JP3223464B2 - Sample processing equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an STM (Scanning
Tunneling Microscope, AF
M (Atomic Force Microscope), M
FM (Magnetic Force Microscope, magnetic force microscope),
A sample processing apparatus for peeling or cleaving a sample in order to observe the three-dimensional shape of the sample surface with atomic-level resolution using a scanning probe microscope such as a scanning ion conductance microscope (SICM). More particularly, the present invention relates to a sample processing apparatus for peeling or cleaving used in a vacuum.

[0002]

2. Description of the Related Art FIG. 9 is a schematic explanatory view of a scanning probe microscope apparatus. In FIG. 9, the scanning probe microscope apparatus U
Are the image observation chamber 01 and the sample pre-processing chamber 0 which are evacuated.
2 and a sample introduction chamber 03. The image observation room 0
An on-off valve 04 is provided between 1 and the sample pre-processing chamber 02 so that they can be shut off in a sealed state. Also,
A similar on-off valve 06 is provided between the sample pretreatment chamber 02 and the sample introduction chamber 03. An STM, which is an example of the scanning probe microscope, is accommodated in the image observation room 01.

In the sample pretreatment chamber 02, a new sample (sample to be subjected to peeling or cleavage processing) and a probe (probe) carried from the sample introduction chamber 03 through the on-off valve 06 are temporarily held. A parking place 07 used for temporarily holding used samples and probes before carrying them out to the sample introduction chamber 03 is provided. The parking 07 includes a turntable 08, a plurality of holder support stages 09 (or peeling member support stages 09 ') supported on the turntable 08, a plurality of probe support stages (not shown), and the turntable 08. And a turntable transport rod 011 for rotating, tilting, moving back and forth, and the like.

The sample introduction chamber 03 is connected to a cylindrical sample introduction guide 014 which supports a sample introduction rod 013 having a chuck 012 mounted at the tip so as to be able to advance and retreat. The retractable sample introduction rod 013 holds the sample holder on which a new sample is mounted by the chuck 014 at the tip thereof, and carries the sample holder into the holder support stage 09 of the parking 07, or mounts the used sample. It is used to carry out the sample holder from the parking area 07.

[0005] The sample preliminary processing chamber 02 is connected to a cleavage sample processing apparatus 016 for performing a cleavage process on a new sample held in the parking area 07. Also,
The sample pre-processing chamber 02 has a chuck 017 at its tip.
A cylindrical sample exchange guide 019 that supports the sample exchange rod 018 to which the is mounted so as to be able to advance and retreat is connected. The retractable sample exchange rod 018 has a chuck 0 at the tip thereof.
17, the holder support stage 0 of the parking 07
The sample holder on which the peeled or cleaved sample 9 is mounted is carried into the image observation room 01, and the sample holder with the used sample mounted thereon is transported from the image observation room 01 to the parking place 07. Used to do.

Next, referring to FIG. 10, the cleavage processing apparatus 0
Sixteen conventional techniques will be described. FIG. 10 is an explanatory view of a conventional example of the cleavage processing apparatus 016. In FIG. 10A, a sample holder H for holding a sample is supported on the holder support stage 09. In the sample holder H,
A positioning portion Ha is formed on the surface holding the sample S, and the chuck 012 shown in FIG.
A held portion Hb held at 018 is formed. The sample S has a holding portion S1 held by a sample holder H,
And a protruding portion S2 protruding from the sample holder H. The cleaving sample processing apparatus 016 has a cleaving mechanism transport member 021 and an operating rod 022 that can move forward and backward with respect to the holder support stage 09. Cleavage mechanism transport member 02
A cleavage positioning member 023 is attached to the tip of the first member 1. The cleavage positioning member 023 is provided with an engaging portion 024 that engages with the positioning portion Ha for positioning with respect to the sample holder H. . Cleavage positioning member 0
23 is advanced toward the holder support stage 09, and the engaging portion 024 is engaged with the positioning portion Ha (see FIG. 10B). The cleavage positioning member 023 is stopped at the cleavage position.

[0007] A clamp 026 is provided on the cleavage positioning member 023 so as to face the sample S held by the sample holder H. In FIG. 10B, when the cleavage positioning member 023 is at the sample cleavage position, the tip of the sample S held by the sample holder H is connected to the clamp 026.
It is in the state inserted. In FIG. 10A, the protruding portion S2 of the sample is provided on the cleavage positioning member 023.
The pressing element 027 that presses downward is rotatably supported around the axis 028. The pressing element 027 receives a force in a counterclockwise direction by a spring mechanism (not shown), and is always in contact with the operating rod 022. The operating rod 022 has a function of moving forward and pressing the contact surface with the pressing element 027 rightward in the figure. In FIG. 10B, when the contact surface with the pressing element 027 is pressed to the right by the operating rod 022, the tip of the pressing element 027 rotates around the axis 028, and the projecting portion S2 of the sample S moves downward. When pressed, the sample S is cleaved, and a cleavage plane is formed in the holding portion S1 of the sample S. At the lower end of the cleavage positioning member 023, a collection container 029 for collecting cleaved sample pieces is supported, and the cleaved sample pieces fall into the collection container 029.

FIG. 11 is an explanatory view of a conventional example of a peeling sample processing apparatus for performing a peeling process. 11, in the sample processing apparatus for peeling, a peeling member supporting stage 09 'is used instead of the holder supporting stage 09 provided in the parking lot 07 shown in FIG. The sample processing apparatus for peeling is constituted by the sample exchange rod 018 which can be moved back and forth, the sample holder for peeling H ', and the peeling member support stage 09'. In FIG. 11A, a chuck 0 provided at the tip of the sample exchange rod 018 (see FIG. 9) capable of moving back and forth.
17 holds the sample holder H '. The sample S is, as shown in FIG. 11A, the sample holder H ′.
Is held in close contact with the sample holding surface. A metal fitting 031 is attached to the surface of the sample S in advance. An opening 032 is formed in the fitting 031. The sample separation member 033 is supported by the holder support stage 09 at a position facing the opening 032.

The sample exchange rod 018 is moved to the holder support stage 0
When the sample holder H 'is moved forward toward 9 and the sample holder H' is moved forward, the sample peeling member 033 penetrates through the opening 032 of the metal fitting 031 as shown in FIG. 11B. At this time, when the turntable 08 (not shown) is tilted so that the peeling member support stage 09 ′ is moved upward, the sample peeling member 033 is moved to the opening portion 032.
It is designed to be hung on. Then, when the sample holder H 'is moved backward as it is, the bracket 031 is moved.
Is peeled from the surface of the sample S to form a peeled surface on the surface of the sample. The metal fitting 031 peeled off from the surface of the sample S is held while being hooked on the sample peeling member 033.

[0010]

However, in the prior art, in FIG. 10B, in order to take out a sample piece dropped into the collection container 029 after cleaving the sample S in FIG. , The vacuum environment in the sample pretreatment chamber 02 must be completely released. Therefore, after the sample piece dropped into the collection container 029 is taken out of the sample pre-processing chamber 02, the sample pre-processing chamber 0
It takes a long time to evacuate 2. In addition, the cleaved sample pieces may not fall into the collection container 029 but remain in the sample pretreatment chamber 02. In a vacuum environment, such a residue becomes a gas emission source and causes a failure to maintain a vacuum.

In FIG. 11B, the metal fitting 031
Is peeled off from the surface of the sample S, the sample peeling member 03
3 may fall into the sample pretreatment chamber 02 without being caught on the sample pretreatment chamber 02. An adhesive is attached to the metal fitting 031 that has fallen into the sample pretreatment chamber 02, and this adhesive becomes a gas release source, which causes a failure to maintain a vacuum. Further, in order to take out the metal fittings 031, the adhesive tape, etc. which have fallen into the sample preliminary processing chamber 02, the vacuum environment in the sample preliminary processing chamber 02 must be released. For this reason, it takes a long time to complete the work of taking out the metal fittings 031, the adhesive tape, and the like that have fallen into the collection container 029 to the outside of the sample pre-processing chamber 02, and to evacuate the sample pre-processing chamber 02 again. .

Further, after the sample S is introduced into the sample preliminary processing chamber 02, an operation of performing a heat treatment and forcibly evacuating to prepare a vacuum environment may be performed. At this time, when the pressure-sensitive adhesive such as the metal fitting 031 and the pressure-sensitive adhesive tape affixed to the sample S is dropped due to low heat resistance, or the amount of gas released by the heat treatment becomes extremely large, and the desired degree of vacuum cannot be obtained. There is. Further, in the case of the above-mentioned conventional technology, the cleavage and peeling operations of the sample are performed at different places. For this reason, there is also a problem that the device becomes complicated.

The present invention has been made in view of the above circumstances, and has the following content as an object. (O01) An object of the present invention is to provide a sample processing apparatus for peeling or cleaving which has a simple structure and which is easy to operate and which can take out a cleaved and peeled sample piece out of the apparatus (in the atmosphere) while maintaining vacuum.

[0014]

Next, the present invention devised to solve the above-mentioned problems will be described. Elements of the present invention are used to facilitate correspondence with elements of the embodiments described later. , The reference numerals of the elements of the embodiment are enclosed in parentheses. The reason why the present invention is described in correspondence with the reference numerals of the embodiments described below is to facilitate understanding of the present invention and not to limit the scope of the present invention to the embodiments.

(1st invention) In order to solve the aforementioned problem,
The sample processing apparatus of the first invention of the present application has the following requirements: (Y01) a sample holding surface (H1a; H3)
a) a sample holder (H1; H3) for holding a plate-shaped sample (S) protruding from a), (Y02) the sample holder (H1; H3)
Sample holder (33 + 34 + 36 + 37) having a holder chuck (36) for holding the holder and a chuck support member (34) for supporting the holder chuck (36), and for transferring the sample holder (H1; H3) to a predetermined working position. ,
(Y03) The cleavage member holder (F), the cleavage support shaft (39) supported by the cleavage member holder (F), and the slit (41b) into which the sample (S) is inserted are formed by the cleavage support shaft ( 39) A cylindrical wall (41a) formed parallel to
(F + 38 + 39 + 41) comprising a bottomed cylindrical member (41) rotatable about the cleavage support shaft (39), and (Y04) a holder support stage for supporting the cleavage member holder (F). (8), (Y0
5) A stage moving mechanism (23) for moving the holder support stage (8) in a direction perpendicular to the sample transport direction of the sample transport member (33 + 34 + 36 + 37) and in a direction perpendicular to the cleavage support shaft (39).

(Second Invention) A sample cleavage device according to a second invention of the present application is the sample cleavage device according to the first invention,
(Y06) The slit (4) supported by the cleavage support shaft (39) and having the following requirements:
The cleavage unit (F + 38 +) having a cleavage contact member (39a) capable of contacting the sample (S) inserted in 1b).
39 + 41).

(Third Invention) A sample processing apparatus according to a third invention of the present application has the following requirements.
(Y01 ') a sample holder (H2; H4) for holding the sample (S) on the sample holding surface (H2a; H4a); (Y02) a holder chuck (36) for holding the sample holder (H2; H4) and the holder A sample transport member (33 + 34 + 3) having a chuck support member (34) for supporting the chuck (36) and transporting the sample holder (H2; H4) to a predetermined work position;
6 + 37), (Y07) a peeling member holder (G), a peeling support shaft (46) supported by the peeling member holder (G),
And a peeling unit (G + 38 + 46 + 47) having a cylindrical wall (47a) having a surface with which the sample (S) comes in contact and having a bottomed cylindrical member (47) rotatable around the peeling support shaft (46). (Y08) a holder supporting stage (8) for supporting the peeling member holder (G), (Y09) the holder supporting stage (8) is perpendicular to the sample transport direction of the sample transport member (33 + 34 + 36 + 37) and is used for the peeling. A stage moving mechanism (23) for moving in a direction perpendicular to the support shaft (46);

[0018]

Next, the operation of the present invention having the above-mentioned features will be described. (Operation of the First Invention) In the sample cleavage device of the first invention of the present application having the above-mentioned features, the plate-shaped sample (S) held by the sample holder (H1; H3) is connected to the sample holder (H1). H
It protrudes from the sample holding surface (H1a; H3a) of 3). The sample transport member (33 + 34 + 36 + 37) has a holder chuck (36) for holding the sample holder (H1; H3) and a chuck supporting member (34) for supporting the holder chuck (36). H1; H3)
To a predetermined working position. The holder support stage (8) supports the cleavage member holder (F) of the cleavage unit (F + 38 + 39 + 41). The cleavage unit holder (F) includes the cleavage unit (F + 38 + 39 + 4).
The cleavage support shaft (39) of 1) and the slit (41b) for inserting the sample (S) are provided by the cleavage support shaft (39).
A cylindrical member (41) having a bottom, which has a cylindrical wall (41a) formed in parallel with and is rotatable around the cleavage support shaft (39). The stage moving mechanism (23)
The holder support stage (8) is connected to the sample transfer member (3).
(3 + 34 + 36 + 37) perpendicular to the sample transport direction and perpendicular to the cleavage support shaft (39).

The holder supporting stage (8) is moved by the stage moving mechanism (23), and the slit (41) is moved.
b) and adjust the position of the sample transport member (33+
34 + 36 + 37), the sample (S) is adjusted by adjusting the position of the sample held in the sample holder (H1; H3).
Can be inserted into the slit (41b).
With the sample (S) inserted into the slit (41b), either the sample (S) or the slit (41b) is moved by one of the stage moving mechanism (23) and the sample transport member (33 + 34 + 36 + 37). The other is moved in a direction perpendicular to the slit (41b). With this movement, the cleavage unit (F + 38 + 39)
The cleavage member holder (F) of (+41) and the cleavage support shaft (39) supported by the cleavage member holder (F) move.
When the sample (S) is inserted into a slit (41b) formed in a cylindrical wall (41a) of the bottomed cylindrical member (41), the bottomed cylindrical member (41) is supported by a cleavage support shaft (39). ) Try to rotate around. However, since the sample (S) is inserted into the slit (41b) of the cylindrical wall (41a), the bottomed cylindrical member (41) does not rotate and exerts a force to break the sample (S). . That is, the sample (S) held in the sample holder (H1; H3) receives a force from the slit (41b) in the rotating direction of the bottomed cylindrical member (41), and the sample holder (H1; H3).
The portion protruding from the sample holding surface (H1a; H3a) of H3) is cut off. Then, a cleavage plane is formed on the sample (S) supported by the sample holder (H1; H3). The cut-off sample piece falls into the bottomed cylindrical member (41) and is collected. For this reason, it is possible to prevent the cut-off sample pieces from falling or falling outside the sample processing apparatus for cleavage,
The work of collecting the sample piece can be performed easily.

(Operation of the Second Invention) In the sample cleavage device of the second invention of the present application, the cleavage unit (F + 38 +
The cleavage contact member (39a) supported by the cleavage support shaft (39 + 41) can contact the sample (S) inserted into the slit (41b). With the sample (S) inserted into the slit (41b), the stage moving mechanism (23) and the sample transport member (33+
34 + 36 + 37), the sample (S)
Alternatively, one of the slits (41b) is moved relative to the other in a direction perpendicular to the slit (41b). With this movement, the cleavage unit (F + 38 + 39 + 41)
Cleaved member holder (F) and said cleaved member holder (F)
The cleavage support shaft (39) supported on the sample (S)
And move relatively. At this time, the cleavage contact member (39a) of the cleavage unit (F + 38 + 39 + 41)
Presses the end of the sample (S) inserted in the slit (41b) in a direction perpendicular to the slit (41b). This pressing force acts as a force point with the opening of the slit (41b) as a fulcrum. Therefore, the sample (S) is broken off at the opening of the slit (41b). The cut-off sample piece falls into the bottomed cylindrical member (41) and is collected. The specimen collected inside the bottomed cylindrical member (41) is placed in the cleavage unit (F + 38 + 3).
9 + 41) and transported outside the apparatus. For this reason, the cleaved sample piece can be prevented from peeling or dropping outside the cleavage sample processing apparatus, and the work of collecting the sample piece can be performed easily.

(Operation of the Third Invention) In the sample cleavage apparatus of the third invention of the present application, the sample holder (H2; H4) holds the sample on the sample holding surface (H2a; H4a). The sample transport member (33 + 34 + 36 + 37) is the sample holder (H
2; a holder chuck (36) for holding H4) and a chuck support member (34) for supporting the holder chuck (36), and transporting the sample holder (H2; H4) to a predetermined working position. . Holder support stage (8)
Supports the peeling member holder (G) of the peeling unit (G + 38 + 46 + 47). The peeling member holder (G) has a peeling support shaft (46) of the peeling unit (G + 38 + 46 + 47) and a cylindrical wall (47a) with which the sample (S) is brought into contact, and the peeling support shaft is provided. (46)
A bottomed cylindrical member (47) rotatable therearound is supported.
An adhesive tape for peeling off the surface of the sample (S) abutting on the outer peripheral surface of the cylindrical wall (47a);
An adhesive or the like is stuck and applied before use. The stage moving mechanism (23) moves the holder supporting stage (8) in a direction perpendicular to the sample transport direction of the sample transport members (33 + 34 + 36 + 37) and in a direction perpendicular to the peeling support shaft (46).

By moving the holder supporting stage (8) by the stage moving mechanism (23), the cylindrical wall (47) is moved.
a) and adjusting the position of the sample transfer member (33+
34 + 36 + 37), the position of the sample held in the sample holder (H2; H4) is adjusted to obtain the sample (S).
Can be brought into contact with the cylindrical wall (47a). While the sample (S) is in contact with the cylindrical wall (47a), the stage moving mechanism (23) and the sample transport member (33)
+ 34 + 36 + 37) to move either the sample (S) or the cylindrical wall (47a) relative to the other in a direction perpendicular to the peeling support shaft (46). With this movement, the peeling unit (G + 38 + 46)
The peeling member holder (G) of (+47) and the peeling support shaft (46) supported by the peeling member holder (G) move relatively to the sample (S). At this time, the bottomed cylindrical member (4) rotatable around the peeling support shaft (46).
7) is rotated because the surface of the cylindrical wall (47a) is in contact with the sample (S). An adhesive tape, an adhesive or the like is attached to the surface of the cylindrical wall (47a) of the bottomed cylindrical member (47),
If it is applied, the sample (S) surface is peeled off with the rotation of the cylindrical wall (47a), and a peeled surface is formed on the sample (S) surface. The surface of the sample (S) peeled off with an adhesive tape, an adhesive, or the like stuck and applied to the surface of the cylindrical wall (47a) is the same as the peeling unit (G + 38 + 46 +
47) and transported outside the apparatus. For this reason, the cleaved sample piece can be prevented from peeling or falling out of the cleavage sample processing apparatus, and the work of collecting the sample piece can be performed easily.

[0023]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the sample processing apparatus of the present invention will be described below with reference to the drawings, but the present invention is not limited to the following embodiments. In order to facilitate the understanding of the following description, coordinate axes X orthogonal to each other in the drawing.
An axis, a Y axis, and a Z axis are defined, and the arrow X direction is forward, the arrow Y direction is left, and the arrow Z direction is upward. In this case, the direction opposite to the X direction (−X direction) is backward, and the direction opposite to the Y direction (−Y
Direction) is to the right, and the opposite direction to the Z direction (-Z direction) is downward. In addition, the front-rear direction including X direction and -X direction or X direction
The term “axial direction” refers to the left-right direction or the Y-axis direction including the Y direction and the −Y direction, and the up-down direction or the Z-axis direction includes the Z direction and the −Z direction. Furthermore, in the figure, "○"
The symbol with “•” in it means an arrow pointing from the back of the paper to the front, and the symbol with “X” in “○” means an arrow pointing from the front to the back of the paper. Shall be.

(Embodiment 1) A first embodiment of a sample processing apparatus according to the present invention will be described with reference to FIGS. FIG. 1 is a schematic explanatory view of a scanning probe microscope apparatus provided with a cleavage sample processing apparatus which is a first embodiment of the sample processing apparatus of the present invention. FIG.
FIG. 2 is an explanatory view of the stage moving mechanism of FIG. FIG. 3 is an enlarged explanatory view of Example 1 of the sample processing apparatus provided in the scanning probe microscope apparatus of FIG. 1, FIG. 3A is a front view, and FIG. 3B is a plan view. FIG. 4 is a view for explaining the operation of the sample processing apparatus shown in FIG. 3 according to the first embodiment. FIG. 4A is a front view, and FIG.
Is a plan view. In FIG. 1, the image observation room 1 has the S
TM is accommodated. An openable and closable internal gate valve 3 is provided between the image observation chamber 1 and the sample pretreatment chamber 2 disposed adjacent to the image observation chamber 1 so as to seal off the space therebetween. The sample preliminary processing chamber 2 is provided with a parking 4.

In FIG. 2, the parking 4 includes a turntable 7 rotatably supported by a table support member 6, a plurality of holder support stages 8 supported on the turntable 7, and a plurality of probe support stages (see FIG. 2). (Not shown). A gear 7a for transmitting a rotational force is formed on the outer periphery of the lower portion of the turntable 7. The holder support stage 8 includes a sample holder H1 (see FIG. 2) for holding a sample, a cleavage device holder F (FIG. 3,
4). The probe support stage (not shown) is a member for supporting a replacement probe (not shown) for replacing a probe (probe) used in the STM.

The table support member 6 is fixedly supported by a table transfer cylinder 9. The inner peripheral surface of the table transfer cylinder 9 is processed so as to have a low coefficient of friction, and the table rotation shaft 11 is supported by the inner peripheral surface of the table transfer cylinder 9. The table rotating shaft 1
A gear (bevel gear) 12 is fixed to one end. The gear 12 meshes with a gear (bevel gear) 13 rotatably supported by the table support member 6. The gear 13 is disposed so as to mesh with the gear 7a of the turntable 7.

A flange portion 14a of a cylindrical table transfer guide 14 is provided on the side wall of the sample pretreatment chamber 2 (see FIG. 2).
Are connected via a bellows 15. The flange portion 14a is positioned and supported by a plurality of tension springs 16a spaced apart in the circumferential direction and a position adjusting screw 16b whose tip abuts against the side wall of the sample pretreatment chamber 2. The periphery of the portion of the table transfer cylinder 9 protruding from the sample pretreatment chamber 2 is sealed by a cylindrical table transfer guide 14 and a bellows 15. A bearing 17 for rotatably and slidably supporting the table transfer cylinder 9 is provided in the table transfer guide 14. Rear ends of the table transfer cylinder 9 and the table rotation shaft 11 ((-Y in FIG. 2)
Cylindrical magnetic members 18 and 19 each having a permanent magnet are fixed to the side end). Further, corresponding to the cylindrical magnetic members 18 and 19, the outer peripheral surface of the table transport guide 14 has magnetic members 21 and 2 having permanent magnets.
2 are slidably and rotatably provided. The sliding of the magnetic members 21 and 22 can be performed integrally.

When the operator rotates the magnetic member 21, the magnetic member 18 rotates simultaneously with the movement of the magnetic member 21. The magnetic member 18 and the table transfer cylinder 9 rotate integrally, and the turntable 7 is tilted accordingly. When an operator rotates the magnetic member 22, the magnetic member 19 is simultaneously rotated in accordance with the movement of the magnetic member 22. When the magnetic member 19 rotates, the table rotation shaft 11 rotates, and the gear (bevel gear) 12 provided at the tip of the table rotation shaft 11 rotates. The rotation of the gear (bevel gear) 12 causes the gear (bevel gear) 1 to rotate.
3 and the gear 7a are rotated, and the turntable 7 is rotated. Further, the magnetic member 21,
When the magnetic members 21 and 22 slide together, the magnetic members 21 and 22
The magnetic members 18 and 19 also move in the Y-axis direction at the same time in accordance with the movement of. And the magnetic member 1
When 8, 19 move in the Y-axis direction, the table transfer cylinder 9 and the table rotation shaft 11 move in the Y-axis direction,
Accordingly, the turntable 7 is moved in the Y-axis direction. The turntable 7 has a function of moving the holder support stage 8 by tilting, rotating, and moving back and forth (Y-axis direction) of the turntable 7. The stage moving mechanism 23 of the present invention is constituted by the elements indicated by the reference numerals 7 to 22.

In FIG. 1, an openable / closable internal gate valve 2 is provided between the sample pretreatment chamber 2 and a sample introduction chamber 25 disposed adjacent to the pretreatment chamber 2 so as to seal off the space therebetween.
6 are provided. A cylindrical sample introduction guide 27 is connected to the sample introduction chamber 25. Inside the sample introduction guide 27, a sample introduction rod 28 is provided.
7 is provided so as to be able to advance and retreat along the axis. At the tip of the sample introduction rod 28, a chuck 2 for holding the sample holder H1 and the cleavage device holder F1 (see FIGS. 3 and 4).
9 are provided. A chuck 29 provided at the tip of the sample introduction rod 28 has a chuck 36 described later shown in FIGS.
The same is used. The sample introduction guide 27
A cylindrical magnetic member 31 having a permanent magnet is rotatably and slidably supported on the outside of the sample holder H. The sample holder H1 and the cleavage device holder F ( 3 and 4) can be slid and rotated along the axis of the sample introduction guide 27. Here, positions where the axis of the sample introduction rod 28 (not shown) intersects the parking 4 are defined as Q1 and Q2, respectively.

In FIG. 1, a cylindrical sample exchange guide 33 is connected to the sample pre-processing chamber 2. Inside the sample exchange guide 33, a sample exchange rod (chuck support member) 34 is supported so as to be able to advance and retreat along the axis of the sample exchange guide 33. A chuck 36 for gripping the sample holder H1 is provided at the tip of the sample exchange rod 34. A cylindrical magnetic member 37 having a permanent magnet is slidably supported outside the sample exchange guide 33, and a cylindrical magnetic member (shown in FIG. Zu) is fixed. The magnetic member (not shown) fixed to the sample exchange rod 34 is configured to slide in conjunction with the sliding movement of the magnetic member 37. Here, the position where the axis of the sample exchange rod 34 intersects the parking 4 is defined as Q3.

In FIG. 3A, a cleavage device holder F is supported on the holder support stage 8. A cleavage support shaft 39 is supported by the cleavage device holder F via a support plate 38. The cleavage support shaft 39 has a notch 39a as a cleavage contact member at the upper end thereof. The support plate 38 is provided with a cleavage member 41 rotatable around a cleavage support shaft 39. The cleavage member 4
1 has a cylindrical wall 41a, and a slit 41b into which a sample is inserted is formed in the cylindrical wall 41a. An inclined groove 41c is provided below the slit 41b. The cleavage units (F + 38 + 39 + 41) of the first invention of the present application are constituted by the reference numerals F, 38, 39, and 41. In FIG. 3A, the sample holder H1 is gripped by the chuck 36 at the tip of the sample exchange rod 34. A plate-shaped sample S is held on the sample holding surface H1a of the sample holder H1. The plate-shaped sample S is placed on the sample holder H1.
And a protruding portion Sb protruding from the sample holding surface H1a of the sample holder H1.

(Operation of the First Embodiment) Next, the operation of the first embodiment having the above-described configuration will be described. In FIG. 1, the cleavage device holder F is introduced into a sample introduction chamber 25 and is gripped by a chuck 29 provided at the tip of the sample introduction rod 28. The cleavage device holder F is supported by the holder support stage 8 at the position Q1. FIG.
In the above, the sample S is introduced into the sample introduction chamber 25 while being held by the sample holder H1. The sample holder H1 holding the sample S is gripped by a chuck 29 provided at the tip of the sample introduction rod 28, and is mounted on the holder support stage 8 at the position Q2. The holder support stage 8 supporting the sample holder H1 is transported to a position Q3 by the rotation of the turntable 7. At the position Q3, the sample holder H1 is
4 and is taken out of the holder support stage 8 by being gripped by the chuck 36 at the tip. After the sample holder H1 is taken out of the holder support stage 8, the cleavage device holder F supported by the holder support stage 8 is moved to the position Q3. At this time, as shown in FIG. 3, the cleavage device holder F at the position Q3 and the sample holder H1 held by the chuck 36 at the tip of the sample exchange rod 34 are arranged at positions facing each other. When the sample exchange rod 34 is advanced in this state, FIG.
State.

In FIG. 4A, the sample exchange rod 34 has moved in the (-Y) direction, and the protruding portion Sb of the sample S has been inserted into the slit 41b. At this time, the sample holding surface H1a of the sample holder H1 is in contact with the cylindrical wall 41a, and the tip of the holder protruding portion Sb is located at an engagement position with the notch 39a. In FIG. 4B, the turntable 7 is rotated to move the holder support stage 8 in the X direction. Along with the movement of the holder support stage 8, the tip of the protruding portion Sb of the sample S becomes
Direction. At this time, a load (pressing force) having the cylindrical wall 41a forming the slit 41b as a fulcrum and the tip of the sample S as a power point acts on the sample S. At this time, the sample S is cut off at the slit 41b (a fulcrum portion), and a cleavage surface is obtained in the sample Sa remaining on the sample holder H1 side. Further, the holder supporting stage 8 is set to X
The cleavage member 41 rotates around the cleavage support shaft 39, and the protruding portion Sb of the sample S that has been cut off is moved.
The tip comes off the notch 39a. The protruding portion Sb of the sample S, the tip of which is displaced from the notch 39a, slides down the inclined groove 41c provided below the slit 41b and is collected inside the cleavage member 41.

The sample S collected inside the cleavage member 41
Can be taken out from the sample pre-processing chamber 2 to the sample introduction chamber 25 by using the sample introduction rod 28 together with the cleavage device holder F. Since this operation is performed by evacuating the sample introduction chamber 25, it is not necessary to completely release the vacuum in the sample preliminary processing chamber 2, and the workability can be improved. Further, since the protruded portion Sb of the sample S that has been cut off does not fall into the cleavage member 41, it is difficult for the protruded portion Sb to remain in the sample pretreatment chamber 2, so that unnecessary gas release can be prevented and a vacuum environment can be maintained. can do.

Second Embodiment Next, a second embodiment of the sample processing apparatus of the present invention will be described with reference to FIGS. FIG. 5 is an enlarged explanatory view of a second embodiment of the sample processing apparatus used in the scanning probe microscope apparatus of FIG. 1 and corresponds to FIG. 3 of the first embodiment. FIG. 6 is a diagram for explaining the operation of the second embodiment of the sample processing apparatus shown in FIG.
FIG. In the description of the second embodiment, components corresponding to the components of the first embodiment are denoted by the same reference numerals, and detailed description thereof will be omitted. The second embodiment is different from the first embodiment in the following points.
In other respects, the configuration is the same as that of the first embodiment.

In FIG. 5A, a peeling device holder G is supported on the holder supporting stage 8 instead of the cleavage device holder F of the first embodiment. A separation support shaft 46 is supported by the separation device holder G via the support plate 38. The support plate 38 is provided with a cylindrical peeling member 47 rotatable around the peeling support shaft 46.
A fixing member 48 is provided on the separation support shaft 46 so that the separation member 47 does not move upward. The peeling member 47 has a cylindrical wall 47a. A slit 47b (see FIG. 5B) is formed in the cylindrical wall 47a. The peeling unit (G + 38) of the present invention is obtained from the peeling device holder G, the support plate 38, the cleavage support shaft 46, and the peeling member 47.
+ 46 + 47). A double-sided adhesive tape 49 is wound around a cylindrical wall 47a of the peeling member 47, and an end of the adhesive tape 49 is accommodated inside the cylindrical wall 47a through a slit 47b. The chuck 36 holds a sample holder H2 instead of the sample holder H1. The sample holding surface H2a of the sample holder H2
The sample S is placed on the sample holding surface H2a 'of the sample holder H2.
And are held substantially parallel to it.

(Operation of Second Embodiment) Next, the operation of the second embodiment having the above-described configuration will be described. From the state shown in FIG. 5, the sample S held by the sample holder H2 is removed from the peeling member 47.
When the sample exchange rod 34 is moved to the right ((-Y) direction) until it comes into contact with the adhesive tape 49 wound around the cylindrical wall 47a of FIG. 6A, the turntable 7 (see FIGS. 1 and 2) is rotated to move the holder support stage 8 in the X direction (see FIG. 6B).
With the movement of the holder support stage 8, the peeling member 47 rotates around the peeling support shaft 46, and the surface of the sample S is peeled off by the adhesive tape 49, so that the sample holder H2
A peeled surface is formed on the surface of the sample S remaining on the side.

Since the sample piece peeled off by the adhesive tape 49 is adhered to the adhesive tape 49, the sample pretreatment chamber 2 is moved from the sample introduction chamber 2 using the sample introduction rod 28 together with the peeling device holder. 25. Since this operation is performed by evacuating the sample introduction chamber 25, it is not necessary to completely release the vacuum in the sample preliminary processing chamber 2, and the workability can be improved. Thereafter, the internal gate valve 26 is shut off, the sample introduction chamber 25 is opened to the atmosphere, and the sample piece and the peeling holder are taken out. In the sample processing apparatus of Example 2, the surface of the sample was peeled off with the adhesive tape 49 wound around the cylindrical wall 47a.
Since the peeled sample piece is held by the adhesiveness of the adhesive tape 49, it is difficult for the sample piece to fall into the sample pretreatment chamber 2 as in the above-described conventional technique. Further, as described above, the adhesive tape 49 is initially wound around the cylindrical wall 47a of the peeling member 47, and is separated from the sample S. Therefore, the sample S is introduced into the sample pretreatment chamber 2. After that, heat treatment can be performed before forcible evacuation for preparing a vacuum environment. For this reason, outgassing from the sample S can be reduced, and the degree of vacuum can be increased.

Third Embodiment Next, a third embodiment of the sample processing apparatus of the present invention will be described with reference to FIG. FIG. 7 is an enlarged explanatory view of Embodiment 3 of the sample processing apparatus. Example 3 is a sample cleavage device. In the description of the third embodiment, components corresponding to the components of the first embodiment are denoted by the same reference numerals, and detailed description thereof will be omitted. The third embodiment differs from the first embodiment in the following points.
In other respects, the configuration is the same as that of the first embodiment.

In FIG. 7A, a sample holder H3 is held by the chuck 36 instead of the sample holder H1 of the first embodiment. The sample S is held in the sample holder H3 so as to face the slit 41b of the cleavage member 41. In the third embodiment, when inserting the sample S into the slit 41b, the turntable 7 is moved in the (-X) direction. Then, as shown in FIG. 7B, the sample S is cleaved by moving the sample holder H3 in the (-Y) direction. In the third embodiment, similarly to the first embodiment, the protruding portion Sb of the sample S collected inside the cleavage member 41 can be taken out of the sample pretreatment chamber 2 together with the cleavage device holder F. For this reason, it is not necessary to completely release the vacuum in the sample preliminary processing chamber 2, and operability can be improved. Further, the protruding portion Sb of the sample S that has been broken off does not fall into the cleavage member 41 and the sample pretreatment chamber 2
Since it does not easily remain in the interior, unnecessary gas emission can be prevented, and a vacuum environment can be maintained.

(Embodiment 4) Next, a sample processing apparatus according to a fourth embodiment of the present invention will be described with reference to FIG. FIG. 8 is an enlarged explanatory view of Embodiment 4 of the sample processing apparatus. Example 4 is a sample peeling device. In the description of the fourth embodiment, the same reference numerals are given to the components corresponding to the components of the second embodiment, and the detailed description is omitted. The fourth embodiment differs from the second embodiment in the following points.
The other points are the same as those of the second embodiment.

In FIG. 8A, a sample holder H4 is held by the chuck 36 instead of the sample holder H2 of the second embodiment. The sample S is held by the sample holder H4 so as to face the cylindrical wall 47a of the peeling member 47. In the fourth embodiment, the turntable 7 (see FIG. 1)
Is moved in the (-X) direction so that the adhesive tape 49 wound around the cylindrical wall 47a is brought into contact with the surface of the sample S. Then, as shown in FIG. 8B, the sample holder H4 is moved in the (-Y) direction (turntable 7 is rotated) to peel off the sample S, thereby forming a peeled surface on the surface. Also in the fourth embodiment, since the sample piece peeled off with the adhesive tape 49 is attached to the adhesive tape 49 similarly to the second embodiment, the sample piece is removed from the sample pretreatment chamber 2 together with the peeling device holder H4. Can be taken out. For this reason, it is not necessary to completely release the vacuum in the sample preliminary processing chamber 2, and operability can be improved. In the sample peeling device of Example 2, the surface of the sample is peeled by the adhesive tape 49 wound around the cylindrical wall 47a, and the peeled sample piece is held by the adhesiveness of the adhesive tape 49. Thus, the sample piece is less likely to fall into the sample pretreatment chamber 2.

(Modifications) Although the embodiments of the present invention have been described in detail, the present invention is not limited to the above-described embodiments, but falls within the scope of the present invention described in the appended claims. Thus, various changes can be made. Modified embodiments of the present invention will be exemplified below. (H01) The adhesive tape 49 can be wound around the cylindrical wall 41a of the cleavage member 41 of the first and third embodiments to be used as a sample peeling device. (H02) In each embodiment, the cleavage member 41 and the peeling member 47 are open at the top, but a lid such as a wire mesh can be provided.

(H03) In the first and third embodiments, a plurality of slits 41b can be formed in the cleavage member 41. In this case, the position of the slit 41b can be moved by rotating the cleavage member 41 by pressing the position shifted from the center of the cleavage member 41 at the tip of the sample S a plurality of times. Then, a plurality of samples S can be cleaved by one cleavage member 41. The cleavage member 41 can be rotated using a drive device such as a motor. (H04) In the second and fourth embodiments, if the length of the cylindrical stripping member 47 along the circumference is longer than the length of the surface to be stripped of the sample, the stripping member 47 is further rotated to obtain 1
The plurality of samples S can be separated by the separation members 47. The rotation of the peeling member 47 can be performed manually or by using a driving device such as a motor as in the case of (H03). (H05) In the second and fourth embodiments, the cylindrical wall 47a
Instead of wrapping the adhesive tape 49 around the cylindrical wall 47a
It is possible to apply an adhesive on the surface. (H06) The present invention can be applied to a sample processing apparatus for peeling or cleaving a sample in a liquid or air, in addition to a sample processing apparatus for peeling or cleaving a sample in a vacuum in addition to a sample processing apparatus for peeling or cleaving a sample in a vacuum. is there.

[0045]

The above-described sample processing apparatus of the present invention has the following effects. (E01) The cleaved or peeled sample piece can be taken out of the apparatus (in the atmosphere) while maintaining the vacuum. (E02) It is possible to provide a sample processing apparatus for peeling or cleaving having a simple structure and good operability.

[Brief description of the drawings]

FIG. 1 is a schematic explanatory view of a sample processing apparatus for peeling or cleavage according to the present invention.

FIG. 2 is an explanatory diagram of the stage moving mechanism of FIG. 1;

FIG. 3 is an enlarged explanatory view of the sample cleavage device in FIG. 1;

FIG. 4 is a diagram illustrating the operation of the sample cleavage device in FIG. 3;

FIG. 5 is an enlarged explanatory view of a sample peeling device;
This corresponds to FIG.

FIG. 6 is an explanatory view of the operation of the sample peeling device, corresponding to FIG.

FIG. 7 is an enlarged explanatory view of a sample cleavage device according to a third embodiment.

FIG. 8 is an enlarged explanatory view of a sample peeling device according to a fourth embodiment.

FIG. 9 is a schematic explanatory view of a conventional sample processing apparatus for peeling or cleaving to which the present invention is applied.

FIG. 10 is an enlarged explanatory view of a mechanism for cleaving the sample observed in FIG. 9;

FIG. 11 is an enlarged explanatory view of a mechanism for peeling the sample observed in FIG. 9;

[Explanation of symbols]

8. Holder supporting stage (H1a; H2a; H3a; H4a)
... sample holding surface, (H1; H2; H3; H4) ... sample holder,
23: Stage moving mechanism, 34: Chuck support member (sample exchange rod), 36: Holder chuck, (33 + 34 + 3)
6 + 37): sample transport member, F: cleavage member holder, 39
... Cleaving support shaft, 39a ... Cleaving contact member, (41; 4)
7) ... cylindrical member with bottom, (41a; 47a) ... cylindrical wall, 41
b: slit into which the sample is inserted, (F + 38 + 39 + 4
1) Cleavage unit, S: sample, G: peeling member holder,
46: peeling support shaft, (G + 38 + 46 + 47): peeling unit.

──────────────────────────────────────────────────の Continued on the front page (58) Fields surveyed (Int. Cl. ⁷ , DB name) G01N 1/28 H01J 37/20 JICST file (JOIS)

Claims (3)

(57) [Claims] 1. A sample processing apparatus having the following requirements: (Y01) a sample holder for holding a plate-like sample protruding from a sample holding surface; and (Y02) a holder chuck for holding the sample holder. A sample transport member having a chuck support member for supporting the holder chuck and transporting the sample holder to a predetermined working position; (Y03) a cleavage member holder; a cleavage support shaft supported by the cleavage member holder;
And a cleavage unit in which the slit into which the sample is inserted has a cylindrical wall formed parallel to the cleavage support axis and is formed of a bottomed cylindrical member rotatable around the cleavage support axis, (Y04) A holder support stage for supporting the cleavage member holder; and (Y05) a stage moving mechanism for moving the holder support stage in a direction perpendicular to the sample transport direction of the sample transport member and perpendicular to the cleavage support axis. 2. The sample processing apparatus according to claim 1, wherein the sample processing apparatus satisfies the following requirements: (Y06) the sample processing apparatus is supported by the cleavage support shaft and can contact a sample inserted into the slit. The cleavage unit having a cleavage contact member. 3. A sample processing apparatus having the following requirements: (Y01 ′) a sample holder for holding a sample on a sample holding surface, (Y02) a holder chuck for holding the sample holder, and the holder chuck. (Y07) a peeling member holder, a peeling support shaft supported by the peeling member holder, and a sample supporting member for transporting the sample holder to a predetermined working position. A peeling unit having a cylindrical wall having a surface in contact with the bottom and having a bottomed cylindrical member rotatable around the peeling support shaft; (Y08) a holder supporting stage for supporting the peeling member holder; and (Y09) the holder. A stage moving mechanism for moving a support stage in a direction perpendicular to the sample transport direction of the sample transport member and perpendicular to the separation support shaft.