Powder sample holder, method of manufacturing the same, powder sample holder set, and powder x-ray diffraction measurement method

Abstract

To provide a powder sample holder which offers an antistatic feature and superior scratch resistance, a method of manufacturing the same, a powder sample holder set comprising the powder sample holder and a leveling member with an antistatic feature and superior scratch resistance, and a powder x-ray diffraction measurement method using the powder sample holder.SOLUTION: A powder sample holder to be filled with a powder sample used in powder x-ray diffraction measurement and a method of manufacturing the same are provided, the powder sample holder having a recess with a bottom surface and a side surface provided on a main surface thereof, where a diamond-like carbon film is provided on the main surface of the powder sample holder and the side surface of the recess.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a powder sample holder used in a powder X-ray diffraction measurement method and a manufacturing method thereof, a powder sample holder set, a powder X-ray diffraction measurement method, a powder sample holder set, and a powder X-ray diffraction measurement method using the powder sample holder. [Background technology]

[0002] In powder X-ray diffraction measurements, a sealed tube or rotating anticathode type X-ray tube is used as the X-ray source, and the crystalline state (composition, structure, etc.) of the compounds contained in the sample can be evaluated by using the pseudo-focusing method or the reflection method using a parallel beam system depending on the sample form, such as powder, lump, plate, or flake. In the pseudo-focusing method, the X-ray tube, the height position of the sample surface, and the detector that detects the X-rays diffracted by the sample are placed on a virtual circumference called the focusing circle. It is important to accurately position the height position of the sample surface on the focusing circle.

[0003] In response to the above-mentioned request, the applicant has disclosed in Patent Document 1 a sample holder consisting of a plate having a through hole, an organic film attached to one side of the plate with an adhesive so as to cover the through hole, and a thin collodion film attached to the inner surface of the organic film so as to fix a powder sample.

[0004] On the other hand, in powder X-ray diffraction measurements using the pseudo-focusing reflection method, the powder sample is often loaded into a powder sample holder, which is a flat molded body made of glass, aluminum, etc., and generally has a circular or square recess formed in the center of one of the flat surfaces, and then used for measurement.

[0005] When filling the concave portion of the powder sample holder with the powder sample, first fill the concave portion of the powder sample holder with the powder sample using a spatula or the like. Next, place the leveling member that comes with the powder sample holder on the surface of the powder sample. Then, slide the leveling member to press and fix the powder sample against the concave portion while leveling off the excess powder sample, so that the main surface, which is the reference surface of the sample holder, and the surface of the powder sample are flush with each other.

[0006] If the grinding operation of the powder sample is performed in only one direction with respect to the surface of the powder sample, the powder sample may have a preferred orientation, or the surface of the powder sample may be tilted rather than parallel to the main surface of the powder sample holder. To avoid such a situation, when grinding the powder sample, the powder sample holder is held with the fingers and the powder sample holder is rotated little by little to grind the powder sample. In other words, in order to randomize the direction in which the powder sample is ground, it is necessary to repeatedly rotate the powder sample holder and grind the powder sample.

[0007] When measuring the powder sample filled in the powder sample holder in this way, one method is to grasp the powder sample holder individually with fingers and place it on the measurement stage of the powder X-ray diffractometer for measurement, or to grasp the powder sample holder with an automatic transfer robot and transport it to and mount it on the measurement stage of the powder X-ray diffractometer.

[0008] When the powder sample preparation process is carried out multiple times in succession, after filling one powder sample into the recess of the powder sample holder, be sure to clean the spatula or scraping member used in that preparation process and to which the powder sample has adhered with alcohol using a paper wiper or a clean room wiper, etc., to prevent contamination of the powder sample in the next preparation process. [Prior art documents] [Patent documents]

[0009] [Patent Document 1] JP 2003-149174 A Summary of the Invention [Problem to be solved by the invention]

[0010] However, there are several challenges associated with this continuous powder sample preparation process. The first problem is that when a glass sample holder and a glass leveling member are used, both of which are insulators, if the powder sample is a powder that easily becomes charged, when the leveling member is brought close to the powder sample, the powder sample may adhere to the leveling member, or conversely, the powder sample may scatter from the sample holder, thereby compromising the workability of the powder sample preparation process.

[0011] The second problem is that the sample holder and the leveling member are rubbed together during the leveling operation. When the excess powder sample is leveled off with the leveling member, the excess powder sample is expelled onto the surface side of the powder sample holder other than the recessed portion. When the leveling member is used to scrape off the expelled powder sample outside the sample holder, the sample holder and the leveling member are also rubbed together.

[0012] As a result, when the powder sample holder and the leveling member are used frequently, the sample holder and the leveling member are scratched. When a leveling operation is performed using a sample holder and a leveling member with such scratches, the scratches are transferred to the surface of the powder sample filled in the recess of the powder sample holder, forming unevenness. Furthermore, when the powder sample buried in the scratches on the main surface of the powder sample holder is removed with a paper wiper, a clean room wiper, or the like, the paper wiper or the clean room wiper comes into contact with the powder sample filled in the recess of the powder sample holder, forming unevenness on the surface of the powder sample, and the flatness of the powder sample surface is lost.

[0013] The optical system is such that the X-rays generated from the X-ray tube diverge before reaching the surface of the powder sample, and the diffracted X-rays from the powder sample are focused on the detector side. For this reason, if the powder sample surface is uneven, the uneven surface can cause errors in the observed diffraction angle in reflection measurements using the pseudo-focusing method, or the diffracted X-rays diffracted at the concave parts can be absorbed by the convex parts, weakening the observed diffraction peak intensity. As a result, it becomes impossible to obtain a good diffraction profile. To avoid this, it becomes necessary to redo the powder sample filling operation, which impairs workability.

[0014] Third, even if you try to wipe the scraper with alcohol-soaked paper wipers or clean room wipers, if the powder sample is sticky, it may not be possible to wipe it off completely. Using a scraper in such a state can cause contamination of the powder sample.

[0015] In summary, in the powder sample preparation process performed before the reflection measurement using the pseudo-focusing method, scratches are formed on the powder sample holder and the leveling member. If a powder sample holder or leveling member with such scratches is used, fine irregularities are formed on the surface of the powder sample. In addition, there are cases where a good quality X-ray diffraction profile cannot be obtained due to the influence of the fine irregularities, and there is also the problem that the adhesion and scattering of the powder sample impairs the workability.

[0016] The present invention has been made under the above-mentioned circumstances, and the problem to be solved by the present invention is to provide a powder sample holder which has an antistatic effect and excellent scratch resistance and a manufacturing method thereof, a powder sample holder set which has the powder sample holder and a scraping member which has an antistatic effect and excellent scratch resistance, and a powder X-ray diffraction measurement method using the powder sample holder. [Means for solving the problem]

[0017] As a result of research conducted to solve the above-mentioned problems, the inventors came up with the idea of ​​providing the above-mentioned powder sample holder with a protective film that can provide scratch resistance and antistatic effects, and completed the present invention.

[0018] That is, the first invention for solving the above-mentioned problems is: A powder sample holder for loading a powder sample used in powder X-ray diffraction measurement, a recess having a bottom surface and a side surface is provided on a main surface of the powder sample holder; The powder sample holder has a protective film provided on the main surface and the side surface of the recess. The second invention is A powder sample holder according to the first aspect of the present invention, Furthermore, the protective film is provided on the bottom surface of the recess. The third invention is A powder sample holder for loading a powder sample used in powder X-ray diffraction measurement, a recess formed by a concave curved surface is provided on a main surface of the powder sample holder; The powder sample holder has a protective film on the main surface and on the recess. The fourth invention is In the powder sample holder according to any one of the first to third aspects of the present invention, the protective film is a diamond-like carbon film. The fifth invention is In the sample holder according to the fourth aspect of the present invention, the color of the diamond-like carbon film is different from the color of the material of the powder sample holder. The sixth invention is A method for producing the powder sample holder according to the first aspect of the present invention, comprising the steps of: The method for producing a powder sample holder includes providing a protective film on the main surface and the side surface of a recess of the powder sample holder into which the powder sample used in the powder X-ray diffraction measurement is filled. The seventh invention is A method for producing a powder sample holder according to the second aspect of the present invention, comprising the steps of: The method for producing a powder sample holder includes providing a protective film on the main surface, bottom surface and side surface of the recess of the powder sample holder into which the powder sample used in the powder X-ray diffraction measurement is to be filled. The eighth invention is A method for producing a powder sample holder according to the third aspect of the present invention, comprising the steps of: The method for producing a powder sample holder includes providing a protective film on the main surface and recesses of the powder sample holder into which the powder sample used in the powder X-ray diffraction measurement is to be filled. The ninth invention is A method for manufacturing a powder sample holder according to any one of the sixth to eighth aspects of the present invention, wherein the protective film is a diamond-like carbon film. The tenth invention is A ninth aspect of the present invention is a method for manufacturing a powder sample holder, in which the color of the diamond-like carbon film and the color of the material of the powder sample holder are made different. The eleventh invention is A powder sample holder set comprising the powder sample holder according to any one of the first to third aspects of the present invention and a leveling member used for leveling a powder sample filled in the powder sample holder, The powder sample holder set has a protective film on the surface of the scraping member. The twelfth invention is The powder sample holder set according to an eleventh aspect of the present invention, wherein the protective film is a diamond-like carbon film. The thirteenth invention is A powder sample holder set according to the twelfth invention, wherein the color of the diamond-like carbon film is different from the color of the material of the powder sample holder. The fourteenth invention is A powder X-ray diffraction measurement method for performing powder X-ray diffraction measurement using a powder sample holder according to any one of the first to third aspects of the present invention. The fifteenth invention is A powder X-ray diffraction measurement method for performing powder X-ray diffraction measurement using the powder sample holder set according to the eleventh invention. Effect of the Invention

[0019] The present invention provides a powder sample holder with scratch resistance and antistatic properties, which makes it possible to obtain a good quality X-ray diffraction profile of the powder sample and improves the workability of the powder sample preparation process. [Brief description of the drawings]

[0020] [Figure 1] FIG. 1 is a schematic perspective view of an example of a powder sample holder according to the present invention. [Diagram 2] FIG. 2 is a schematic perspective view of an example of a leveling member according to the present invention. [Diagram 3] FIG. 2 is a schematic cross-sectional view showing a position where a protective film is formed on an example of a powder sample holder according to the present invention. [Figure 4] FIG. 11 is a schematic cross-sectional view showing the position of a protective film formed on a different example of the powder sample holder according to the present invention. [Diagram 5] FIG. 11 is a schematic cross-sectional view showing the position of a protective film formed on yet another example of the powder sample holder according to the present invention. [Figure 6] FIG. 11 is a schematic cross-sectional view showing the position of a protective film formed on still another example of the powder sample holder according to the present invention. [Figure 7] 4 is a schematic cross-sectional view showing a position where a protective film is formed on the leveling member according to an example of the leveling member of the present invention. FIG. [Figure 8] 1 is a schematic cross-sectional view showing a method of leveling a powder sample filled in a powder sample holder according to the present invention by using a leveling member according to the present invention. FIG. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0021] The powder sample holder and the powder sample holder set according to the present invention will be described with reference to the drawings. FIG. 1 is a schematic perspective view of an example of a powder sample holder according to the present invention. In FIG. 1, one flat surface of the powder sample holder 11 is a flat surface on the side where the recess 12 for filling the powder sample is provided, and this flat surface is the main surface 13. FIG. 1 shows a holder in which the powder sample holder 11 has a disk-shaped outer shape and the recess 12 is also round, but the shape is not particularly limited, and powder sample holders 11 having a flat plate shape and recesses 12 for filling the powder sample having a square shape are also generally available commercially. In addition, the powder sample holder 11 used for powder X-ray diffraction measurement can be made of glass, resin, or metal. The present invention can be applied to powder sample holders 11 having any shape and any material.

[0022] In the present invention, a powder sample holder 11 having a disk-shaped outer shape and a recess 12 having a round shape will be described as an example. The powder sample holder 11 has an outer periphery of 30 to 50 mmφ and a thickness of about 1 to 2 mm, and the recess 12 has a size of 20 to 25 mmφ and a depth of about 0.2 to 0.5 mm.

[0023] The recess 12 has a bottom surface 15 and a side surface 16, and the bottom surface 15 is roughly ground glass-like to prevent the filled powder sample from falling off. On the other hand, as described above, since the height position of the powder sample surface and the filled powder sample surface need to be aligned on the concentration circle of the powder X-ray diffraction device, the main surface 13 of the powder sample holder 11 serves as a reference surface for the sample height and is machined with higher precision than the other surfaces.

[0024] FIG. 2 is a schematic perspective view of an example of a leveling member according to the present invention. 2, the leveling member 21 is a flat plate made of glass, resin, or metal, but is preferably made of glass. The leveling member 21, together with the above-mentioned powder sample holder 11, constitutes a powder sample holder set according to the present invention. In this specification, the leveling member will be described by taking as an example a glass plate 23 constituting the leveling member, which has both front and back surfaces 24 of the leveling member. In the scraping member 21, the edge 22 that scrapes the powder sample is straight and is chamfered with high precision.

[0025] 3 to 5 are schematic cross-sectional views showing different positions at which a protective film is formed on an example of the powder sample holder 11 according to the present invention. 3 shows that a protective film 14 is provided on the main surface 13 of the powder sample holder 11 and on the entire bottom surface 15 and side surface 16 of the recess 12. The side surface 16 is provided perpendicular to the bottom surface 15. As a result, this is an example in which the bottom area of ​​the bottom surface 15 of the recess 12 is equal to the opening area of ​​the recess 12.

[0026] 4 shows that a protective film 14 is provided on the main surface 13 of the powder sample holder 11 and on the entire bottom surface 15 and side surface 16 of the recess 12, and the protective film 14 is provided on these entire surfaces, but the side surface 16 is provided at an angle exceeding perpendicular to the bottom surface 15. As a result, this is an example in which the opening area of ​​the recess 12 is larger than the base area of ​​the bottom surface 15 of the recess 12, and the recess 12 has an inverted truncated cone structure or an inverted truncated pyramid structure.

[0027] There is no particular limitation on the method for manufacturing the powder sample holder 11 in which the recess 12 has an inverted truncated cone structure or an inverted truncated pyramid structure. The recess 12 may be formed or the side surface 16 of the recess 12 may be inclined by machining at a machining center. Specifically, a cylindrical or prismatic end mill is used as a grinding blade to perform pocket machining and groove machining to form a cylindrical or prismatic recess 12 on the main surface 13 of the powder sample holder 11. Next, a tapered end mill is used to form an inclined surface on the side surface 16 of the recess 12. Alternatively, a cylindrical end mill may be used to incline a glass sample holder to form an inclined surface. The same applies when the powder sample holder 11 is made of resin or metal.

[0028] Furthermore, machining of the powder sample holder 11 in which the area of ​​the opening of the recess 12 is greater than the area of ​​the bottom surface 15 of the recess 12 does not require high precision machining as is required for the main surface 13. Therefore, for example, it is possible to use a tool such as a router bit used for precision engraving or dentistry to grind the side surface 16 of the recess 12 of the powder sample holder 11 having a normal cylindrical or prismatic recess, thereby machining the recess 12 into a predetermined inverted truncated cone structure or inverted truncated pyramid structure. The same applies when the powder sample holder 11 is made of resin or metal.

[0029] Figure 5 shows an example in which, like Figure 3, the side surface 16 is formed perpendicular to the bottom surface 15, and the bottom area of ​​the bottom surface 15 of the recess 12 is equal to the opening area of ​​the recess 12, but a protective film 14 is provided on the main surface 13 of the powder sample holder 11 and the side surface 16 of the recess 12, but no protective film 14 is provided on the bottom surface 15. Furthermore, although not shown, in the same manner as described using Figure 4, the side surface 16 is set at an angle greater than perpendicular to the bottom surface 15, with the result that the opening area of ​​the recess 12 is greater than the base area of ​​the bottom surface 15 of the recess 12. A protective film 14 is provided on the main surface 13 of the powder sample holder 11 and the side surface 16 of the recess 12, but in some cases no protective film 14 is provided on the bottom surface 15. A protective film 14 is provided on the main surface 13 of the powder sample holder 11 and on the side surface 16 of the recess 12, but an example in which the protective film 14 is not provided on the bottom surface 15 is a configuration used when there is concern that the protective film 14 may interfere with powder X-ray diffraction measurement of the powder sample 31 described below.

[0030] 6 shows an example in which the recess 12 has a concave curved surface 17, and a protective film 14 is provided on the entire surface of the main surface 13 of the powder sample holder 11 and the recess 12. In this case, the contact area between the powder sample holder 11 and the powder sample is larger than in the above-mentioned inverted truncated cone shape or inverted truncated pyramid shape, and the physical adhesive force between them is increased. This makes it possible to further prevent the powder sample from falling off the powder sample holder and to prevent the flatness of the powder sample surface from being damaged.

[0031] Furthermore, since the recess 12 has a concave curved surface 17, there is no corner formed by the bottom surface 15 and the side surface 16 as in the cases shown in Figures 3 to 5, which is even more preferable as it further increases the physical adhesion force between the powder sample holder 11 and the powder sample.

[0032] There is no particular restriction on the method for manufacturing the powder sample holder 11 in which the recess 12 has the concave curved surface 17, but it may be a machining method in a machining center. Specifically, an end mill having a ball-shaped (spherical) grinding blade may be used to form the recess 12 having the concave curved surface 17 on the reference surface 13 of the powder sample holder. The same applies when the powder sample holder 11 is made of resin or metal.

[0033] Any of the powder sample holders 11 described with reference to Figures 3 to 6 can be used in the present invention. However, the powder sample holder 11 described with reference to Figures 3 and 5 is easy to manufacture. The powder sample holder 11 described with reference to Figure 4 allows for easy operation of leveling off the powder sample with the leveling member 21. The powder sample holder 11 described with reference to Figure 6 makes it easy to ensure the flatness of the powder sample surface when leveling off the powder sample with the leveling member 21.

[0034] The protective film 14 is not limited to any material as long as it has scratch resistance and antistatic properties. Specifically, oxide films, nitride films, oxynitride films, diamond-like carbon films (sometimes referred to as "DLC films" in the present invention), etc. are possible, with DLC films being preferred.

[0035] The DLC film has a diamond bond (SP 3 bond) and graphite bond (SP 2 DLC film has intermediate properties between diamond and graphite, with both bonds (a) and (b) being mixed, and has high hardness and a small coefficient of friction, and has an amorphous structure. DLC film is also excellent in terms of imparting wear resistance, friction resistance, and contamination resistance to the protective film 14, in addition to scratch resistance and antistatic effects.

[0036] The formation of the protective film 14 on the powder sample holder 11 and the formation of the film 25 on the leveling member, which will be described later, will be described using a method for forming a DLC film as an example.

[0037] The method for forming the DLC film is not particularly limited, and any of known methods such as vacuum deposition, ion beam assisted deposition, gas cluster ion beam assisted deposition, ion plating, ion beam sputtering, magnetron sputtering, bias sputtering, ECR (Electron Cyclotron Resonance) sputtering, radio frequency (RF) sputtering, thermal CVD (Chemical Vapor Deposition), plasma CVD, photo CVD, etc., may be appropriately adopted. Among these, the film is preferably formed by sputtering.

[0038] When forming a DLC film, if the film forming conditions are such that the diamond structure side is selected, the DLC film becomes hard, and if the film forming conditions are such that the graphite structure side is selected, the DLC film becomes soft. In the present invention, however, a film on the hard diamond structure side is preferable. In addition, the film color of the DLC film is usually a glossy black color, but it can take on a reddish brown, blue, or yellow gloss by controlling the film forming conditions. By using this change in color of the DLC film, the color of the DLC film can be made different from the material (material) of the powder sample holder 11. By making the protective film and the material (material) of the powder sample holder 11 different colors, not only can it be confirmed whether the protective film is evenly formed on the powder sample holder, but also, if peeling of the protective film (DLC film) occurs, the occurrence of the peeling can be determined.

[0039] By appropriately adjusting the film formation conditions (type of sputtering target, sputtering time, type of gas introduced) and forming the film by sputtering, a protective film 14 with high adhesion is provided on the main surface 13 of the powder sample holder 11 and the entire bottom surface 15 and side surface 16 of the recess 12. Note that if the gas pressure during film formation is high, the film formed by sputtering will have a fine uneven structure on the film surface. Since it is preferable that the surface of the protective film 14 is flat, it is preferable that the film formation gas pressure is low.

[0040] 5, the protective film 14 may be formed on the main surface 13 of the powder sample holder 11 and the side surface 16 of the recess 12. In this case, to prevent the protective film 14 from adhering to the bottom surface 15 of the recess 12, this portion may be masked with resin, tape, or the like.

[0041] FIG. 7 shows a schematic cross-sectional view of the leveling member 21 described in FIG. As shown in FIG. 7, it is preferable that a protective film 25 of the leveling member, similar to the protective film 14, is provided on both the front and back surfaces 24 of the glass plate 23 constituting the leveling member.

[0042] The leveling operation of a powder sample according to the present invention will be described with reference to FIG. FIG. 8 is a schematic cross-sectional view showing a method of leveling off the powder sample 31 filled in the powder sample holder 11 shown in FIG. 3 described above, using the leveling member 21 shown in FIG. 7 described above.

[0043] A predetermined amount of powder sample 31 is poured into the recess 12 of the powder sample holder 11 using a spatula or the like. At this time, if a large amount of powder sample 31 is poured compared to the volume of the recess 12 of the powder sample holder 11, it will take a long time to grind down the powder sample 31. Therefore, an appropriate amount of powder sample 31 is poured relative to the volume of the recess 12. Then, the main surface 13 of the powder sample holder 11 and the surface of the ground-off powder sample 31 are aligned, and the surface of the powder sample 31 is made smooth.

[0044] At this time, since the protective film 14 covering the powder sample holder 11 is conductive, even if the powder sample 31 placed on the spatula is brought close to the powder sample holder 11, the powder sample 31 will not scatter due to static electricity.

[0045] The front or back surface of the leveling member 21 is brought into contact with the main surface 13 (i.e., the flat surface portion other than the recessed portion) of the powder sample holder 11, and while maintaining this state, the leveling member 21 is moved to level off the powder sample 31. More specifically, while keeping the flat surface of the leveling member 21 in surface contact with the main surface 13 (i.e., the flat surface portion other than the recessed portion 12) of the powder sample holder 11 in close contact with each other, the leveling member 21 is moved to level off the powder sample 31.

[0046] At this time, since the powder sample holder 11 and the leveling member 21 are provided with an antistatic effect, when the powder sample 31 is filled into the recess 12 of the powder sample holder 11 or when the powder sample 31 is leveled by the leveling member 21, the powder sample 31 does not scatter or adhere to the leveling member 21. As a result, the main surface 13 of the powder sample holder 11 and the surface of the powder sample 31 filled in the recess 12 can easily be made flush with each other.

[0047] During the leveling operation, the powder sample holder 11 and the leveling member 21 rub against each other to level off excess powder sample 31. However, the main surface 13 of the powder sample holder 11 is covered with a protective film 14, and the glass plate 23 constituting the leveling member is provided with protective films 25 on both the front and back surfaces 24 of the leveling member, so that the powder sample holder 11 and the leveling member 21 are not scratched.

[0048] After the leveling operation is completed, the powder sample 31 adhering to the main surface 13 of the powder sample holder 11 or to both sides 24 of the leveling member, even if the powder sample 31 is sticky, can be removed with a paper wiper soaked in alcohol or a clean room wiper. As a result, no contamination occurs even if the same leveling member 21 is used to subsequently level another powder sample 31.

[0049] In other words, when performing powder X-ray diffraction measurement, high workability can be ensured by performing the powder X-ray diffraction measurement using the powder sample holder 11 or powder sample holder set according to the present invention.

[0050] The protective film 14 can be made amorphous by controlling the film formation conditions during sputtering. When this configuration is adopted, even if the powder sample 31 is filled into the powder sample holder 11 provided with the protective film 14 covering the entire surfaces of the main surface 13, the bottom surface 15 of the recess 12, and the side surfaces 16, and X-ray diffraction measurement is performed, no crystalline diffraction peaks originating from the protective film 14 are detected. As a result, it is possible to prevent the protective film 14 from interfering with the powder X-ray diffraction measurement and subsequent analysis. EXAMPLES

[0051] An example will be described in which a colored DLC film is formed as a protective film on a powder sample holder and a leveling member.

[0052] Example 1 A circular glass holder for XRD (outer diameter 32 mm, thickness 2 mm, circular groove φ16 mm, groove depth 0.2 mm, manufactured by Spectris) was prepared as a powder sample holder, and a glass flat plate (35 mm × 50 mm × thickness 2 mm, manufactured by Overseas X-Ray Services) was prepared as a leveling member. The powder sample holder and the glass leveling member were colorless and transparent.

[0053] A diamond-like carbon (DLC) film was produced on the leveling member by DC magnetron sputtering using a carbon sintered target (4N purity, 64 x 600 x 6 mmt).

[0054] The distance between the target and the glass powder sample holder and the glass leveling member was 55 mm. The vacuum in the chamber was 2×10 -4 ~1×10 -4 When the deposition gas pressure reached 0.3 Pa, Ar gas with a purity of 99.9999% was introduced into the chamber to set the deposition gas pressure to 0.3 Pa. The DC power density at the target input was 2.2 W / cm 2 It was carried out in.

[0055] The diamond-like carbon film was formed to a thickness of 200 nm by rotating the powder sample holder and the glass scraper, which were placed facing the sintered carbon target, without heating. The film formation conditions, film thickness, film color, and film properties are shown in Table 1.

[0056] The powder sample holder and the surface of the scraping material were yellow in color. The evaluation of whether the film was diamond-like carbon was performed using a Bruker Optics Laser Raman Microscope (SENTERRA) to measure the SP of the carbon component. 2 Bonded carbon, SP 3 The mixed state of bonded carbon was analyzed. From the Raman spectrum, SP originating from carbon was 2 Bonded carbon, SP 3 The Raman peaks of the bonded carbon were evaluated by peak fitting using a Gaussian waveform. 2 Bonded carbon, SP 3 The presence of bonded carbon was confirmed, and it was confirmed that the film formed was a diamond-like carbon film.

[0057] Example 2 Diamond-like carbon films were formed on the surfaces of a glass powder sample holder and a glass scraping member in the same manner as in Example 1, except that the deposition gas pressure was changed to 1.4 Pa. The deposition conditions, film thickness, film color, and film properties are shown in Table 1. The powder sample holder and the surface of the scraping material were brown in color. 2 Bonded carbon, SP 3 The presence of bonded carbon was confirmed, and it was confirmed that the film formed was a diamond-like carbon film.

[0058] Example 3 Diamond-like carbon films were formed on the surfaces of a glass powder sample holder and a glass scraping member in the same manner as in Example 1, except that the deposition gas pressure was changed to 3.0 Pa. The deposition conditions, film thickness, film color, and film properties are shown in Table 1. The powder sample holder and the surface of the scraping material were black. 2 Bonded carbon, SP3 The presence of bonded carbon was confirmed, and it was confirmed that the film formed was a diamond-like carbon film.

[0059] [Table 1] [Explanation of symbols]

[0060] 11. Powder sample holder 12. Recess 13. Main surface 14.Protective film 15. Bottom 16. Side 17. Concave surface 21.Flattening material 22. Edge of scraping material 23. Glass plate constituting the scraping member 24. Front and back sides of the scraping material 25.Protective film for scraping parts 31. Powder sample

Claims

1. A powder sample holder for loading a powder sample used in powder X-ray diffraction measurement, comprising: a recess having a bottom surface and a side surface is provided on a main surface of the powder sample holder; A powder sample holder in which a protective film is provided on the main surface and the side surface of the recess.

2. 2. A powder sample holder according to claim 1, Furthermore, the protective film is provided on the bottom surface of the recess.

3. A powder sample holder for loading a powder sample used in powder X-ray diffraction measurement, comprising: a recess formed by a concave curved surface is provided on a main surface of the powder sample holder; A powder sample holder, the powder sample holder having a protective film on the main surface and the recess.

4. 4. A powder sample holder according to claim 1, wherein the protective film is a diamond-like carbon film.

5. 5. The sample holder according to claim 4, wherein the color of the diamond-like carbon film is different from the color of the material of the powder sample holder.

6. 2. A method for manufacturing a powder sample holder according to claim 1, comprising the steps of: A method for manufacturing a powder sample holder, comprising providing a protective film on the main surface and the side surface of a recess of the powder sample holder into which a powder sample used in the powder X-ray diffraction measurement is to be filled.

7. 3. A method for manufacturing a powder sample holder according to claim 2, comprising the steps of: A method for manufacturing a powder sample holder, comprising providing a protective film on the main surface of the powder sample holder into which the powder sample used in the powder X-ray diffraction measurement is to be filled, and on the bottom and side surfaces of the recess.

8. A method for manufacturing a powder sample holder according to claim 3, comprising the steps of: A method for manufacturing a powder sample holder, comprising providing a protective film on the main surface and recess of the powder sample holder into which the powder sample used in the powder X-ray diffraction measurement is to be filled.

9. 9. The method for manufacturing a powder sample holder according to claim 6, wherein the protective film is a diamond-like carbon film.

10. 10. The method for manufacturing a powder sample holder according to claim 9, wherein the color of the diamond-like carbon film is different from the color of the material of the powder sample holder.

11. 4. A powder sample holder set comprising the powder sample holder according to claim 1 and a leveling member used to level a powder sample filled in the powder sample holder, A powder sample holder set in which a protective film is provided on the surface of the scraping member.

12. 12. The powder sample holder set according to claim 11, wherein the protective film is a diamond-like carbon film.

13. 13. The powder sample holder set according to claim 12, wherein the color of the diamond-like carbon film is different from the color of the material of the powder sample holder.

14. A powder X-ray diffraction measurement method, comprising: carrying out powder X-ray diffraction measurement using the powder sample holder according to any one of claims 1 to 3.

15. A powder X-ray diffraction measurement method comprising the steps of: performing powder X-ray diffraction measurement using the powder sample holder set according to claim 11 .

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