JP2014146493A - Sample table for electron microscope observation and cross section observation method of sample - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method which allows for accurate cross-section observation, by preventing decomposition of a sample which is decomposed easily when exposed to the atmosphere.SOLUTION: A sample table 10 for electron microscope used for cross-section observation of a sample subjected to cross-section processing includes a sample table body 11 having a recess 13 of predetermined depth in an upper surface 11a of the body trunk, and at least one through hole 14 formed in a trunk side face 11b to penetrate from the side face 11b to the recess 13, and a fixing member 12 being inserted into the through hole 14. In the sample table 10 for electron microscope, a sample table for cross-section processing that is mounting a sample subjected to cross-section processing is mounted in the recess 13 of the sample table body 11, and attached while being fixed by the fixing member 12 penetrated the through hole 14.

Description

  The present invention relates to an electron microscope observation sample stage used for an electron microscope, and a sample cross-sectional observation method using an electron microscope using the electron microscope sample stage.

  Powder particles are used in various fields and applications, and the particles are often subjected to various treatments in order to give the particles performance such as heat resistance and oxidation resistance. In developing such particles, it is important to investigate in detail what the powder particle shape is.

  Usually, as a method for evaluating the shape of powder particles, surface / cross-section observation using a scanning electron microscope (SEM) is used. When cross-sectional processing of powder particles by SEM is performed, the particles are embedded in a thermosetting resin and then embedded in the resin, and then the resin-embedded sample is placed on the sample stage, and a wide range of cross-sectional processing is performed with less processing distortion. Processing is performed using a cross section polisher (CP) capable of Thereafter, the cross-section processed sample is removed from the sample stage and placed on the SEM sample stage to observe the cross-section processed portion.

  However, when the powder particles to be observed are oxide particles, etc., the particles themselves react with moisture in the atmosphere only after being exposed to the atmosphere for a few minutes, so that the original state of the particles cannot be accurately captured. This makes it impossible to perform cross-sectional observation with high accuracy.

  As an example of practical application of such a method, for example, Patent Document 1 proposes a scanning electron microscope sample stage and reports that a multipurpose scanning electron microscope sample stage has been developed. However, it has only been reported that this sample stage is a sample stage suitable for focused ion beam processing observation and SEM observation, so that it is possible to perform cross-sectional observation while preventing alteration of a sample such as oxide particles. The idea of making is not shown.

  As another practical application example, for example, there is a sample stage for an electron microscope described in Patent Document 2, and a sample stage for an electron microscope capable of EBSD analysis has been reported. However, this sample stage is limited to the EBSD analysis, and Patent Document 2 does not disclose the concept of performing the cross-sectional observation while preventing the deterioration of the sample such as oxide particles.

JP-A-11-149896 JP 2011-204367 A

  The present invention has been proposed in view of such circumstances, and it is possible to perform accurate cross-sectional observation of a sample that is easily altered by being exposed to the atmosphere, preventing the alteration of the sample. The purpose is to apply a method that enables

  The inventors of the present invention have made extensive studies to achieve the above-mentioned object, and after processing a cross section with a cross section polisher or the like, the processed sample is removed and placed on a sample stage of an electron microscope such as an SEM. We developed a sample stage for an electron microscope that can be moved directly into the barrel of an electron microscope without cross-sectional observation.

  That is, the electron microscope observation sample stage according to the present invention is an electron microscope sample stage for observing the cross section of the sample after the cross section processing, and has a concave portion with a predetermined depth on the upper surface of the body trunk. And a sample base body in which at least one through-hole penetrating from the side surface to the recess is formed on the side surface of the main body, and a fixing member inserted into the through-hole, and performing the cross-section processing The sample table for cross-section processing on which the sample is placed is placed in the concave portion of the sample table main body, and fixed and attached by the fixing member penetrating the through hole.

  Further, a sample cross-sectional observation method is a sample cross-sectional observation method in which a cross-section of a sample to be observed is processed and the cross-section of the sample obtained by processing is observed using an electron microscope. The sample stage has a recess having a predetermined depth on the upper surface of the main body body, and at least one through hole penetrating from the side surface to the recess is formed on the side surface of the main body, and the through hole The cross-section processing sample stage is placed in the concave portion of the sample stage main body in a state where the cross-section processing sample is placed on the cross-section processing sample stage. The sample is fixed by the fixing member penetrating the hole, and the cross section of the sample is observed with an electron microscope.

  According to the sample stage for an electron microscope according to the present invention, the cross-sectioned sample can be attached to the sample stage of the electron microscope as it is and placed on the cross-section sample stage for cross-sectional observation. Therefore, even in the case of a sample such as oxide particles, alteration of the sample can be prevented and accurate cross-sectional observation can be performed.

It is the top view (A) and perspective view (B) which show the sample holder which mounts an electron microscope sample stand. It is a perspective view of the sample stand for electron microscopes. It is the top view (A) and front view (B) of the sample stand for electron microscopes. It is the figure (B) which showed the figure (A) which shows a base, and the electron microscope sample stand integrated with the base. It is a figure for demonstrating a state when an observation object sample is mounted with respect to the sample stand for electron microscopes. It is a figure for demonstrating the structure of the lens barrel of an electron microscope, and the flow of operation which attaches the sample stand for electron microscopes to the sample stage in the lens barrel. 2 is a cross-sectional observation photograph by an electron microscope (SEM) in Example 1. FIG. 6 is a cross-sectional observation photograph by an electron microscope (SEM) in Comparative Example 1. FIG.

Hereinafter, a specific embodiment to which the present invention is applied (hereinafter referred to as “the present embodiment”) will be described in detail in the following order with reference to the drawings. In addition, this invention is not limited to the following embodiment, A change is possible in the range which does not deviate from the summary of this invention.
1. 1. Configuration of electron microscope sample stage 2. Place the sample to be observed on the electron microscope sample stage. About cross-section processing and cross-section observation

<1. Structure of electron microscope sample stage>
The electron microscope sample stage according to the present embodiment is an observation that performs cross-sectional structure observation, crystal orientation analysis of a cross-sectional crystal structure by a backscattered electron diffraction pattern, and the like using an electron microscope such as a scanning electron microscope (SEM). It is the sample stand for electron microscopes for mounting a sample. On this electron microscope sample stage, a cross-section processed sample (cross-section processed sample) is placed for observation, and the cross-section processed sample is placed, for example, an electron microscope as shown in FIG. The sample holder 1 is detachably attached to the sample stage mounting portion 2 formed on the sample holder 1.

  FIG. 2 is a perspective view schematically showing the electron microscope sample stage according to the present embodiment. 3 is a top view (A) and a front view (B) of the electron microscope sample stage. As shown in FIGS. 2 and 3, the electron microscope sample stage 10 includes a sample stage body 11 and a fixing member 12.

  The sample stage main body 11 has a body portion formed of, for example, a cylindrical metal member, and has a recess 13 having a predetermined depth on the upper surface 11a of the body body portion. As described above, the electron microscope sample stage 10 is characterized in that the body upper surface 11a of the sample stage body 11 has the recess 13 having a predetermined depth. As will be described in detail later, in the electron microscope sample stage 10, the cross section processing sample stage (for example, a cross section polisher) in which the observation target sample subjected to cross section processing is placed in the recess 13 provided in the sample stage main body 11. The sample stage) is placed and fixed.

  The shape of the body portion of the sample stage main body 11 is not limited to the above-described cylindrical shape, and any shape can be used as long as the concave portion 13 can be formed on the upper surface 11a. For example, the shape may be a quadrangular column or a polygonal column. Further, the size is not particularly limited, and the size can be set on the electron microscope to be used. Specifically, for example, a cylindrical shape having a diameter of about 10 to 20 mm and a height of about 10 to 15 mm can be used.

  Further, the material of the sample stage main body 11 is not particularly limited as long as it does not affect the cross-sectional observation by the electron microscope and the EBSD measurement. Specifically, a material that is conductive and does not have magnetism, such as aluminum or brass, can be used.

  The shape of the recess 13 provided on the upper surface 11a of the sample stage main body 11 is not particularly limited as long as the cross section processing sample stage placed on the recess 13 can be securely fixed. For example, as shown in FIGS. 2 and 3, the body portion of the sample base body 11 is formed into a concave portion 13 that is hollowed out into a rectangular parallelepiped shape so that the sample base for cross section processing of the rectangular parallelepiped can be placed and fixed. it can.

  Moreover, it is preferable that the depth of the recessed part 13 is shorter than the length of the height direction of the cross-section processing sample base mounted and fixed. Thereby, as shown in FIG. 5 to be described later, when the cross-section processing sample stage is placed, the upper portion of the cross-section processing sample stage can be protruded from the recess 13. It is possible to prevent the observation target sample placed on the table from coming into contact with the upper surface 11a of the sample table main body 11, and to prevent the accurate cross-sectional observation from being disturbed. Specifically, the depth of the concave portion 13 is, for example, the concave portion 13 having a depth of about 5 mm when the cross-section processing sample stage has a rectangular parallelepiped shape with a height of about 8 mm.

  In addition, the sample table main body 11 is formed with at least one through hole 14 penetrating from the side surface 11b to the recess 13 in the main body trunk side surface 11b. A fixing member 12 to be described later is inserted into the through hole 14. The fixing member 12 is made of, for example, a screw, and the through hole 14 constitutes a hole in which the screw-like fixing member 12 can be screwed.

  The formation position of the through hole 14 (formation position on the main body trunk side surface 11b) is not particularly limited, and the cross-section processing sample stage placed in the recess 13 is fixed by the fixing member 12 penetrating the through hole 14. It can be set as a position where it can be done. Specifically, as the height position, when the depth of the recess 13 is about 5 mm, the height position of the center position of the through hole 14 can be about 2.5 mm. Further, the horizontal position can be a position where the through hole 14 is formed so as to pass through the center of the sample table main body 11 and to be orthogonal to the formation direction of the recess 13.

  As described above, the fixing member 12 is made of a screw, for example. As shown in FIG. 2A, the fixing member 12 is inserted into a through-hole 14 formed in the sample table main body 11 and placed in the recess 13 of the sample table main body 11 and the sample table for cross section processing. The main body 11 is supported and fixed. As a result, the cross-section processing sample stage placed in the concave portion 13 of the sample stage main body 11 is prevented from being displaced or dropped from a predetermined position of the sample stage main body 11, thereby enabling accurate cross-sectional observation. To do.

  The shape of the fixing member 12 is not limited to the above-described screw shape, and may be any shape as long as the sample base body 11 and the cross section processing sample base can be fixed. The screw shape is preferable in that it can be fixed while being adjusted to the sample stage. Further, the material is not particularly limited, and it can be made of a material such as aluminum as in the case of the sample table main body 11.

  The electron microscope sample stage 10 can be integrated with a pedestal attached to a sample holder that can be mounted on a sample stage in a barrel of the electron microscope to be used. FIG. 4 is a schematic diagram showing the electron microscope sample stage 10 and the pedestal 20.

  The pedestal 20 has, for example, a disk shape or a flat plate shape, and can be attached to the sample table mounting portion 2 formed on the sample holder 1 shown in FIG. The pedestal 20 is also formed of a material that does not affect the cross-sectional observation or the like, for example, aluminum or brass.

  This pedestal 20 has a shaft 21 at a substantially central position thereof. The axis | shaft 21 is fixed perpendicularly | vertically with respect to the base 20, for example, is formed in the column shape. The shaft 21 is also formed of a material such as aluminum, for example, like the base 20.

  As shown in FIGS. 2 to 4, a hole 15 formed perpendicular to the lower surface 11 c is provided on the lower surface 11 c of the main body of the sample base 10 for electron microscope from the lower surface 11 c toward the recess 13. A shaft 21 that is erected perpendicularly to the pedestal 20 is inserted into the hole 15. Thus, by inserting the shaft 21 into the hole 15 of the electron microscope sample stage 10, the electron microscope sample stage 10 is fixed to the pedestal 20 and integrated.

  Further, by integrating the pedestal 20 with the shaft 21 vertically set up in this way and the electron microscope sample table 10, the electron microscope sample table 10 is rotated in the circumferential direction around the shaft 21. Can be made. Thereby, when performing observation with an electron microscope or the like, the electron microscope sample stage 10 on which the sample to be observed is placed can be adjusted to an appropriate angle, and more accurate observation or the like can be performed.

  The hole 15 formed from the main body trunk lower surface 11c of the electron microscope sample stage 10 may penetrate to the concave portion 13, and in the main body trunk facing the concave portion 13 from the main body trunk lower surface 11c. You may have a hole bottom part on the way.

  Further, the surface shape of the shaft 21 is not particularly limited. However, as shown in FIG. 4, the surface shape of the shaft 21 is a screw shape so that the shaft 21 can be screwed into the hole portion 15 of the electron microscope sample stage 10. It is preferable. As a result, the height position of the electron microscope sample stage 10 can be freely adjusted with respect to the base 20. In addition, by using the screw-like surface shape in this way, the electron microscope sample stage 10 can be rotated more smoothly in the circumferential direction around the shaft 21.

  The electron microscope sample stage 10 integrated with the pedestal 20 is placed on the sample stage mounting part 2 of the sample holder 1 as shown in the configuration diagram of FIG. A sample holder 1 on which a table 10 is placed is transported and attached to a sample stage 4 in a lens barrel 3 of an electron microscope.

<2. Placement of observation sample on electron microscope sample stage>
FIG. 5 is a diagram for explaining a state when an observation target sample is placed on the electron microscope sample stage 10 having the above-described configuration. As shown in FIG. 5, the cross-section processing sample stage 30 is placed and fixed on the electron microscope sample stage 10 at the position of the recess 13. In other words, the sample 40 to be observed by the electron microscope is placed on the sample table 30 for cross-section processing, subjected to the cross-section processing as a pretreatment for observation, and then placed on the sample table 30 for cross-section processing. In this state, it is placed and fixed on the electron microscope sample stage 10.

  Specifically, a procedure for placing the observation target sample 40 on the electron microscope sample stage 10 will be described.

  First, after placing the observation target sample 40 on the cross-section processing sample stage 30 and performing cross-section processing, the cross-section processing sample stage 30 on which the observation target sample 40 is placed is quickly transferred to the electron microscope sample stage 10. It is made to mount in the recessed part 13 of. As described above, since the concave portion 13 of the electron microscope sample stage 10 is formed along the shape of the cross section processing sample base 30, the cross section processing sample base 30 is easily placed in the concave portion 13. be able to.

  Next, the fixing member 12 is screwed and inserted through the through hole 14 provided in the body body side surface 11b of the electron microscope sample stage 10 with the cross section processing sample stage 30 placed in the recess 13. To go. Then, the tip end portion 12 a of the fixing member 12 comes into contact with the cross-section processing sample base 30 placed in the concave portion 13, and the fixing member 12 is screwed into the through hole 14, whereby the cross-section processing sample base 30. Is fixed to the electron microscope sample stage 10.

  Then, when the cross-section processing sample stage 30 with the observation target sample 40 placed thereon is fixed and attached to the concave portion 13 of the electron microscope sample stage 10, it is quickly attached to the lens barrel of the electron microscope. It is attached to the sample stage mounting part 2 of the sample holder 1 that can be mounted on the inner sample stage, and the cross section is observed with an electron microscope. Specifically, when the cross-section processing sample stage 30 with the observation target sample 40 placed thereon is fixed to the electron microscope sample stage 10, as shown in FIG. 20 to be placed on the sample holder 1. Then, the sample holder 1 on which the electron microscope sample stage 10 is placed is transported and attached to the sample stage 4 in the lens barrel 3 of the electron microscope, and cross-sectional observation is performed.

  Here, the electron microscope sample stage 10 according to the present embodiment can be particularly suitably used when cross-sectional observation is performed on a sample such as oxide particles that are easily altered by contact with the atmosphere. For example, in the case of oxide particles, the reactivity with water is high, and it reacts with moisture in the atmosphere only after being exposed to the atmosphere for a few minutes, thereby causing alteration of the particles. If the particles are altered in this way, the altered portion becomes a shadow in the cross-sectional observation, so that accurate cross-sectional observation as a whole cannot be performed. This alteration of particles is more likely to occur as the time of exposure to the atmosphere increases. However, in the cross-sectional observation with the conventional electron microscope, after performing the cross-section processing on the observation target sample, the sample is removed from the cross-section processing sample stage and replaced with the electron microscope sample stage. It was exposed to the atmosphere for about 5 to 10 minutes.

  On the other hand, in the electron microscope sample stage 10 according to the present embodiment, as described above, the observation target sample 40 such as oxide particles is mounted on the cross-section processing sample stage 30 used when the cross-section process is performed. The cross section processing sample stage 30 can be placed on the electron microscope sample stage 10 in the state of being placed. Therefore, unlike the conventional method, it is not necessary to remove the observation target sample from the cross-section processing sample stage and replace it with the electron microscope sample stage after the cross-section processing is completed. As a result, the observation target sample can be quickly set in the lens barrel of the electron microscope, and the time during which the observation target sample such as oxide particles is exposed to the atmosphere can be extremely short. It is possible to prevent the deterioration due to the contact.

  According to such an electron microscope sample stage 10, even if it is a sample such as an oxide particle that easily changes in quality due to contact with the atmosphere, the original state of the particle can be accurately captured, and a highly accurate cross section is obtained. Observation and particle state evaluation can be performed.

<3. Regarding cross-section processing and cross-section observation of specimens to be observed>
Here, the cross-section processing method and the cross-section observation method of the observation target sample will be described below with examples.

(Cross section processing method)
The cross-section processing method is not particularly limited, and can be performed using, for example, a cross section polisher (CP). The cross section polisher is a method of cutting a sample to perform cross-section processing by irradiating a sample exposed from a shielding plate with a broad argon ion (Ar ⁺ ) beam and performing ion etching. According to this cross section polisher, a wide range of cross-section processing can be performed, and a smooth cross-section having no processing distortion can be formed, thereby enabling cross-section observation with higher accuracy and the like.

  Specifically, in the cross section polisher, first, a sample such as an oxide particle to be observed is mixed with a resin such as a thermosetting epoxy resin to form a mixture, and the mixture is sandwiched between slide glasses or the like. Then, heat treatment is performed to cure the resin. Thus, the sample is embedded with resin (resin embedding).

  Next, the sample obtained by embedding the resin is cut to a predetermined size, and the sample is then applied to a cross section polisher sample table (cross section processing sample table) by applying wax (mounting wax) or the like. wear. At this time, the sample is pasted so as to protrude from the end of the cross section polisher sample stage.

  Then, a shielding plate is placed so that the sample protrudes immediately above the sample, the processing position is positioned with a microscope image, and the cross section is processed by irradiating an argon ion beam from above. Specifically, an argon ion beam is generated by an argon ion gun in a vacuum, and the argon ion beam is irradiated from a direction perpendicular to a sample surface that is a cross section to be manufactured. By this cross-section processing, the portion of the sample that protrudes from the shielding plate is shaved by irradiation with an argon ion beam, and the cross-section is exposed to obtain a processed cross-section. The acceleration voltage of the argon ion beam is not particularly limited and is preferably adjusted according to the characteristics of the sample, but is preferably about 3 to 6 kV.

(Section observation with electron microscope)
In the present embodiment, after performing the above-described cross-section processing, the cross-section processed sample is attached to the electron microscope sample stage while being placed on the cross-section processing sample stage. That is, as shown in FIG. 5, the observation target sample 40 that has been subjected to cross-section processing with a cross-section polisher or the like is placed on the cross-section processing sample base (cross-section polisher sample base) 30 and the cross-section thereof is maintained. The processing sample stage 30 is mounted by being placed and fixed in the recess 13 of the electron microscope sample stage 10.

  Then, this electron microscope sample stage 10 is fixed to a pedestal 20 that can be attached to and detached from the sample stage mounting portion 2 formed on the sample holder 1 of the scanning electron microscope, for example, via a shaft 21, and as shown in FIG. The sample holder 1 on which the electron microscope sample stage 10 is placed is set on the sample stage 4 in the lens barrel 3 of the electron microscope. Thereby, cross-sectional observation and cross-sectional structure analysis with an electron microscope are possible.

  Observation with an electron microscope such as a scanning microscope (SEM) can be performed according to a conventionally known method. Specifically, the observation target sample 40 having a cross-section processed is irradiated with an electron beam, and secondary electrons, reflected electrons, or transmitted electrons are detected by the irradiated electron beam, and an image of the sample to be observed is obtained. obtain. For example, in the case of an SEM, the lens barrel 3 is provided with a filament 5 for generating an electron beam, a lens system for a condenser (focusing) lens 6 and an objective lens 7, a deflection coil 8 and the like (FIG. 6). The electron beam X generated from 5 is focused by the lens system and controlled to be deflected by the deflection coil 8, and directed toward the observation target sample 40 of the electron microscope sample stage 10 placed on the sample stage 1 below the lens barrel 3. By irradiating, an image of the sample is obtained. When acquiring the secondary electron image by the detected electrons, set the acceleration voltage, condenser lens current value, objective aperture diameter, working distance, etc. in consideration of the resolution, etc., and then shoot to acquire the image data. Can be done.

  In addition, for example, the crystal orientation can be derived by acquiring a diffraction pattern derived from a crystal structure by an EBSD detector mounted on a scanning electron microscope and performing crystallographic analysis (EBSD method).

  Examples of the present invention will be described below, but the present invention is not limited to the following examples. In this example and comparative example, the oxide particles that react with moisture in the atmosphere and easily change in quality when exposed to the atmosphere are used as the observation sample, and the sample is processed by cross-section processing. Observation (cross-sectional observation) was performed on the cross section.

[Example 1]
(Cross section processing)
Oxide particles were used as a sample to be observed, and first, the sample and a thermosetting epoxy resin (G2 manufactured by Gatan) were sufficiently mixed to prepare a mixture. Next, a nitroflon adhesive tape (manufactured by Nitto Denko Corporation) is pasted on the surface of the slide glass, the mixture prepared thereon is placed, sandwiched between another slide glass, and 120 ° C. for 5 minutes on the hot plate. The resin was cured under conditions.

  After that, the cured and resin-embedded sample is cut into a size of about 8 mm × 10 mm with a razor and then attached to a cross section polisher sample table coated with wax (JEOL mounting wax), and the cross section polisher ( Cross-section processing was performed using SM-09010 manufactured by JEOL Ltd. and setting the acceleration voltage of the argon ion beam to 5 kV.

(Section observation with electron microscope)
After that, the cross-section processed sample was mounted on the scanning electron microscope (SEM) sample stage while it was mounted on the cross-section polisher sample stage, and was quickly moved to the SEM column for cross-sectional observation by SEM. .

  Here, as shown in the schematic diagram of FIG. 2, the electron microscope sample stage has a cylindrical shape with a diameter of 15 mm and a height of 10 mm, and a concave portion with a depth of 5 mm is formed on the upper surface of the main body trunk. In addition, a sample stage was used in which one through-hole penetrating from the side surface to the concave portion was formed on the side surface of the main body (a height position of 2.5 mm from the upper surface of the main body). The sample to be observed is attached to the electron microscope sample stage by placing the cross section polisher sample stage with the cross-section processed sample placed in the recess formed on the upper surface of the main body of the sample stage. Attached by fixing. A hole was provided in the lower surface of the main body of the sample base from the lower surface toward the recess, and was fixed to a pedestal attached to a sample holder that can be mounted on the sample stage in the SEM column. The sample stage and the pedestal were fixed by inserting a shaft erected perpendicularly to the pedestal into a hole provided in the lower surface of the main body of the sample stage.

  The cross section of the sample was observed using SEM (S-4700, manufactured by Hitachi High-Technologies Corporation) under the conditions of an acceleration voltage of 1 kV and a working distance of 6.1 mm.

(Section observation result)
FIG. 7 shows an SEM image obtained by cross-sectional observation. As is clear from the observation photograph of FIG. 7, the obtained particle cross section was not observed at all in the state where the oxide particles as the sample were altered, and an accurate cross section observation could be performed.

  As described above, by using the above-described electron microscope sample stage, it is possible to prevent the oxide particles from being altered, and to accurately grasp the state of the original particle cross section and to perform high-precision cross-section observation. I understood.

[Comparative Example 1]
(Cross section processing)
In the same manner as in Example 1, cross-section processing using a cross-section polisher was performed using oxide particles as an observation target sample.

(Section observation with electron microscope)
Next, in Comparative Example 1, the cross-section processed sample is removed from the cross section polisher sample table using precision tweezers, attached to the existing SEM observation sample table with double-sided tape, and quickly moved to the SEM column. The cross-sectional shape of the sample was observed by SEM. Similarly to Example 1, the cross-sectional observation was performed using SEM (S-4700, manufactured by Hitachi High-Technologies Corporation) under the conditions of an acceleration voltage of 1 kV and a working distance of 6.1 mm.

(Section observation result)
FIG. 8 shows an SEM image obtained by cross-sectional observation. As is apparent from the observation photograph of FIG. 8, it can be seen that a plurality of altered portions (circled portions in FIG. 8) of the oxide particles as the sample are observed in the obtained particle cross section. For this reason, the state of the original oxide particles could not be accurately grasped, and high-precision cross-section observation could not be performed.

  This alteration of the sample is considered to have occurred because the sample reacted with moisture in the atmosphere. That is, by performing the work of replacing the cross-section processed sample from the cross-section processing sample stage to the electron microscope sample stage over a period of several minutes, a time to react with moisture in the atmosphere occurs, and as a result, It is thought that the sample has been altered.

  DESCRIPTION OF SYMBOLS 10 Sample stand for electron microscopes, 11 Sample stand main body, 11a Main body trunk | drum upper surface, 11b Main body trunk | drum side surface, 11c Main body trunk | drum lower surface, 12 Fixing member, 13 Recessed part, 14 Through-hole, 15 hole part, 20 Base, 21 axis 30 Sample stage for cross-section processing, 40 Sample to be observed

Claims (7)

A sample stage for an electron microscope for performing cross-sectional observation of a sample after performing cross-section processing,
A sample base body having a recess of a predetermined depth on the upper surface of the main body body, and at least one through-hole penetrating from the side surface to the recess is formed on the side surface of the main body body;
A fixing member inserted into the through hole,
A cross-section processing sample stage on which the cross-section processed sample is placed is placed in a concave portion of the sample base body, and is fixed and attached by the fixing member penetrating the through hole. Sample stage for microscope observation. A pedestal attached to a sample holder that can be mounted on a sample stage in a barrel of an electron microscope;
A shaft fixed perpendicular to the pedestal,
A hole is formed in the sample base body perpendicularly to the bottom surface of the main body from the bottom surface of the main body toward the concave portion, and the shaft is inserted into the hole so that the sample is inserted. The sample base for an electron microscope according to claim 1, wherein the base body is fixed to the pedestal.   3. The sample stage for an electron microscope according to claim 2, wherein the sample stage main body is rotatable in a circumferential direction of the shaft while being inserted into the shaft.   The depth of the recess of the sample table main body is shorter than the length in the height direction of the sample table for cross-section processing placed in the recess, and when the sample table for cross-section processing is placed, The sample stage for an electron microscope according to any one of claims 1 to 3, wherein an upper part of the sample stage protrudes from the recess.   The sample table for cross-section processing is a sample table for a cross cushion polisher, and a sample embedded with a resin is placed on the sample table, and the cross section of the sample is cut. The sample stand for electron microscopes of any one of Claim 4.   6. The electron microscope sample stage according to claim 1, wherein in the cross-sectional observation, a secondary electron image of the cross-section processed sample is observed using a scanning electron microscope. A sample cross-sectional observation method of performing cross-sectional processing of a sample to be observed and observing a cross-section of the sample obtained by processing using an electron microscope,
The sample stage of the electron microscope is
A sample base main body having a concave portion of a predetermined depth on the upper surface of the main body body, and at least one through-hole penetrating from the side surface to the concave portion on the side surface of the main body body;
A fixing member inserted into the through hole,
With the cross-section processed sample placed on the cross-section processing sample base, the cross-section processing sample base is placed in the concave portion of the sample base main body and fixed by the fixing member penetrating the through hole. And observing the cross section of the sample with an electron microscope.