 a side of the powder holding unit 20. Furthermore, the positioning part 40 is provided in each of the base part 10 and the powder holding | maintenance part 20, and when manufacturing the sample for a measurement, by aligning both in a powder holder, the powder accommodating holes 30a- The positional relationship between 30i and the marking unit 50 can be determined.

  In the powder holder 100 of this embodiment, the hardness of the powder holding part 20 needs to be smaller than the hardness of the base part 10. Hereinafter, the configuration of the powder holder 100 will be described in detail.

(Base part)
The base part 10 only needs to have a hardness higher than that of the powder holding part 20, and the material is not particularly limited. In the powder holder of the present embodiment, when a pressurizing process described later is performed in a state where the powder holding unit 20 is disposed on the base unit 10, the powder holding unit 20 is deformed and the base It suffices if the portion 10 is not deformed. As a specific hardness, for example, the Brinell hardness (H _B ) of the base part 10 is preferably 150 or more. Here, “Brinell hardness (H _B )” in the present specification means a value obtained as follows. That is, when a steel ball having a diameter of 10 mm is pressed by applying a load of 3000 kg perpendicularly to the material surface, the value obtained by dividing the test load by the indentation surface area is defined as Brinell hardness (H _B ) (reference: “Chemical Handbook” ”Author: The Chemical Society of Japan, Publisher: Maruzen Co., Ltd., issued June 20, 1975).

  Examples of the material of the base unit 10 include stainless steel and carbon steel.

  The size of the base 10 is not particularly limited. For example, the diameter L1 shown in FIG. 1 is preferably 20 to 90 mm, and the thickness H1 shown in FIG. 2 is preferably 10 to 20 mm. . If the diameter L1 is in the above range, it can be more reliably placed on a sample stage such as a general EPMA analyzer, and the powder holding part can have a larger number of powder receiving holes. Moreover, if thickness H1 is said range, while being able to suppress the load to the sample stand of the analyzer by the weight increase of a base part, the intensity | strength of a base part can be ensured more reliably.

(Powder holding part)
The powder holding part 20 should just have the hardness smaller than the base part 10, and it does not specifically limit about a material. In the powder holder of the present embodiment, when the pressurizing process described later is performed in a state where the powder holding unit 20 is disposed on the base unit 10, the base unit 10 is not deformed and the powder is held. The part 20 may be plastically deformed. As specific hardness, for example, it is preferable that the Brinell hardness (H _B ) of the powder holding unit 20 is less than 80.

  Examples of the material of the powder holding unit 20 include Al, Pb, Zr, Cu, Sn, and alloys thereof.

  Although it does not specifically limit about the magnitude | size of the powder holding | maintenance part 20, For example, it is preferable that the diameter L2 shown by FIG. 1 is 10-70 mm, and the thickness H2 shown by FIG. 2 is 2-3 mm. preferable. If the diameter L2 is in the above range, a sufficient area of the marking surface 12a can be secured, and the powder holding portion can have a larger number of powder containing holes. In addition, when the thickness H2 is in the above range, the handleability of the powder holding unit is good, and the load on the sample stage of the analyzer due to the increase in the weight of the powder holding unit can be more reliably reduced. it can.

  Further, since the powder holding unit 20 is plastically deformed by pressurization, there may be a clearance H3 between the position of the surface of the powder holding unit 20 opposite to the base 10 and the position of the marking surface 12a. preferable. In the present embodiment, it is preferable that the clearance H3 is 0.5 to 1 mm. If there is a clearance H3 in such a range, the powder holding part 20 can be plastically deformed by pressurization to sufficiently smooth the surface of the measurement sample, and the powder holding part can be excessively deformed to form a powder. It is possible to prevent the opening position of the accommodation hole from being greatly displaced.

(Powder containing hole)
The size of the opening of the powder containing holes 30a to 30i is not particularly limited as long as a sufficient measurement region is ensured after the powder holding unit 20 is pressurized. In the powder holder 100 of this embodiment, it is preferable that the hole diameter of the opening of the powder containing holes 30a to 30i is 3 to 5 mm. If it is less than 3 mm, the opening area of the powder container hole becomes small due to the pressurization and measurement becomes difficult, or the position of the powder container hole shifts and the positional relationship between the marking part and the powder container hole changes. It tends to be. On the other hand, when the hole diameter of the opening exceeds 5 mm, a large amount of powder tends to be required.

  As for the number of the powder accommodation holes, the opening of the powder accommodation holes is crushed by the pressurizing process described later, and the measurement area cannot be secured, or the opening position of the powder accommodation holes is shifted and the marking portion and the powder accommodation It is preferable to set so that the positional relationship with the hole does not change significantly. In the powder holder 100 of this embodiment, it is preferable that the space | interval of powder accommodation holes is ensured 1 mm or more.

(Marking surface)
The marking surface 12a should just ensure the area for providing the marking part 50. FIG.

(Marking part)
Examples of the marking unit 50 include a mark provided so that it can be visually confirmed, and specifically, an X mark, a dot mark, and the like. In addition, when a plurality of marking portions are provided, it is preferable to change the shape so that each of the marking portions can be distinguished or to engrave a number in the vicinity. Further, when pressing the powder holding part with a smooth surface, a concave portion is formed on the marking surface 12a and a marking portion is provided on the bottom surface of the concave portion in order to prevent the marking portion from being crushed by the smooth surface and being unable to be confirmed. It may be done. Moreover, although the position where the marking part 50 is provided is not particularly limited, for example, the fact that each marking part 50 is evenly separated on the marking surface 12a can recognize the position of the powder containing hole more accurately. Is preferable.

(Positioning part)
The powder holder 100 shown in FIG. 1 has an alignment portion 40 provided on the base and the powder holding portion so that the marking portion 50 and the powder containing holes 30a to 30i are in a predetermined positional relationship. Are in a state of being combined with each other. Examples of the alignment portion include a mark provided so as to be visually confirmed as shown in FIG. 1, and specifically, a mark formed by marking.

  Next, a method for manufacturing a measurement sample using the powder holder 100, that is, a method for manufacturing a measurement sample holder will be described.

  FIG. 4 is a diagram for explaining an embodiment of the measurement sample manufacturing method of the present invention. 4A to 4D show a process of manufacturing a measurement sample (measurement sample holder) using the powder holder 100. FIG. FIG. 4A shows a cross-sectional view of the powder holder 100 taken along the line II-II in FIG. 1. Hereinafter, the measurement sample of the present invention will be described with reference to a portion corresponding to the cross-sectional view. An embodiment of the manufacturing method will be described in detail. In addition, although the method to manufacture the sample for a measurement using the said powder holder 100 is demonstrated here, this invention is not limited to this.

(Powder holder preparation process)
As shown in FIG. 4A, a powder holder preparation process for preparing the powder holder 100 described above is performed. At this time, the alignment portions 40 are preferably aligned with each other.

(Powder filling process)
Next, powder serving as a measurement sample is filled in each of the powder containing holes 30a to 30i (powder filling step). FIG. 4B shows a cross-sectional view of the powder holder 100 filled with powder (a cross section taken along the line II-II in FIG. 1). As shown in FIG. 4B, the surface of the powder (for example, 60d, 60e, 60f) filled in each powder accommodating hole is opposite to the base 10 of the powder holding unit 20, as shown in FIG. It is preferable to fill the surface 20a (hereinafter referred to as “surface to be pressed”) so as to be aligned. At this time, for example, if the powder is a mixture of raw materials such as ceramic (metal oxide, etc.), the powder is filled so as to be 50 to 70% of the theoretical density of the ceramic formed from the raw materials. Is preferred.

(Pressure process)
Next, the powder holder 100 filled with the powder is placed on the base jig 90, and the pressed surface 20a of the powder holding unit 20 is pressed with the pressing jig 70 having the smooth surface 80, thereby storing the powder. A measurement sample is obtained in the holes 30a to 30i (pressurization step) (FIG. 4C). This pressurizing step can be performed using, for example, a general mechanical or manual hydraulic press.

  The measurement samples 62d, 62e, and 62f (see FIG. 4D) are placed in the powder receiving holes 30a to 30i of the powder holding unit 21 that has been deformed as shown in FIG. Is obtained. That is, the measurement sample holder 101 having the measurement sample is manufactured.

  As described above, when the powder holder 100 of the present embodiment is used, the powder receiving holes 30a to 30i are filled with powder, and then the pressed surface 20a of the powder holding unit 20 is pressed with the smooth surface 80. Thereby, the powder holding part 20 can be deformed without deforming the base part 10. Thereby, as the powder holding part 20 is deformed, the powder filled in the powder accommodation holes 30a to 30i is also pressed with a smooth surface, so that the measurement has a smooth surface in the powder accommodation holes 30a to 30i. A plurality of samples can be obtained simultaneously. Then, the obtained measurement sample holder 101 can be placed on the sample stage of the analyzer to perform measurement. Therefore, by using the powder holder 100 of the present embodiment, a measurement sample can be easily obtained from the powder, and measurement can be performed without taking out the measurement sample from the powder holder. Can be improved.

  The smooth surface 80 of the pressing jig 70 preferably has an arithmetic average roughness Ra of 1 μm or less. Here, the arithmetic average roughness Ra is an arithmetic average roughness Ra defined by JIS-B-0601-1994. By pressurizing the powder holding part 20 with the pressing jig 70 having such a smooth surface, sufficient smoothness can be imparted to the surface of the measurement sample obtained in each powder accommodating hole.

  Further, the arithmetic average roughness Ra of the surface of the measurement sample obtained in each powder accommodating hole by the pressurizing step is preferably 5 μm or less, more preferably 3 μm or less, and more preferably 1 μm or less. More preferably. By setting the arithmetic average roughness Ra of the surface of the measurement sample to 5 μm or less, for example, in elemental analysis using an EPMA analyzer, measurement accuracy can be further improved.

In addition, when the powder holding unit 20 is pressed and deformed, the powder is applied while the smooth surface 80 of the pressing jig 70 and the surface 92 of the base jig 90 contacting the base part 10 are opposed in parallel. It is preferable to pressurize the holding unit 20. In the present invention, the surface of the measurement sample (for example, sample surfaces 65d, 65e and 65f shown in FIG. 4 (d)) obtained in each of the powder accommodating holes 30a to 30i after the pressurizing step, The difference between the maximum value and the minimum value of the distance (for example, L _d , L _e , L _f shown in FIG. 4D) with the surface 92 that contacts the base portion 10 of the tool 90 is set to 5 μm or less. The thickness is preferably 3 μm or less, more preferably 1 μm or less. When the difference between the maximum value and the minimum value is 5 μm or less, the measurement efficiency can be improved more reliably in the sample analysis method for a plurality of samples described later.

  In addition, since the powder holding unit 20 is plastically deformed by the pressing jig 70 in the pressing step, the hardness of the pressing jig 70 is preferably larger than the hardness of the powder holding unit 20. In the measurement sample manufacturing method of the present invention, it is possible to use a pressurizing jig 70 made of the same material as that of the base part 10, so that the shape of the base part 10 (particularly, the shape of the powder holding part receiving concave part and the marking surface). ) From the viewpoint of protection.

The pressurizing pressure depends on the material of the powder holding unit 20, the degree to which the powder holding unit 20 is deformed, and the type of powder. For example, the powder holding unit 20 is made of aluminum. When the thickness of the powder holding part is reduced by 0.5 to 1 mm by pressurization and a measurement sample is obtained from powder mixed with raw materials such as ceramic (metal oxide or the like), the pressure is 600 to 1000 kg / cm ^2. Is preferred. The pressing time is preferably set as appropriate depending on the properties of the powder. For example, when a powder mixed with a raw material (metal oxide or the like) such as ceramic is used as a sample, the above pressure is set to 30. A sample for measurement can be obtained by pressurizing for ~ 90 seconds.

[Sample analysis method]
Next, the sample analysis method of the present invention will be described.

  As one embodiment of the sample analysis method of the present invention, a sample for sequentially performing elemental analysis by an EPMA analyzer on a plurality of measurement samples included in the measurement sample holder 101 obtained using the powder holder 100 described above The analysis method will be described.

  First, an EPMA analyzer used in the sample analysis method of this embodiment will be described. FIG. 5 is a schematic configuration diagram showing the configuration of the EPMA analyzer. The EPMA analyzer shown in FIG. 5 includes an electron gun E, a sample stage T, a driving device M, a spectral crystal AC, a detector D, and a control unit C. In the present embodiment, a WDS (Wave Dpersive Spectroscopy) is used as the detector D. The control unit C is electrically connected to the driving device M, can control the driving device M to move the sample stage T to a predetermined position, and can read the position of the sample stage T. . Further, the control unit C performs elemental analysis by controlling the electron gun E, the spectral crystal AC, and the detector D based on a predetermined program. In the elemental analysis, the surface of the sample S1 placed on the sample stage T is irradiated with the electron beam L, the X-rays generated from the sample S1 are separated by the spectral crystal AC, and the spectrum is detected by the detector D. Is done. Here, when the angle α between the X-ray guided to the spectroscopic crystal set at a predetermined position and the sample surface changes, it is detected as different data. Therefore, in elemental analysis using an EPMA analyzer, the sample surface is measured at the beginning of the measurement. Must be adjusted to a predetermined position (focus position of the electron beam). Therefore, when analyzing a plurality of samples, it is necessary to align the sample surface with a predetermined position (focus position of the electron beam) for each measurement. Hereinafter, the sample analysis method of this embodiment will be described.

(Step 1)
The measurement sample (measurement sample holder 101) obtained by the measurement sample manufacturing method of the present embodiment described above is placed on the sample stage T of the analyzer (placement step).

(Step 2)
Next, the control unit C stores data indicating the positional relationship between the marking unit 50 and the powder storage holes 30a to 30i of the powder holder 100. For example, data represented by two-dimensional coordinates can be used as shown in FIG. The coordinates shown in FIG. 6A are represented by values obtained by projecting the position of the powder accommodation hole onto the surface on which the powder holder 100 is placed. In the analyzer, the surface on which the powder holder 100 is placed, that is, the surface of the sample table T is adjusted so as to be orthogonal to the incident line.

(Step 3)
Next, the marking portion 50 of the measurement sample holder 101 arranged on the sample stage T is confirmed with a visible microscope, SEM, etc., and the position of the marking portion 50 at this time is shown in a reference point (FIG. 6B). 0, 0, 0)) is stored in the control unit C (reference point setting step). Further, the control unit C sets a straight line passing through the reference point and parallel to the incident line as the Z axis, a plane passing through the reference point and having the incident line as a normal line as an XY plane, and further sets the X axis in a predetermined direction. Set to.

(Step 4)
Next, the sample stage T is moved so that the surface of the measurement sample in the powder containing hole 30a is aligned with the incident region of the electron beam. At this time, the position of the measurement sample surface of the powder containing hole 30a in the EPMA apparatus is recognized as (X _a , Y _a , Z _a ) based on the position of the sample stage T. Further, the sample stage T is moved in the Z-axis direction so that the electron beam is focused on the surface of the measurement sample in the powder containing hole 30a. The Z coordinate when the electron beam is in focus is _ZFP , and this coordinate is set as the Z coordinate during EPMA measurement. The control unit C recognizes coordinates (X _a , Y _a , Z _FP ) corresponding to the powder accommodation hole 30a as an appropriate position of the sample stage T when measuring the measurement sample in the powder accommodation hole 30a. Let Here, in the measurement sample holder 101 obtained by the measurement sample manufacturing method of the present embodiment described above, the measurement sample surface of the powder accommodation hole 30a and the measurement samples of the other powder accommodation holes 30b to 30i. The surfaces of are located on the same plane. Furthermore, this surface is parallel to the surface of the sample stage T. Thus, Z coordinates corresponding to the surface of the measurement sample other powder container hole 30b~30i also has a _{Z FP.} At this time, the control unit C can also recognize the X and Y coordinates corresponding to the surface of the measurement sample in the powder containing holes 30b to 30i. This will be described below.

As shown in FIG. 6 (a), the coordinate data indicating the positions of the powder receiving holes 30a to 30i with respect to the marking portion 50, which is the reference point, is the powder containing holes 30a (X _a0 , Y _a0 ), The body accommodation holes 30b are (X _b0 , Y _b0 ),... And the powder accommodation holes 30i are obtained in advance such as (X _i0 , Y _i0 ). This data is stored in the control unit C in step 2 above. ing. In the EPMA apparatus, as described above, the coordinates corresponding to the powder accommodating hole 30a are (X _a , Y _a ) with respect to the XY coordinates (0, 0) of the marking portion 50 which is the reference point. Here, since the measurement sample holder 101 is usually freely arranged on the sample stage T, (X _a , Y _a ) and (X _a0 , Y _a0 ) often do not match. This shift in coordinates is derived from the rotation of the measurement sample holder 101. Therefore, the control unit C calculates the rotation angle based on the values of (X _a , Y _a ) and (X _a0 , Y _a0 ), and corrects the rotation of this angle for the other powder containing holes 30b to 30i. This is performed for the coordinates ( _Xb0 , _Yb0 ) to ( _Xi0 , _Yi0 ). As a result, coordinates (X _b , Y _b , Z _FP) corresponding to the powder receiving holes 30b to 30i are used as appropriate positions of the sample stage T when measuring the measurement samples in the powder receiving holes 30b to 30i. ) To (X _i , Y _i , Z _FP ) are recognized by the control unit C (see FIG. 6C). In this way, the control unit C does not check the surface of the measurement sample in the powder containing holes 30b to 30i with a visible microscope or SEM, and the control unit C measures the sample receiving hole 30b to 30i. As an accurate position, the X and Y coordinates corresponding to each powder accommodating hole and the focal position _ZFP of the electron beam are recognized. In addition, from the viewpoint of more accurately correcting the position of the powder accommodation holes 30b to 30i described above, when the surface of the measurement sample in the powder accommodation hole 30a is aligned with the focal position of the electron beam, It is preferable to use a place as close as possible to the center of the opening, and set the position at this time to the coordinates (X _a , Y _a , Z _FP ) corresponding to the powder containing hole 30a.

(Step 5)
Next, as the measurement order of the measurement samples in the powder accommodation holes 30a to 30i, the powder accommodation holes to be measured corresponding to the order are input to the control unit C. For example, the powder receiving hole 30a is input as the first measurement sample, the powder storage hole 30b is input as the second measurement sample, and the powder storage hole 30i is input as the ninth measurement sample.

(Step 6)
The powder accommodation hole 30a to be measured first is irradiated with an electron beam L from the electron gun E under the control of the control unit C, and the X-rays generated from the powder accommodation hole 30a are dispersed by the spectral crystal AC. Spectroscopy is detected by detector D and elemental analysis is performed.

(Step 7)
When the elemental analysis of the measurement sample in the powder containing hole 30a is completed, the control unit C controls the driving device M to control the sample stage T and the coordinates (X corresponding to the measurement position of the powder containing hole 30b to be measured next. _b , Y _b , Z _FP ) to adjust the surface of the measurement sample in the powder containing hole 30b to the focal position of the electron beam.

(Step 8)
Next, the powder container hole 30b is irradiated with an electron beam L from the electron gun E under the control of the control unit C, and the X-ray generated from the powder container hole 30b is dispersed by the spectral crystal AC. It is detected by the detector D and elemental analysis is performed.

(Step 9)
When the elemental analysis of the measurement sample in the powder containing hole 30b is completed, the control unit C further repeats Step 7 and Step 8 for the remaining measurement samples based on the order input in Step 5, Elemental analysis of the measurement sample is performed (the above steps 6 to 9 are sample analysis steps).

  As described above, by using the measurement sample holder 101 obtained by the measurement sample manufacturing method of the above-described embodiment, the surfaces of the measurement samples obtained in the plurality of powder containing holes 30a to 30i are obtained. If it can be located on one surface and the marking part 50 is used as a reference point, based on the positional relationship (FIG. 6A) between the marking part 50 and the powder accommodating holes 30a to 30i obtained in advance. It is easy to match the surface of each measurement sample to a predetermined coordinate position. That is, as described above, if the position of the marking unit 50 is confirmed and the surface of one measurement sample is aligned with the focal position of the electron beam, the control unit C can automatically measure a plurality of samples. Measurement efficiency can be greatly improved.

  Next, a second embodiment of the powder holder according to the present invention will be described. In addition, the same code | symbol is attached | subjected about the component same or equivalent to 1st Embodiment, and the overlapping description is abbreviate | omitted. In addition, the dimensional ratio in each drawing does not necessarily match the actual dimensional ratio.

  7-9 is a figure which shows 2nd Embodiment of the powder holder of this invention. FIG. 7 is a schematic plan view showing a second embodiment of the powder holder of the present invention. 8 is a cross-sectional view taken along line VIII-VIII in FIG. FIG. 9 is an exploded perspective view showing a second embodiment of the powder holder of the present invention. 7-9, the cylindrical powder holding | maintenance part 20 has the convex part 42 as a 1st slip prevention part in the outer periphery, and the base part 10 is powder holding | maintenance. The powder of the first embodiment in that the inner wall of the part receiving recess 11 has a recess 41 as a second shift prevention part, having a shape complementary to the convex part 42 as the first shift prevention part. Different from the body holder 100. Here, the convex portion 42 is fitted into the concave portion 41.

  According to the powder holder 110 described above, the powder holding unit 20 is placed in the powder holding unit accommodating recess 11 of the base unit 10 so that the first deviation preventing unit 42 and the second deviation preventing unit 41 are fitted. The marking portion 50 and the powder containing holes 30a to 30i can be in a predetermined positional relationship, and the above-described alignment portion can be omitted. In addition, the powder holding unit 20 is firmly fixed to the base unit 10 by the first shift preventing unit 42 and the second shift preventing unit 41. Thereby, also in the said pressurization process, the shift | offset | difference of the base part 10 and the powder holding | maintenance part 20 can be suppressed more reliably, and, thereby, the measurement which has a smooth surface in the powder accommodating holes 30a-30i The sample for use can be obtained more reliably. In the powder holder 110, the first deviation preventing part may be a concave part and the second deviation preventing part may be a convex part. Further, the shapes and positions of the first shift prevention unit 42 and the second shift prevention unit 41 are not particularly limited as long as the above effects can be obtained.

  Next, a third embodiment of the powder holder according to the present invention will be described. In addition, the same code | symbol is attached | subjected about the component same or equivalent to 1st Embodiment, and the overlapping description is abbreviate | omitted. In addition, the dimensional ratio in each drawing does not necessarily match the actual dimensional ratio.

  FIGS. 10-12 is a figure which shows 3rd Embodiment of the powder holder of this invention. FIG. 10 is a schematic plan view showing a third embodiment of the powder holder of the present invention. FIG. 11 is a cross-sectional view taken along line XI-XI in FIG. FIG. 12 is an exploded perspective view showing a third embodiment of the powder holder of the present invention. The powder holder 120 shown in FIGS. 10 to 12 is different from the powder holder 110 in terms of the positions of the first shift prevention unit and the second shift prevention unit. That is, in the powder holder 120, the powder holding unit 20 has a convex portion 43 as a first deviation prevention unit on the base 10 side of the powder holding unit 20, that is, on the side opposite to the pressed surface 20 a. The base portion 10 has a concave portion 44 as a second deviation prevention portion having a shape complementary to the first deviation prevention portion 43 on the bottom surface 11a of the powder holding portion accommodating depression 11. Here, the convex portion 43 is fitted into the concave portion 44. Also in this powder holder 120, as in the powder holder 110 shown in FIGS. 7 to 9, the base part 10 is attached so that the first deviation prevention part 43 and the second deviation prevention part 44 are fitted. By fitting the powder holding unit 20, the marking unit 50 and the powder containing holes 30 a to 30 i can be in a predetermined positional relationship, and the above positioning unit can be omitted. In addition, the powder holding unit 20 is firmly fixed to the base unit 10 by the first shift prevention unit 43 and the second shift prevention unit 44. Thereby, also in the said pressurization process, the shift | offset | difference of the base part 10 and the powder holding | maintenance part 20 can be suppressed more reliably, and, thereby, the measurement which has a smooth surface in the powder accommodating holes 30a-30i The sample for use can be obtained more reliably. In the powder holder 120, the first deviation preventing part may be a concave part and the second deviation preventing part may be a convex part. Further, the shapes and positions of the first shift prevention unit 43 and the second shift prevention unit 44 are not particularly limited as long as the above effects can be obtained.

  13 and 14 are views showing a fourth embodiment of the powder holder of the present invention. FIG. 13 is a schematic plan view showing a fourth embodiment of the powder holder of the present invention, and FIG. 14 is an exploded perspective view showing the fourth embodiment of the powder holder of the present invention. The powder holder 130 shown in FIGS. 13 and 14 is different from the powder holder 100 in that a part of the outer peripheral surface of the powder holding unit 20 is a flat surface 13. Further, the base part 10 has a powder holding part accommodating recess 11 b having a shape complementary to the shape of the powder holding part 20 on one surface of the base part 10. The powder holding unit 20 is fitted in the powder holding unit accommodating recess of the base unit 10.

  In the powder holder 130 shown in FIGS. 13 and 14, since the powder holding unit 20 is fitted into the base unit 10, the rotation of the powder holding unit 20 is limited in the powder holding unit receiving recess 11b. Has been. Accordingly, the marking unit 50 and the powder containing holes 30a to 30i can be easily positioned at predetermined positions without the above-described alignment unit included in the powder holder 100 or the shift prevention unit included in the powder holders 110 and 120. Thus, the measurement efficiency can be improved in the analysis of the plurality of samples. Further, according to the powder holder 130, the powder holding part 20 is firmly fixed to the base part 10, so that the deviation between the base part 10 and the powder holding part 20 is further reduced in the pressurizing step. It can suppress reliably, and, thereby, the measurement sample which has a smooth surface in powder accommodating hole 30a-30i can be obtained more reliably.

  FIGS. 15-17 is a figure which shows 5th Embodiment of the powder holder of this invention. FIG. 15 is a schematic plan view showing a fifth embodiment of the powder holder of the present invention. 16 is a cross-sectional view taken along line XVI-XVI in FIG. FIG. 17 is an exploded perspective view showing a fifth embodiment of the powder holder of the present invention. The powder holder 140 shown in FIGS. 15 to 17 is different from the powder holder 100 in that the opening of the powder holding portion accommodating recess 11c is smaller in the depth direction. Further, in the powder holding part 20, the base part 10 side of the powder holding part 20 has a shape complementary to the shape of the powder holding part accommodating recess 11c. If the powder holding portion accommodating recess 11c has such a shape, it becomes easy to extract the powder holding portion 20 from the base portion 10, and the measurement sample holder that has finished the measurement is held with the base portion 10 and the powder holding portion. It becomes easier to disassemble into parts 20. Thereby, when reusing a base part, the effort and time until a new powder holder is obtained combining with a new powder holding part can be reduced. The shape of the powder holding portion accommodating recess 11c is not limited to the shape shown in FIGS. 16 and 17 as long as the powder holding portion 20 can be easily extracted from the base portion 10.

  18-20 is a figure which shows 6th Embodiment of the powder holder of this invention. FIG. 18 is a schematic plan view showing a sixth embodiment of the powder holder of the present invention. 19 is a cross-sectional view taken along the line XIX-XIX in FIG. FIG. 20 is an exploded perspective view showing a sixth embodiment of the powder holder of the present invention. A powder holder 150 shown in FIGS. 18 to 20 is different from the powder holder 100 in that the base part 10 has a through hole 52 connected to the powder holding part accommodating recess 11. The through hole 52 communicates from the surface of the base 10 opposite to the powder holding portion receiving recess 11, that is, from the bottom surface 53 of the base 10 to the bottom surface 54 of the powder holding portion receiving recess 11. By having such a through-hole 52, in the measurement sample holder after the measurement, for example, a rod-shaped instrument is inserted into the through-hole 52 and the powder holding unit 20 is easily pushed out from the base unit 10. This makes it easier to disassemble the measurement sample holder that has been measured into the base 10 and the powder holding unit 20. Thereby, when reusing a base part, the effort and time until a new powder holder is obtained combining with a new powder holding part can be reduced.

  21-23 is a figure which shows 7th Embodiment of the powder holder of this invention. FIG. 21 is a schematic plan view showing a seventh embodiment of the powder holder of the present invention. 22 is a cross-sectional view taken along line XXII-XXII in FIG. FIG. 23 is an exploded perspective view showing a seventh embodiment of the powder holder of the present invention. The powder holder 160 shown in FIGS. 21 to 23 is different from the powder holder 140 in that the base portion 10 has a through hole 52 connected to the powder holding portion accommodating recess 11c. The through hole 52 communicates from the outer peripheral wall 55 of the base portion 10 to the inner peripheral wall 56 of the powder holding portion accommodating recess 11c. By having such a through-hole 52, in the measurement sample holder after the measurement, for example, a rod-shaped instrument is inserted into the through-hole 52 and the powder holding unit 20 is easily pushed out from the base unit 10. This makes it easier to disassemble the measurement sample holder that has been measured into the base 10 and the powder holding unit 20. Thereby, when reusing a base part, the effort and time until a new powder holder is obtained combining with a new powder holding part can be reduced.

  The size of the through hole 52 is not particularly limited as long as, for example, a rod-like tool can be inserted into the through hole and the powder holding unit can be pushed out from the base unit. Further, the position of the through hole 52 is not particularly limited to the position shown in FIGS. 19 and 20 and FIGS. 22 and 23.

  As mentioned above, although embodiment of this invention was described, this invention is not limited to the said embodiment. For example, the shape of the base portion 10 is not limited to a cylinder having a powder holding portion accommodation recess, but may be a quadrangular column having a powder holding portion accommodation recess or other shapes. Further, the shape of the powder holding unit 20 is not limited to a cylindrical shape, and may be a quadrangular prism or other shapes. Further, the opening shape of the powder containing holes 30a to 30i can be a square or other shapes other than the circular shape. Further, the powder containing hole may be a hole penetrating the powder holding part or a non-through hole.

  The measurement sample manufacturing method according to the present invention is not limited to the above-described embodiment, and various modifications are possible. For example, the pressing jig 70 shown in FIG. 4C has a shape protruding outward from the pressed surface 20a of the powder holding unit 20, but the pressed surface 20a has the shape. A combined male pressurizing jig can be used instead. In this case, the degree of deformation of the powder holding unit 20 is not limited to the clearance H3 shown in FIG.

  The sample analysis method according to the present invention is not limited to the above-described embodiment, and various modifications can be made. For example, in the above embodiment, the above steps 2 and 5 can be performed before step 1. In addition, when using a powder holder provided with two marking portions, the rotation of the sample holder for measurement can be corrected by checking the position of each marking portion in the analyzer. Even if the surface of the measurement sample 30a is not aligned with the irradiation region of the electron beam, the XY coordinates in the apparatus corresponding to the measurement sample surfaces of all the powder receiving holes 30a to 30i can be calculated.

Further, in the above embodiment, the measurement sample manufactured by the measurement sample manufacturing method of the present invention is used for elemental analysis by the EPMA apparatus. In addition to this, an electron beam or X It can be used in a method of analyzing a sample by irradiating a line and detecting the generated X-ray as an outgoing line. For example, an analysis using an electron beam as an incident ray includes, for example, an analysis using an EPMA device, and an analysis using an X-ray as an incident ray includes, for example, an analysis using a fluorescent X-ray analyzer. Moreover, as a detector for detecting the generated X-ray, EDS (Energy Dispersive Spectroscopy) or the like can be used in addition to WDS. In addition, the sample analysis method of the present invention may be a method of analyzing a sample by irradiating a measurement sample manufactured by the measurement sample manufacturing method of the present invention with a laser as an incident line. An example is Laser Ablation ICP-MS analysis.

FIG. 1 is a schematic plan view showing a first embodiment of the powder holder of the present invention. FIG. 2 is a cross-sectional view taken along the line II-II in FIG. FIG. 3 is an exploded perspective view showing the first embodiment of the powder holder of the present invention. FIG. 4 is a diagram for explaining an embodiment of the measurement sample manufacturing method of the present invention. FIG. 5 is a schematic configuration diagram showing a configuration of an EPMA analyzer for explaining an embodiment of the sample analysis method of the present invention. FIG. 6 is a plan view of a powder holder for explaining an embodiment of the measurement sample manufacturing method of the present invention. FIG. 7 is a view showing a second embodiment of the powder holder of the present invention. 8 is a cross-sectional view taken along line VIII-VIII in FIG. FIG. 9 is an exploded perspective view showing a second embodiment of the powder holder of the present invention. FIG. 10 is a schematic plan view showing a third embodiment of the powder holder of the present invention. 11 is a cross-sectional view taken along line XI-XI in FIG. FIG. 12 is an exploded perspective view showing a third embodiment of the powder holder of the present invention. FIG. 13 is a schematic plan view showing a fourth embodiment of the powder holder of the present invention. FIG. 14 is an exploded perspective view showing a fourth embodiment of the powder holder of the present invention. FIG. 15 is a schematic plan view showing a fifth embodiment of the powder holder of the present invention. 16 is a cross-sectional view taken along line XVI-XVI in FIG. FIG. 17 is an exploded perspective view showing a fifth embodiment of the powder holder of the present invention. FIG. 18 is a schematic plan view showing a sixth embodiment of the powder holder of the present invention. 19 is a cross-sectional view taken along the line XIX-XIX in FIG. FIG. 20 is an exploded perspective view showing a sixth embodiment of the powder holder of the present invention. FIG. 21 is a schematic plan view showing a seventh embodiment of the powder holder of the present invention. 22 is a cross-sectional view taken along line XXII-XXII in FIG. FIG. 23 is an exploded perspective view showing a seventh embodiment of the powder holder of the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 ... Base part, 11, 11b, 11c ... Powder holding part accommodation recessed part, 12a ... Marking surface, 20 ... Powder holding part, 30a-30i ... Powder accommodation hole, 40 ... Positioning part, 42, 43 ... First deviation prevention part, 41, 44 ... second deviation prevention part, 50 ... marking part, 52 ... through hole, 60d, 60e, 60f ... powder surface, 62d, 62e, 62f ... measurement sample, 65d , 65e, 65f ... sample surface, 70 ... pressurizing jig, 80 ... smooth surface, 90 ... base jig, 100 ... powder holder, 101 ... sample holder for measurement, 110, 120, 130, 140, 150, 160: Powder holder.

Claims (12)

A base part, and a powder holding part provided on the base part,
The powder holding part has at least one powder containing hole for containing powder on the opposite side of the base part of the powder holding part;
The powder holder whose hardness of the said powder holding part is smaller than the hardness of the said base part. 2. The powder holder according to claim 1, wherein the powder holding part has a plurality of powder containing holes for containing powder on a side opposite to the base part of the powder holding part. The base portion has an annular marking surface that protrudes outward from the surface of the powder holding portion opposite to the base portion and surrounds the powder holding portion, and the marking surface includes The powder holder according to claim 2, wherein at least one marking portion is provided. The powder holder according to claim 3, wherein an alignment portion that aligns the powder containing hole with a predetermined position with respect to the marking portion is provided in the base portion and the powder holding portion, respectively. . The said base part has a powder holding part accommodation recessed part which accommodates the said powder holding part, and the said powder holding part is engage | inserted by this powder holding part accommodation recessed part. 2. The powder holder according to item 1. 6. The powder holder according to claim 5, wherein the powder holding portion accommodating recess of the base portion has an opening of the powder holding portion accommodating recess that decreases in the depth direction. The powder holder according to claim 5 or 6, wherein the base portion has a through-hole connected to the powder holding portion accommodating recess provided in the base portion. The base portion has a first slip prevention portion that prevents the base portion and the powder holding portion from slipping, and the powder holding portion is complementary to the first slip prevention portion. The powder holder of any one of Claims 1-7 which has a 2nd slip prevention part which has a shape. In the powder holder according to any one of claims 1 to 8, a powder filling step of filling the powder holding hole of the powder holding portion with powder,
A pressurizing step of obtaining a measurement sample in the powder accommodating hole by pressurizing the surface of the powder holding portion opposite to the base portion with a smooth surface;
A method for producing a sample for measurement, comprising: The measurement sample obtained by the measurement sample production method according to claim 9 is irradiated with an electron beam or an X-ray as an incident ray, and the X-ray generated from the measurement sample is detected as an outgoing ray, thereby A sample analysis method for analyzing a measurement sample. The sample analysis method according to claim 10, wherein the measurement sample is analyzed by detecting X-rays obtained by further analyzing X-rays generated from the measurement sample with a spectral crystal as the outgoing rays. A sample analysis method for analyzing a plurality of samples by irradiating the sample with an electron beam or an X-ray as an incident ray and detecting an X-ray generated from the sample as an outgoing ray for each sample. Because
The powder holder according to claim 3, wherein a powder filling step of filling the powder holding hole of the powder holding portion with powder, and a surface of the powder holding portion on the opposite side of the base portion. Placing the measurement sample holder obtained by the process including the pressurization process of obtaining the measurement sample in the powder accommodating hole by pressurizing with a smooth surface on the sample stage,
A reference point setting step for confirming the marking portion of the measurement sample holder and setting it as a reference point;
For each measurement sample, the surface of the measurement sample is set to the irradiation position of the electron beam or X-ray based on the reference point and the predetermined positional relationship between the powder receiving hole and the marking portion. In addition, a sample analysis step of irradiating an electron beam or an X-ray as an incident ray and detecting an X-ray generated from the measurement sample as an outgoing ray;
A sample analysis method.

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