JP2018163109A - Sample holder for cross-sectional sample preparation device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample holder used with a cross-sectional sample preparation device, which allows for easily preparing an oblique section, preparing highly reproducible samples, and performing highly accurate inspection.SOLUTION: A sample holder 1 used with a cross-sectional sample preparation device comprises a cuboid-shaped base material 2 having one surface configured to act as a sample holding surface 3 for holding a sample S, where the sample holding surface 3 of the base material 2 is sloped. This obliquely positions the sample S with respect to a horizontally moving cutting blade 9, which allows the sample S to be obliquely sliced off by moving the cutting blade 9 in such an arrangement, making an oblique section 27 on the sample S.SELECTED DRAWING: Figure 5

Description

  The present invention relates to a sample holder used in a cross-sectional sample preparation apparatus that holds a sample used for inspection of an electron microscope or the like.

When performing cross-sectional observation with a transmission electron microscope (TEM), a scanning electron microscope (SEM), or the like, it is necessary to cut out a sample sample using a cross-sectional sample preparation device such as a microtome or an ultramicrotome.
As such a cross-section sample preparation device, a sample holding means having a sample holder for holding a sample, a position adjusting means for adjusting the height and inclination of the sample holding means, and a cutting blade for cutting the sample are moved in the horizontal direction. What is provided with the cutting | disconnection means is known (for example, refer patent document 1).

Conventionally, when performing detailed layer analysis in cross-sectional observation of an electron microscope or the like, a method of observing a shaved cross-sectional portion (oblique cross-section) by shaving a sample obliquely using the cross-sectional sample preparation apparatus as described above Has been done.
In the cross-section sample preparation apparatus as described above, the cutting blade moves in the horizontal direction. Therefore, when using such a cross-section sample preparation apparatus to prepare an oblique cross section in the sample, the position adjustment means uses the sample holder of the sample holding means Was tilted, the cutting blade was moved with respect to the slanted sample, and the sample was cut off obliquely to produce a slanted cross section.

JP 2003-130767 A

However, since the cross-section sample preparation apparatus as described above normally uses the sample holding means in a horizontal position, when the sample holding means is inclined to produce an oblique cross section, the inclined sample holding means is placed in the horizontal position. There was a problem that the work was troublesome.
In addition, since the adjustment of the inclination angle is performed by a manual handle operation by the operator, it is difficult to finely adjust the angle, and it is difficult to produce an oblique section having the same angle again.
An object of the present invention is to provide a sample holder that can be used for a cross-section sample preparation apparatus that can easily produce an oblique cross-section and can perform high-reproducibility sample preparation and high-precision inspection.

  In order to achieve the above-mentioned object, the invention according to claim 1 is a sample holder used in a cross-section sample preparation apparatus comprising a rectangular parallelepiped base and one surface of the base being a sample holding surface for holding a sample. And the said base | substrate has the said sample holding surface inclined, It is characterized by the above-mentioned.

  According to a second aspect of the present invention, the base body according to the first aspect is configured by a plurality of rectangular parallelepiped blocks, and the plurality of blocks constituting the base body have a predetermined sample holding surface of the base body. It is characterized by being appropriately selected from a plurality of prepared blocks so as to have an inclination angle of.

  The invention described in claim 3 is characterized in that a shift prevention means is provided in the plurality of blocks constituting the base body described in claim 2.

According to the sample holder of claim 1, since the sample holding surface of the substrate is inclined, when the sample holding means is in the horizontal position, the sample is disposed obliquely with respect to the cutting blade that moves in the horizontal direction. Is done. When the cutting blade is moved in this state, the sample is cut off obliquely, and an oblique cross section is produced in the sample. Therefore, it is possible to easily produce an oblique cross section without operating the position adjusting means and inclining the sample holding means as in the prior art.
Further, according to the sample holder of the first aspect, for example, if a sample holder having a sample holding surface with an inclination angle of 1 ° is used, anyone can easily produce an oblique cross section with an angle of 1 °. As described above, even when an oblique section with a small angle is manufactured, a sample with high reproducibility can be manufactured, and as a result, a highly accurate inspection can be performed.

  According to the sample holder of the second aspect, the base body is composed of a plurality of rectangular parallelepiped blocks, and the plurality of blocks constituting the base body are arranged such that the sample holding surface of the base body has a predetermined inclination angle. Since the block is appropriately selected from a plurality of prepared blocks, for example, an inclined block having one inclined surface and a horizontal block having two horizontal surfaces facing each other are prepared. As appropriate, the inclination angle of the sample holding surface can be easily adjusted, and an oblique cross section having a desired angle can be easily produced.

  According to the sample holder of the third aspect, since the displacement prevention means is provided in the plurality of blocks constituting the substrate, the image is not observed even in cross-sectional observation with an electron microscope in which the image is blurred by slight vibration. The inspection can be performed accurately without blurring.

It is a perspective view which shows the 1st example of the sample holder used for the cross-section sample preparation apparatus which concerns on this invention. It is explanatory drawing of the sample holder shown in FIG. It is a perspective view which shows a cross-section sample preparation apparatus. It is explanatory drawing which shows the state which fixed the sample holder shown in FIG. 1 to a fixed clamp. It is process drawing which shows the process of producing an oblique cross section. It is an expansion process figure which shows the process of producing an oblique cross section. It is a perspective view which shows the 2nd example of the sample holder used for the cross-section sample preparation apparatus which concerns on this invention. It is explanatory drawing which shows the state which combined the block. It is an exploded view of the block provided with the slip prevention means.

Hereinafter, embodiments of a sample holder used in a cross-sectional sample preparation apparatus according to the present invention will be described in detail with reference to the drawings.
1 to 6 show a first example of the embodiment of the sample holder used in the cross-sectional sample preparation apparatus according to the present invention. FIG. 1 is a perspective view showing the sample holder of the first example, and FIG. FIG. 3 is a perspective view showing a cross-section sample preparation device, FIG. 4 is an explanatory view showing a state in which the sample holder shown in FIG. 1 is fixed to a fixed clamp, and FIG. FIG. 6 is an enlarged process diagram showing a process for producing an oblique section.

  The sample holder 1 of this example includes a rectangular parallelepiped base 2. The base body 2 is formed of a material having conductivity, and is preferably formed of a material having high conductivity such as brass, copper material, aluminum material, or the like.

  The base 2 is a sample holding surface 3 on which one surface holds the sample S. In this example, the resin film 4 is provided between the sample S and the sample holding surface 3, but the sample S may be held directly on the sample holding surface 3. The resin film 4 is provided so that the cutting edge does not come into contact with the sample holding surface 3 when an oblique cross section is formed on the sample S, and a resin film having an appropriate thickness is preferable. As the resin film 4, for example, a PET film or a PP film is used.

  In the present invention, the sample holding surface 3 of the substrate 2 is formed in an inclined shape. The inclined sample holding surface 3 is a flat inclined surface from the top 5 to the bottom 6, and the surface facing the sample holding surface 3 is a horizontal plane. Further, the left and right surfaces with respect to the inclination direction of the inclined sample holding surface 3 are formed in the same shape.

  The inclination angle of the sample holding surface 3 (the angle formed between the horizontal line L passing through the top 5 of the sample holding surface 3 and the sample holding surface 3) θ is appropriately set according to the angle of the oblique cross section to be produced on the sample S. That is, when an oblique cross section having an angle of 1 ° is formed on the sample S, the sample holder 1 having an inclination angle θ of the sample holding surface 3 of 1 ° is used.

FIG. 3 is a perspective view of a cross-sectional sample preparation apparatus in which a sample holder is used.
The cross-sectional sample preparation apparatus shown in FIG. 3 is a so-called sliding microtome, and includes a sample holding means 7 having a sample holder 1, a position adjusting means 8 for adjusting the height and inclination of the sample holding means 7, A cutting means 10 that movably supports the cutting blade 9 is provided.

The sample holding means 7 includes a fixed clamp 11 that clamps and fixes the sample holder 1 and a stage 12 to which the fixed clamp 11 is attached.
The fixed clamp 11 includes a base 13 on which the sample holder 1 is placed, a fixed arm 14 and a movable arm 15 for fixing the sample holder, and a movable arm opening / closing lever 16, and the movable arm opening / closing lever 16 is operated. Then, the movable arm 15 is opened, the sample holder 1 is placed on the base 13 between the fixed arm 14 and the movable arm 15, the movable arm opening / closing lever 16 is operated to close the movable arm 15, and the fixed arm 14 The sample holder 1 is sandwiched and fixed between the movable arm 15 and the movable arm 15.
The stage 12 has a dish shape with a wall portion 17 formed around it, and the fixed clamp 11 is attached to the stage surrounded by the wall portion 17.

  The position adjusting means 8 includes an elevating mechanism 18 and an elevating adjustment handle 19. The elevating mechanism 18 is fixed to the stage 12 via the intermediary table 20, and the stage 12 moves up and down together with the elevating mechanism 18 by operating the elevating adjustment handle 19.

  The cutting means 10 includes a cutting blade 9 for cutting and cutting the sample S, a cutting blade holding portion 21 for supporting and fixing the cutting blade 9, and a rail 22 for moving the cutting blade in the horizontal direction. The cutting edge 9 supported and fixed to the portion 21 is configured to move in the horizontal direction along the rail 22.

Next, a method for producing an oblique cross section in a sample using the cross-section sample preparation apparatus to which such a sample holder is attached will be described.
First, a sample holder 1 having a sample holding surface 3 having a desired inclination angle is prepared (FIG. 5A), and a resin film 4 cut larger than the sample S is attached to the sample holding surface 3 of the substrate 2 with a double-sided tape or the like (FIG. 5). 5B). At this time, the resin film 4 is pasted with its end aligned with the top 5 of the sample holding surface 3. Although depending on the thickness of the resin film 4, when the resin film 4 is thin, it is preferable to overlap a plurality of resin films 4 so that the thickness of the entire resin film is about 1 mm.
And the sample S (paper piece) is affixed on the resin film 4 with a double-sided tape etc. (FIG. 5C). At this time, similarly to the resin film 4, the sample S is attached with its end portion aligned with the top portion 5 of the sample holding surface 3.

  The sample holder 1 holding the sample S in this way is placed on the base 13 of the fixed clamp 11 so that the cutting edge 9 passes from the bottom 6 to the top 5 of the sample holding surface 3, and is movable with the fixed arm 14. It is clamped by the arm 15 and fixed to the fixed clamp 11. Then, the fixed clamp 11 with the sample holder 1 fixed is attached to the stage 12 set in the horizontal position, the lift adjustment handle 19 is operated, the stage 12 is moved upward, and the sample S is moved to a predetermined height. (FIGS. 3 and 4). And the cutting blade holding | maintenance part 21 is moved along a horizontal direction, and the upper surface of the sample S is cut off diagonally with the cutting blade 9, and as shown in FIG. 6, the oblique cross section 23 is produced in the sample S (FIG. 5D). .

  According to the sample holder 1 of the first example as described above, the sample holding surface 3 of the base 2 is inclined, so that when the stage 12 is in the horizontal position, the sample S is in the moving direction of the cutting edge 9. It is arranged diagonally. When the cutting blade 9 is moved in this state, the sample S is cut off obliquely, and the oblique section 23 can be easily produced.

  In addition, according to this example, for example, if the sample holder 1 having the inclination angle θ of the sample holding surface 3 of 1 ° is used, anyone can easily produce the oblique section 23 having an angle of 1 °. As described above, even when the oblique section 23 having a small angle is produced, the sample S with high reproducibility can be produced, and as a result, a highly accurate inspection can be performed. In particular, even in the case of a thin sample such as paper, by reducing the inclination angle of the sample holding surface, the length of the cross section becomes longer than when the angle is large, and a wide range of cross sections are observed. Therefore, a highly accurate inspection can be performed.

  Further, in the sample holder 1 of this example, since the base 2 is formed of a conductive material, the sample holder 1 holding the sample S can be set on an electron microscope as it is to observe a cross section.

  7 to 9 show a second example of the sample holder according to the present invention, FIG. 7 is a perspective view showing the sample holder of the second example, and FIG. 8 is an explanatory view showing a state in which the blocks are combined. 9 is an exploded view of a block provided with a shift prevention means. The same parts as those in the first example are denoted by the same reference numerals, and the description thereof is omitted.

In the sample holder 24 of this example, the base body 25 is composed of a plurality of blocks 26 having a rectangular parallelepiped shape.
The plurality of blocks 26 constituting the base body 25 are provided with an inclined block 28 having an inclined surface 27 formed in an inclined shape, and a horizontal block 30 having a horizontal surface 29 on two opposing surfaces. The sample holding surface 3 is appropriately selected so as to have a predetermined inclination angle.

  That is, the base 25 is a plurality of blocks 26 appropriately selected from a plurality of blocks 26 (inclined blocks 28 and horizontal blocks 30) prepared in advance so that the sample holding surface 3 of the base 25 has a predetermined inclination angle. It is configured. The plurality of blocks 26 are coupled to each other by screws (not shown) and fixed. Further, the block 26 is formed of a material having conductivity, and is preferably formed of a material having high conductivity such as, for example, brass, copper material, or aluminum material.

  In the inclined block 28, the surface facing the inclined surface 27 is a horizontal surface, and the left and right surfaces are formed in the same shape with respect to the inclination direction of the inclined surface 27. Further, the shape of the horizontal block 30 is not particularly limited as long as it has horizontal surfaces 29 on at least two opposing surfaces. However, in this example, the horizontal blocks 30 have a complete rectangular parallelepiped shape in which the opposing surfaces are formed in the same shape.

  In this example, as the block 26, a plurality of inclined blocks 28 having different angles of the inclined surface 27, for example, the angles of the inclined surface 27 are 0.5 °, 1.0 °, 2.0 °, and 3.0 °. An inclined block 28 and a horizontal block 30 are prepared.

  As shown in FIG. 8A, when the inclination angle θ of the sample holding surface 3 of the substrate 25 is set to 0.5 °, the inclined block 28 in which the angle of the inclined surface 27 is 0.5 °, and the horizontal block 30 are stacked and formed such that the inclined surface 27 and the horizontal surface 29 become the upper surface.

  As shown in FIG. 8B, when the inclination angle θ of the sample holding surface 3 of the substrate 25 is set to 1.5 °, an inclined block 28 having an inclined surface 27 having an angle of 1.0 °; The inclined blocks 28 with the inclined surfaces 27 having an angle of 0.5 ° are stacked and formed such that the inclined surfaces 27 are the upper surfaces.

  Further, as shown in FIG. 8C, when the inclination angle θ of the sample holding surface 3 of the substrate 25 is set to 5.0 °, an inclined block 28 in which the angle of the inclined surface 27 is 2.0 °; The inclined blocks 28 having the inclined surfaces 27 having an angle of 3.0 ° are stacked and formed such that the inclined surfaces 27 are the upper surfaces.

  Since the other configuration is the same as that of the first example, the description of the first example is cited. The production of the oblique section 23 using the sample holder 24 of the second example is the same as that of the first example, so the description of the first example is cited.

  According to such a second example, as shown in FIGS. 8A to 8C, the inclination angle θ of the sample holding surface 3 can be set by appropriately combining the inclination block 28 and the horizontal block 30 prepared in advance. It can be adjusted easily, and the oblique section 23 having a desired angle can be easily produced.

  Further, as shown in FIG. 9, misalignment prevention means 31 may be provided in a plurality of blocks 26 constituting the base body 25. The misalignment prevention means 31 is configured such that one of the stacked blocks 26 is provided with a convex portion 32, the other block 26 is provided with a concave portion 33, and the convex portion 32 and the concave portion 33 are fitted to each other. It is possible to prevent the deviation. In this example, as for the slip prevention means 31, although the convex part 32 becomes rail shape and the recessed part 33 becomes groove shape, the shape of the slip prevention means 31 is not specifically limited. In the cross-sectional observation using the electron microscope, the image is blurred even with a slight vibration. Even when set to, the image can be accurately inspected without blurring.

1, 24 Sample holder 2, 25 Base 3 Sample holding surface 4 Resin film 5 Top 6 Bottom 7 Sample holding means 8 Position adjusting means 9 Cutting edge 10 Cutting means 11 Fixed clamp 12 Stage 13 Base 14 Fixed arm 15 Movable arm 16 Movable Arm opening / closing lever 17 Wall portion 18 Elevating mechanism 19 Elevating adjustment handle 20 Intermediary base 21 Cutting blade holding portion 22 Rail 23 Oblique section 26 Block 27 Inclined surface 28 Inclined block 29 Horizontal surface 31 Displacement preventing means 32 Convex portion 33 Concavity S Sample L Horizontal line θ Inclination angle

Claims (3)

A sample holder for use in a cross-section sample preparation device comprising a rectangular parallelepiped base and one surface of the base serving as a sample holding surface for holding a sample,
A sample holder used in a cross-section sample preparation apparatus, wherein the substrate has an inclined sample holding surface.   The base body is composed of a plurality of rectangular parallelepiped blocks, and the plurality of blocks constituting the base body are appropriately selected from the plurality of prepared blocks so that the sample holding surface of the base body has a predetermined inclination angle. The sample holder used for the cross-section sample preparation device according to claim 1, wherein the sample holder is selected.   The sample holder used in the cross-section sample preparation apparatus according to claim 2, wherein a misalignment prevention means is provided in a plurality of blocks constituting the substrate.

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