JP2017187480A - Resin solidification piece preparation tool - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a resin solidification piece preparation tool capable of preparing a resin solidification piece having a suitable shape and size.SOLUTION: A resin solidification piece preparation tool 300 comprises: a first tool 100 having a rectangular parallelepiped shape space formed by a through hole 12 having a cross-section rectangle having a length of 2-12 mm and a width of 1-3 mm and having a granular material sample and a resin injected into the through hole from the opening on one side of the through hole (an upper side) in the state that an opening on the other side (a lower side) of the through hole is blocked by a polymer film 40; and a second tool 200 for pushing a resin solidification piece by fitting the second tool from the opening on the one side (the upper side) into the through hole in the state that the resin is solidified in the through hole, and the blockage of the opening on the other side (the lower side) is released by the polymer film.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a resin consolidated piece production jig.

  When analyzing a powder sample, a resin-solidified piece produced by resin-solidifying the powder sample is molded to produce an observation sample (see, for example, Patent Documents 1 and 2). Further, when molding the resin consolidated piece, the observation cross section may be ion milled.

Japanese Patent Laying-Open No. 2015-40724 Japanese Patent Laying-Open No. 2015-114241

  In the ion milling process, it is necessary to set the resin consolidated piece on the holder without a gap with the shielding plate. For this purpose, the angle formed by at least one pair of adjacent two surfaces of the resin consolidated piece is made substantially vertical. There is a need. Moreover, since the observation sample to be analyzed needs to be held in an existing holder, the size is limited.

  However, at present, no effective method has been proposed for producing a resin-solidified piece of a granular sample that satisfies the above-described conditions. For example, in order to produce a small sample piece to be held by an existing holder, a method is conceivable in which a resin-solidified piece of a certain size is produced, then cut to a predetermined size, polished and molded. However, when a small sample piece is extremely small, there is a problem that corners are broken during cutting and polishing. In addition, some of the particulate samples introduced into the resin consolidated pieces may be altered by moisture or heat. In this case, the observation surface comes into contact with moisture or is generated by friction during cutting or polishing operations. There was a problem that accurate analysis could not be performed due to deterioration due to heat.

  This invention is made | formed in view of said subject, and it aims at providing the resin-solidified piece preparation jig | tool which can produce the resin-solidified piece of a suitable shape and a magnitude | size.

  In the resin-bonded piece manufacturing jig of the present invention, a rectangular parallelepiped space is formed by a through hole having a rectangular section of 2 to 12 mm in length and 1 to 3 mm in width, and an opening on one side of the through hole is closed by a closing member A first jig in which a granular material sample and a resin are injected into the through-hole from the opening on the other side of the through-hole in a state of being formed, and the resin is solidified in the through-hole; and In a state where the opening on the one side by the closing member is released, the resin solidified piece containing the powder sample and the resin is inserted into the through hole from the opening on the other side. A second jig to be extruded.

  The resin-consolidated piece preparation jig of the present invention has an effect that a resin-consolidated piece having an appropriate shape and size can be prepared.

It is a perspective view which shows the structure of the resin consolidation piece preparation jig which concerns on one Embodiment. Fig.2 (a)-FIG.2 (c) are the figures for demonstrating the production method of a resin consolidated piece. It is a perspective view which shows a resin consolidated piece. FIG. 4A to FIG. 4C are diagrams for explaining the procedure for setting the resin consolidated piece on the holder stand. FIG. 5A and FIG. 5B are diagrams schematically showing ion polishing in the case where two adjacent surfaces of the resin consolidated piece are 90 °. FIG. 6A and FIG. 6B are diagrams schematically showing ion polishing in the case where two adjacent surfaces of the resin consolidated piece are not 90 °.

  Hereinafter, the resin consolidated piece preparation jig according to an embodiment will be described in detail with reference to FIGS. FIG. 1 is a perspective view schematically showing a configuration of a resin consolidated piece producing jig 300 according to an embodiment.

  The resin-solidified piece preparation jig 300 is a jig for producing a resin-solidified piece that is the basis of an observation sample that is finally analyzed and observed by a scanning electron microscope (SEM). As shown in FIG. 1, a first jig 100 and a second jig 200 are provided.

  The first jig 100 has a substantially columnar shape, and has two frame members 10 and a resin portion 20 as a deformation suppressing member.

  The frame-like member 10 is a substantially cylindrical member made of, for example, nylon and having a through-hole 12 having a rectangular cross section. A rectangular parallelepiped space is formed in the frame-shaped member 10 by the through hole 12. The cross section of the through-hole 12 shall be 2-12 mm long and 1-3 mm wide. Moreover, the depth of the through-hole 12 shall be about 6 mm. Here, the inner surface forming the through hole 12 of the frame-shaped member 10 is smooth with few irregularities. In addition, as a material of the frame-shaped member 10, a silicon system, a metal system, etc. may be used.

  The resin portion 20 is made of epoxy resin and is a member that surrounds the periphery of the side surface of the frame-shaped member 10 in order to suppress deformation of the two frame-shaped members 10. When the resin is injected into the frame-shaped member together with the granular sample and consolidated, the frame-shaped member may be deformed due to the pressure of the injected resin or the volume change during consolidation. The portion 20 can suppress the deformation of the frame-shaped member 10 and can maintain the cross-sectional shape of the through hole 12 to be rectangular. Thus, by providing a deformation suppressing member such as the resin portion 20 around the frame-shaped member, there is no problem even if a material that is easily deformed is selected as the frame-shaped member. For this reason, when selecting the material of the frame-like member, it is possible to preferentially select a material that can easily extrude the resin after the resin is consolidated. In addition, since the frame-shaped member alone is very small as a jig, it becomes difficult to fix the frame-shaped member during the extruding operation after resin consolidation, and the workability is lowered, but it is easy to fix by providing a deformation suppressing member. This also leads to improved workability. The upper surface of the resin part 20 and the upper surface of the frame member 10 are flush with each other, and the lower surface of the resin part 20 and the lower surface of the frame member 10 are flush with each other.

  Note that when the resin-bonded piece using the first jig 100 is manufactured, a closing member is provided on the lower surface of the first jig 100 so as to close the opening on one side (lower side) of the through hole 12. The polymer film (for example, PET (Polyethylene terephthalate) film) 40 is provided and fixed by an adhesive tape 50 (see FIG. 2A). The polymer film 40 has a flat surface with almost no unevenness.

  In FIG. 1, the two jigs 10 are provided on the first jig 100. However, the present invention is not limited to this, and one or three or more frames 10 may be provided.

  The second jig 200 has a base portion 62 and an extrusion plate 60. The base portion 62 has a substantially cylindrical shape, and is in a state in which one end portion of the extrusion plate 60 is inserted. The extrusion plate 60 is a metal plate having a rectangular cross section. The extrusion plate 60 has a size that fits into the through hole 12 formed in the frame-shaped member 10 of the first jig 100. That is, the cross-sectional rectangle of the extrusion plate 60 is substantially the same as or slightly smaller than the cross-sectional rectangle of the through hole 12. A notch 60 a is provided at the end (other end) of the pusher plate 60 opposite to the base portion 62.

  Next, a method for producing a resin-solidified piece using the resin-solidified piece producing jig 300 will be described with reference to FIGS. 2 (a) to 2 (c). In addition, the production work of the resin consolidated piece is performed in an inert gas (in the glove box).

  First, as shown in FIG. 2A, the worker provides a polymer film 40 on the lower surface of the first jig 100 so as to close the opening on one side (lower side) of the through hole 12. Fix with adhesive tape 50.

  Next, as shown in FIG. 2 (b), the operator puts the granular material sample 80 into the through hole 12 through the opening on the other side (upper side) of the through hole 12 and injects the resin material 90. Here, the resin material 90 is obtained by leaving the epoxy-embedded resin in an atmosphere of 40 ° C. for about 1 hour and then mixing a curing agent at a ratio of 25: 3 (= epoxy-embedded resin: curing agent), for example. is there. In the present embodiment, as described above, the upper surfaces of the frame-shaped member 10 and the resin portion 20 are flush with each other. Therefore, even when the granular material sample 80 or the resin material 90 is removed from the through hole 12 when it is put into the through hole 12, the powder sample 80 and the resin material 90 can be stirred again using a toothpick or a spoon.

  Thereafter, the operator performs vacuum degassing (or vacuum degassing) of the first jig 100 in FIG. Thereby, the granular material sample 80 and the resin material 90 are mixed and settled to the bottom of the through-hole 12. After that, it is allowed to stand until it is consolidated in the atmosphere, and it waits until the mixture of the powder sample 80 and the resin material 90 is consolidated.

  Next, the operator removes the adhesive tape 50 and the polymer film 40 from the first jig 100 as shown in FIG. 2 (c), and moves the extrusion plate 60 of the second jig 200 to the frame-shaped member 10. It inserts into the through-hole 12 from the opening on the other side (upper side). Thereby, the resin consolidated piece 180 as shown in FIG. 3 is pushed out from the through hole 12 of the first jig 100. In this case, since the extrusion plate 60 is in surface contact with the resin consolidated piece 180, a large pressure is not applied to the resin consolidated piece 180. Thereby, it can suppress that the resin consolidated piece 180 deform | transforms or breaks. In addition, since the notch 60a is provided in the edge part of the extrusion board 60, insertion of the extrusion board 60 to the through-hole 12 becomes easy.

  Here, since the resin consolidated piece 180 of FIG. 3 is cast in the through-hole 12 having a rectangular cross section, a surface 80a to be ion-polished (ion milling) in a later step and a surface adjacent to the surface 80a. The angle formed by 80b is 90 °. Further, the surface 80a to be ion-polished has almost no unevenness because the polymer film 40 is in contact with the surface 80a in FIG. For this reason, it is not necessary to perform mechanical polishing, chemical polishing, or the like before ion polishing of the surface 80a to be ion polished.

  In this embodiment, A-type, BF-type, and O-type outlet plug blades are used as the extrusion plate 60 of the second jig 200, and the A-type is used as the frame-shaped member 10 of the first jig 100. A Titra cap that can be attached to a plug plug blade of BF type or O type can be used. In this case, since the outlet plug blade and the tie tiger cap are fitted, the resin consolidated piece 180 can be pushed out, and a resin sized piece of an appropriate size can be produced by using the tie tiger cap. .

  Next, the ion polishing process of the resin consolidated piece will be described.

  In the ion polishing step, an operator first prepares a holder stand 120 as shown in FIG. 4A in an inert gas (in a glove box). Here, the holder stand 120 includes a flat shielding plate 122 and an alignment portion 124 having an alignment surface 124a. The angle between the lower surface of the shielding plate 122 and the alignment surface 124a is vertical (90 °).

  Next, the operator positions the resin consolidated piece 180 as shown in FIG. In this case, alignment is performed by applying the surface 80 a to be ion-polished to the alignment surface 124 a and applying the surface 80 b to the shielding plate 122. Here, the angle formed by the surfaces 80a and 80b is set to 90 °, so that no gap is generated between the shielding plate 122 and the resin consolidated piece 180.

  Next, the operator screws the fixing member 130 that fixes the position of the resin consolidated piece 180 on the holder stand 120. Thereafter, a cap that puts the inside of the holder stand 120 into an atmosphere shut-off state is attached to the holder stand 120, and in that state, the holder stand 120 is installed in the Ar ion polishing apparatus, and ion polishing is executed. In the holder stand 120, the distance between the shielding plate 122 and the alignment surface 124a is about 1 mm, and the resin consolidated piece 180 is sandwiched and fixed between the shielding plate 122 and the fixing member 130. Requires a dimension of about 1 mm. Therefore, the dimension of the resin consolidated piece 180 in the left-right direction in FIG. 4B needs to be 2 mm or more.

  Here, ion polishing will be described in more detail with reference to FIGS. FIG. 5A shows a case where the angle formed by the surfaces 80a and 80b is 90 °, and FIG. 6A shows a case where the angle formed by the surfaces 80a and 80b is not 90 ° (comparative example). Yes. In the case of FIG. 5A, when ion polishing is performed, the observation cross section can be smoothly polished as shown in FIG. 5B. On the other hand, in the case of FIG. 6A, a gap is generated between the surface 80b and the shielding plate 122. Therefore, when ion polishing is performed in this state, as shown in FIG. Ar ions enter between 80b and the observation cross section cannot be polished smoothly.

  Thus, in this embodiment, since the resin solidified piece having the angle of 90 ° formed by the surfaces 80a and 80b is produced using the resin solidified piece production jig 300 of FIG. 1, observation is performed by ion polishing. The cross section can be in an appropriate state.

  After the ion polishing is completed, a cap is attached to the holder stand 120, and the holder stand 120 with the cap attached is taken out from the Ar ion polishing apparatus and placed on a scanning electron microscope (SEM). In the SEM, after evacuating the inside of the SEM, the cap is removed from the holder stand 120, and observation and analysis of the observation surface of the resin consolidated piece (observation sample) after ion polishing are executed.

  As described above in detail, according to the present embodiment, the resin-bonded piece manufacturing jig 300 has a rectangular parallelepiped space formed by the through holes 12 having a rectangular section of 2 to 12 mm in length and 1 to 3 mm in width, In a state where the opening on one side (lower side) of the through hole 12 is closed by the polymer film 40, the granular material sample 80 and the resin material are inserted into the through hole 12 from the opening on the other side (upper side) of the through hole 12. In the state where the first jig 100 into which 90 is injected and the resin material 90 are solidified in the through-hole 12 and the blockage of the one side (lower side) opening by the polymer film 40 is released And a second jig 200 that pushes out the resin consolidated piece by fitting into the through-hole 12 from the opening on the other side (upper side). As a result, it is possible to cast a resin consolidated piece 180 having an appropriate size suitable for the size of the holder stand 120 on which the resin consolidated piece is set when performing ion polishing. As the holder stand 120, there are a holder stand that can hold a sample of 4 to 5 mm × 3 to 5 mm × 2 mm and a holder stand that can hold a sample of 12 mm × 6 mm × 3 mm. In addition, since the resin consolidated piece 180 is cast using the through hole 12 (rectangular space) having a rectangular cross section, the angle formed between the surface 80a to be ion-polished and the adjacent surface 80b can be 90 °. . Accordingly, no gap is generated between the shielding plate 122 and the surface 80b during ion polishing, so that the observation surface can be polished to an appropriate state.

  Further, in the present embodiment, the wall surface forming the through hole 12 of the first jig 100 is a smooth surface with few irregularities, so that the resin material 90 and the frame-like member 10 do not adhere or adhere to each other, and the resin solid It is possible to smoothly extrude the binding piece 180 from the frame-shaped member 10.

  In the present embodiment, the first jig 100 is provided around the frame-shaped member 10 in which the through-hole 12 is formed and the side surface of the frame-shaped member 10, and is a resin that suppresses deformation of the frame-shaped member 10. Part 20. Thereby, even if the frame-shaped member 10 is a flexible member, the deformation of the frame-shaped member 10 is suppressed, so that the angle between two adjacent surfaces of the resin consolidated piece 180 can be 90 °.

  In the present embodiment, the upper surface of the resin portion 20 is flush with the upper surface of the frame member 10. Thus, even if the powder sample 80 or the resin material 90 is spilled around the through hole 12, it can be scraped with a toothpick or a medicine spoon. At this time, if the deformation suppressing member is made of the same resin as that embedded in the frame-shaped member, even if the deformation suppressing member is accidentally shaved when scraping a spilled sample, the powder is not contained in the frame-shaped member. It is possible to prevent foreign matters other than the granular sample and the resin from being mixed.

  In the present embodiment, the second jig 200 includes A-type, BF-type, and O-type outlet plug blades, and the frame-shaped member 10 of the first jig 100 is attached to the outlet plug blade. Possible tie tiger caps. Thereby, it becomes possible to prepare the resin consolidated piece preparation jig 300 simply and inexpensively using a commercially available product.

  In the present embodiment, the opening on the lower side of the through hole 12 is closed with the polymer film 40. Thereby, the surface 80a to be ion-polished of the resin consolidated piece 180 can be flattened. This eliminates the need for mechanical polishing or chemical polishing before ion polishing of the surface 80a to be ion polished. In this case, since it is not necessary to perform polishing using water or the like, it is possible to prevent the granular sample from being altered by water or the like.

  In addition, although the said embodiment demonstrated the case where the 1st jig | tool 100 had the frame-shaped member 10 and the resin part 20, it is not restricted to this. For example, the first jig 100 may be an object in which a through hole having a rectangular cross section is formed in part. In this case, as the material of the object, a material that does not affect the observation and analysis of the granular sample 80 and that does not deform the cross-sectional shape of the through hole can be used.

  The above-described embodiment is an example of a preferred embodiment of the present invention. However, the present invention is not limited to this, and various modifications can be made without departing from the scope of the present invention.

DESCRIPTION OF SYMBOLS 10 Frame-shaped member 12 Through-hole 20 Resin part (deformation suppression member)
40 Polymer film (occlusion member)
80 Powder Sample 90 Resin 100 First Jig 180 Resin Consolidated Piece 200 Second Jig 300 Resin Consolidated Piece Jig

Claims (7)

A rectangular parallelepiped space is formed by a through hole having a rectangular cross section of 2 to 12 mm in length and 1 to 3 mm in width, and the opening on the other side of the through hole is closed by the closing member on one side of the through hole. A first jig in which a granular material sample and a resin are injected into the through hole from a portion;
In the state where the resin is solidified in the through hole and the state where the opening of the one side by the closing member is released, the resin is inserted into the through hole from the other side of the opening, And a second jig for extruding the resin solid piece including the powder sample and the resin.   The resin-bonded piece manufacturing jig according to claim 1, wherein a wall surface forming the through hole of the first jig is a smooth surface. The first jig is
A frame-like member in which the through hole is formed;
3. The resin-bonded piece manufacturing jig according to claim 1, further comprising: a deformation suppressing member that is provided around a side surface of the frame-shaped member and suppresses deformation of the frame-shaped member.   The resin deformation piece manufacturing jig according to claim 3, wherein the deformation suppressing member is made of the same resin as the resin included in the resin consolidation piece.   5. The resin-bonded piece manufacturing jig according to claim 3, wherein the deformation suppressing member has a surface flush with a surface around the opening on the other side of the frame-shaped member. The second jig includes A-type, BF-type, and O-type outlet plug blades,
6. The resin consolidated piece production according to claim 3, wherein the frame-shaped member of the first jig is a tie tiger cap that can be attached to the outlet plug insertion blade. jig.   The resin-occlusion piece production jig according to any one of claims 1 to 6, wherein the closing member is a polymer film.

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