JP2017026574A - Sample stage and sample processing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample stage for processing ion beams, easy to handle.SOLUTION: There is provided the sample stage for holding a sample S when the sample S is irradiated with ion beams and is processed. The sample stage includes: a sample fixing part 20, to which the sample S is fixed; a supporting part 10, which supports the sample fixing part 20. The sample fixing part 20 is protruded from the supporting part 10 in a first direction A and is made of a metal having rolled tissues of crystal grains of which longer direction corresponds to a second direction B, which intersects with the first direction A in the planer view.SELECTED DRAWING: Figure 2

Description

  The present invention relates to a sample stage and a sample processing method.

  As a method for preparing a sample for a transmission electron microscope (TEM), the sample is processed and extracted by a focused ion beam (FIB) apparatus, the extracted sample is fixed to a sample stage, and the sample fixed to the sample stage is fixed. A method of performing additional machining with a broad ion beam apparatus is known.

  In the sample processed by the FIB apparatus, highly accelerated Ga ions used in the FIB processing are implanted into the sample surface, so there are thick damaged layers of about 10 nm to 40 nm on the front and back surfaces of the sample observation surface, respectively. To do.

  In the damaged layer, the sample is amorphized, the atoms are transferred, the composition is changed, and the crystal is crystallized, so that the sample is different from the original sample state. For example, when the thickness of the sample is processed to 100 nm with an FIB apparatus, if the damage layer to be formed is 30 nm, the thickness of the part that maintains the original state of the sample is 40 nm. Therefore, even if such a sample is observed by TEM, detailed analysis is difficult. In addition, in order to observe a sample with higher resolution by TEM, if the thickness of the sample is processed to 30 nm or less with an FIB apparatus, the part that maintains the original state of the sample is lost, and the entire sample is damaged. Since it becomes a layer, the original state of the sample cannot be observed.

  Therefore, in order to perform detailed TEM observation of a sample processed by the FIB apparatus, it is necessary to thin the damaged layer generated by the FIB processing. Therefore, when preparing a sample for TEM, the damaged layer is removed by processing the sample processed by the FIB apparatus with a low acceleration ion beam using a broad ion beam apparatus.

  A minute sample that has been processed into a size of about several tens of μm square and about 1 μm in thickness by the FIB apparatus is difficult to handle, such as being transferred to another apparatus, and is thus fixed to the sample stage. After the sample fixed on the sample stage is processed to a thickness of 100 nm or less suitable for TEM observation by the FIB apparatus, the damage layer is removed by the broad ion beam apparatus.

  As such a sample stage, for example, in Patent Document 1, a silicon substrate is used as a material, and a step structure in which a sample fixing part protrudes from a base part and decreases in thickness toward a tip part is manufactured by a semiconductor process technology. A sample stage is disclosed.

JP 2006-226970 A

  However, since the sample base of Patent Document 1 is made of a silicon substrate, it may be cracked or chipped when fixing the sample to the sample fixing part or carrying the sample base with tweezers. Attention was necessary.

The present invention has been made in view of the above problems, and one of the objects according to some aspects of the present invention is to provide an easy-to-handle sample stage. Another object of some aspects of the present invention is to provide a sample processing method using the sample stage.

(1) The sample stage according to the present invention is:
A sample stage for processing an ion beam used for holding the sample when processing the sample by irradiating the sample with an ion beam,
A sample fixing part to which the sample is fixed;
A support part supporting the sample fixing part;
Including
The sample fixing portion is made of a metal having a rolling structure that is protruded from the support portion in a first direction and that is composed of crystal grains having a longitudinal direction in a second direction that intersects the first direction in a plan view. .

  In such a sample stage, since the sample fixing part is made of a metal having a rolled structure, for example, the sample fixing part has a sample in comparison with a case where the sample fixing part is made of a material such as silicon or ceramics. It is easy to handle without fixing or cracking when carrying the sample table with tweezers.

  Further, in such a sample stage, a metal having a rolled structure composed of crystal grains having a sample fixing portion protruding from the support portion in the first direction and having a longitudinal direction in the second direction intersecting the first direction in plan view. Therefore, when processing a sample with an ion beam, it is thicker than when the sample fixing part protrudes in the plan view and the longitudinal direction of the crystal grains is the same direction while preventing reattachment. A sample with small unevenness can be obtained.

(2) In the sample stage according to the present invention,
The sample fixing part may have a root part connected to the support part and a tip part having a smaller width than the root part.

  In such a sample stage, it is possible to prevent the sample fixing portion from being bent or rounded and deforming its shape, and to reduce the processing amount when processing the tip of the sample fixing portion with a focused ion beam or the like. Can be reduced.

(3) In the sample stage according to the present invention,
At least a part of the outer edge of the support portion has an arc shape in plan view,
The distal end portion of the sample fixing portion may be located at the center of the arc in plan view.

(4) In the sample stage according to the present invention,
The angle formed by the first direction and the second direction in plan view may be 45 degrees or more and 90 degrees or less.

  With such a sample stage, it is possible to obtain a sample with smaller thickness unevenness.

(5) In the sample stage according to the present invention,
The angle formed by the first direction and the second direction in plan view may be 90 degrees.

  With such a sample stage, it is possible to obtain a sample with smaller thickness unevenness.

(6) In the sample stage according to the present invention,
The metal constituting the sample fixing part may be copper, molybdenum, rhodium, ruthenium, rhenium, beryllium, titanium, or an alloy containing at least one of these metals.

(7) The sample stage according to the present invention is:
A sample stage for processing an ion beam used for holding the sample when processing the sample by irradiating the sample with an ion beam,
A sample fixing part to which the sample is fixed;
A support part supporting the sample fixing part;
Including
The sample fixing part is made of a material made of crystal grains protruding from the support part in a first direction and having a longitudinal direction in a second direction intersecting the first direction.

  In such a sample stage, the sample fixing part protrudes from the support part in the first direction and is made of a material composed of crystal grains having a longitudinal direction in the second direction intersecting the first direction in plan view. When processing a sample with an ion beam, a sample with less thickness unevenness can be obtained as compared with the case where the direction in which the sample fixing portion protrudes and the longitudinal direction of the crystal grains are the same in plan view.

(8) The sample stage according to the present invention is:
A sample stage for ion beam processing, having a sample fixing part to which a sample is fixed, and fixed in a plan view so that the tip side of the sample protrudes from the end surface of the sample fixing part,
The sample fixing part is made of a metal having a rolled structure made up of crystal grains having a longitudinal direction in a direction intersecting with the direction of the normal of the end face of the sample fixing part in plan view.

  In such a sample stage, since the sample fixing part is made of a metal having a rolled structure, for example, the sample fixing part has a sample in comparison with a case where the sample fixing part is made of a material such as silicon or ceramics. It is easy to handle without fixing or cracking when carrying the sample table with tweezers.

  Further, in such a sample stage, the sample fixing part is made of a metal having a rolling structure made of crystal grains having a longitudinal direction in a direction intersecting with the direction of the normal of the end face of the sample fixing part in plan view. Therefore, when processing a sample with an ion beam, it is possible to obtain a sample with less thickness unevenness compared to the case where the perpendicular direction of the end surface of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view. Can do.

(9) The sample processing method according to the present invention includes:
A sample fixing part to which the sample is fixed, and a support part supporting the sample fixing part, wherein the sample fixing part protrudes from the support part in a first direction and intersects the first direction. Preparing a sample stage composed of a metal having a rolled structure composed of crystal grains having a longitudinal direction in two directions;
Fixing the sample to the sample fixing part;
Processing the sample fixed to the sample stage using an ion beam;
including.

  In such a sample processing method, since the sample fixing part of the sample stage is made of a metal having a rolled structure, it is easy to handle. Further, in such a sample processing method, the sample fixing portion of the sample stage protrudes from the support portion in the first direction, and is formed of crystal grains having a longitudinal direction in the second direction intersecting the first direction in plan view. Since it is made of a metal having a structure, in the process of processing a sample with an ion beam, the thickness unevenness is larger than that in the plan view when the protruding direction of the sample fixing portion and the longitudinal direction of the crystal grains are the same direction. A small sample can be obtained.

(10) In the sample processing method according to the present invention,
In the step of fixing the sample to the sample fixing portion, the sample may be fixed to the tip portion of the sample fixing portion such that the tip side of the sample protrudes from the sample fixing portion.

(11) In the sample processing method according to the present invention,
In the step of processing the sample fixed to the sample stage using an ion beam, the ion beam is applied to the sample fixed to the tip of the sample fixing unit from the base side of the sample fixing unit. It may be irradiated.

  In such a sample processing method, a sample with less thickness unevenness can be obtained as compared with the case where the direction in which the sample fixing portion protrudes and the longitudinal direction of the crystal grains are the same in plan view.

(12) In the sample processing method according to the present invention,
Prior to the step of fixing the sample to the sample fixing portion, a step of thinning the sample fixing portion using an ion beam may be included.

  In such a sample processing method, since the thickness of the sample fixing portion can be reduced, the sample fixed on the sample stage can be attached to an electron microscope or the like while preventing reattachment in ion beam processing (broad ion beam processing). When introduced and analyzed, system noise can be reduced.

(13) A sample processing method according to the present invention includes:
A sample fixing part to which the sample is fixed, and a support part supporting the sample fixing part, wherein the sample fixing part protrudes from the support part in a first direction and intersects the first direction. Preparing a sample stage composed of a material composed of crystal grains having a longitudinal direction in two directions;
Fixing the sample to the sample fixing part;
Processing the sample fixed to the sample stage using an ion beam;
including.

  In such a sample processing method, the sample fixing portion of the sample stage protrudes from the support portion in the first direction, and is composed of a material composed of crystal grains having a longitudinal direction in the second direction intersecting the first direction in plan view. Therefore, when processing a sample with an ion beam, it is possible to obtain a sample with a small thickness unevenness compared to the case where the protruding direction of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view. Can do.

(14) A sample processing method according to the present invention includes:
A sample fixing portion to which the sample is fixed, and the sample fixing portion has a rolling structure composed of crystal grains having a longitudinal direction in a direction intersecting with a direction of a normal to an end surface of the sample fixing portion in plan view Preparing a sample stage made of metal;
Fixing the sample to the sample fixing portion so that the tip side of the sample protrudes from the end surface of the sample fixing portion in plan view;
Processing the sample fixed to the sample stage using an ion beam;
including.

  In such a sample processing method, since the sample fixing part of the sample stage is made of a metal having a rolled structure, it is easy to handle. Further, in such a sample processing method, the sample fixing portion of the sample stage has a rolled structure composed of crystal grains having a longitudinal direction in a direction intersecting with the direction of the normal of the end surface of the sample fixing portion in plan view. Therefore, when processing a sample with an ion beam, the thickness unevenness is small compared to the case where the perpendicular direction of the end surface of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view. A sample can be obtained.

The top view which shows typically the sample stand which concerns on this embodiment. The top view which shows typically the sample fixing | fixed part of the sample stand which concerns on this embodiment. Sectional drawing which shows typically the sample fixing | fixed part of the sample stand which concerns on this embodiment. An optical micrograph of molybdenum foil produced by cold roll rolling. Bright-field scanning electron microscope image of molybdenum foil produced by cold roll rolling. The flowchart which shows an example of the flow of the sample processing method using the sample stand which concerns on this embodiment. The figure which shows typically the process of thinning a sample fixing | fixed part with a broad ion beam. The figure which shows typically the process of thinning a sample fixing | fixed part with a broad ion beam. The figure which shows typically the process of thinning a sample fixing | fixed part with a broad ion beam. The figure which shows typically the process of thinning a sample fixing | fixed part with a broad ion beam. The perspective view which shows typically the sample fixed to the sample fixing | fixed part. The figure which shows typically the process of processing a sample with a broad ion beam. The figure which shows typically the process of processing a sample with a broad ion beam. The figure for demonstrating a sputtering phenomenon. The figure for demonstrating a sputtering phenomenon. The figure for demonstrating a sputtering phenomenon. The perspective view which shows typically the front-end | tip part of the sample fixing | fixed part of the sample stand which concerns on a reference example. The figure for demonstrating the effect of shadowing. The perspective view which shows typically the sample stand concerning a 1st modification. The top view which shows typically the sample stand concerning a 2nd modification. The top view which shows typically the sample fixing | fixed part of the sample stand which concerns on a 2nd modification. The figure which shows typically the process of processing a sample with a broad ion beam.

  DESCRIPTION OF EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings. The embodiments described below do not unduly limit the contents of the present invention described in the claims. In addition, not all of the configurations described below are essential constituent requirements of the present invention.

1. First, a sample table according to this embodiment will be described with reference to the drawings. FIG. 1 is a plan view schematically showing a sample table 100 according to the present embodiment. FIG. 2 is a plan view schematically showing the sample fixing unit 20 of the sample stage 100 according to the present embodiment. FIG. 3 is a cross-sectional view schematically showing the sample fixing portion 20 of the sample stage 100 according to the present embodiment, and is a cross-sectional view taken along the line III-III in FIG. 2 and 3 show a state in which the sample S is fixed to the sample fixing unit 20.

  As shown in FIGS. 1 to 3, the sample stage 100 includes a support unit 10 and a sample fixing unit 20. The sample table 100 is a sample table for ion beam processing that is used to hold the sample S when the sample S is processed by irradiating the sample S with an ion beam. Below, when the sample stage 100 produces the sample for electron microscopes including a transmission electron microscope (TEM) and a scanning transmission electron microscope (STEM), the sample for electron microscope sample preparation used in order to hold | maintain a sample. An example of a table will be described. The sample stage 100 can hold the sample S when observing the sample S with an electron microscope.

The support unit 10 supports the sample fixing unit 20. The support part 10 is a plate-shaped member. As shown in FIG. 1, the planar shape of the support portion 10 is a substantially semicircular shape with a circle cut out. Support part 10
Has a notch surface 11 formed by notching a circle. A part of the outer edge of the support portion 10 has an arc shape in plan view (as viewed from the direction perpendicular to the main surface of the support portion 10). The arc is, for example, a part of a circle having a diameter of 3 mm. The thickness of the support portion 10 is, for example, about 5 μm.

  The support 10 has a protrusion 12 having a shape that matches the sample holding mechanism of the broad ion beam apparatus. Thereby, the sample stage 100 can be easily attached to the broad ion beam apparatus with good position reproducibility.

  The sample fixing unit 20 is supported by the support unit 10. The sample fixing unit 20 protrudes from the support unit 10 in the first direction A as shown in FIGS. 2 and 3. The sample fixing part 20 protrudes in the in-plane direction of the plate-like support part 10. In the illustrated example, the sample fixing portion 20 protrudes from the notch surface 11 of the support portion 10 in the perpendicular direction of the notch surface 11. That is, at this time, the first direction A is a perpendicular direction of the notch surface 11. The sample fixing portion 20 protrudes from the support portion 10 to form a convex portion. In the illustrated example, the sample fixing part 20 is a part protruding from the support part 10.

  The sample fixing part 20 has a root part 22 connected to the support part 10 and a tip part 24 having a smaller width than the root part 22. The root portion 22 is one end portion of the sample fixing portion 20, and the tip portion 24 is the other end portion of the sample fixing portion 20. The first direction A in which the sample fixing part 20 protrudes is a direction from the root part 22 toward the tip part 24.

  The width W24 of the distal end portion 24 is a distal end portion in a direction orthogonal to the first direction A, which is the direction in which the sample fixing portion 20 protrudes, as viewed in plan view shown in FIG. 24 size. The width W22 of the root portion 22 is the size of the root portion 22 in the direction orthogonal to the first direction A, which is the direction in which the sample fixing portion 20 protrudes, in the plan view shown in FIG. The width W24 of the distal end portion 24 is, for example, about 50 μm, and the width W22 of the root portion 22 is, for example, about 100 μm. The length L20 of the sample fixing unit 20 in the first direction A is, for example, about 150 μm.

  As described above, a part of the outer edge of the support portion 10 has an arc shape in plan view, and the distal end portion 24 of the sample fixing portion 20 is located at the center of the arc. In the illustrated example, the end surface 25 of the tip 24 of the sample fixing unit 20 is linear in plan view, and the direction of the perpendicular P of the end surface 25 is the same as the first direction A.

  As shown in FIG. 3, the main surface 21a (upper surface in the illustrated example) and the main surface 21b (lower surface in the illustrated example) of the sample fixing unit 20 are flat surfaces. The main surface 21a of the sample fixing unit 20 is continuous with one main surface (upper surface) of the support unit 10, and the main surface 21b of the sample fixing unit 20 is continuous with the other main surface (lower surface) of the support unit 10. Yes. The thickness of the sample fixing portion 20 (the distance between the main surfaces 21a and 21b) is equal to the thickness of the support portion 10 and is, for example, about 5 μm.

  The sample S is fixed to the distal end portion 24 of the sample fixing portion 20. In the illustrated example, the sample S is fixed to the main surface 21 b of the sample fixing unit 20. The sample S is fixed so that the tip of the sample S protrudes from the tip 24 (end surface 25) of the sample fixing part 20 in plan view. The base side of the sample S is fixed to the sample fixing unit 20, and the tip side of the sample S is an open end. That is, in the sample stage 100, the sample S is supported in a cantilever shape.

As shown in FIG. 3, the sample S includes an observation region S1 on the tip side of the sample S and a buffer unit S2 on the side where the sample S is fixed (the portion of the sample S fixed to the sample fixing unit 20). It is processed as follows. The buffer unit S2 is provided to prevent the observation region S1 from becoming a shadow of the sample fixing unit 20 due to the thickness of the sample fixing unit 20 when the broad ion beam is irradiated at a shallow angle with respect to the observation region S1. .

  The sample fixing unit 20 is made of a metal having a rolled structure. The metal having a rolled structure is a metal processed by rolling, and is a metal in which crystal grains have a longitudinal direction in a specific direction by rolling. The metal which comprises the sample fixing | fixed part 20 is a metal which has the rolling structure | tissue formed by cold rolling, for example.

  A metal having a rolled structure used for the sample fixing unit 20 (hereinafter also referred to as “rolled material”) is processed by repeatedly performing cold rolling with a roll while interposing annealing, for example. By this rolling process, the crystal grains are deformed to form a rolled structure (fiber structure) composed of crystal grains of several tens μm or more in the rolling direction and about several μm in the direction perpendicular to the rolling direction. That is, the crystal grains constituting the rolled structure have a longitudinal direction in the rolling direction.

  FIG. 4 is an optical microscope image of a 5 μm-thick molybdenum foil produced by cold roll rolling. FIG. 5 is a bright-field scanning electron microscope image (BF-STEM image) of a 5 μm-thick molybdenum foil produced by cold roll rolling.

  In the optical microscope image shown in FIG. 4, the rolling structure of the rolled material (molybdenum foil) is observed as rolling streaks. In the BF-STEM image shown in FIG. 5, a rolled structure composed of crystal grains having a longitudinal direction in a specific direction is observed. In the optical microscope image shown in FIG. 4, the direction along the rolling stripe, that is, the second direction B that is the longitudinal direction of the crystal grains constituting the rolled structure is indicated by an arrow. Similarly, in the BF-STEM photograph shown in FIG. 5, the second direction B, which is the longitudinal direction of the crystal grains constituting the rolled structure (the specific direction), is indicated by an arrow. Thus, the longitudinal direction (second direction B) of the crystal grains constituting the rolled structure can be confirmed by an optical microscope image or an electron microscope image.

  As shown in FIG. 2, the longitudinal direction (second direction B) of the crystal grains constituting the rolled structure is a direction intersecting with the projecting direction (first direction A) of the sample fixing portion 20 in plan view. is there. That is, in the plan view, the first direction A and the second direction B are not parallel (not the same direction), and the angle formed by the first direction A and the second direction B is greater than 0 degree and 90 degrees or less. It is. Note that the angle formed by the first direction A and the second direction B in plan view is more preferably 45 degrees or more and 90 degrees or less, and still more preferably 90 degrees. The reason will be described later. When the angle formed by the first direction A and the second direction B is 90 degrees in plan view (in the case shown in FIG. 2), the direction in which the sample fixing unit 20 protrudes and the sample fixing unit 20 in plan view. This is a case where the longitudinal direction of the crystal grains of the rolled material constituting the material is orthogonal.

  The metal constituting the sample fixing unit 20 is, for example, copper, molybdenum, rhodium, ruthenium, rhenium, beryllium, titanium, or an alloy containing at least one of these metals. When the sample fixing unit 20 is made of one kind of metal, for example, compared with a case where the sample fixing unit 20 is made of a plurality of types of metals, electron beam excitation such as energy dispersive X-ray spectroscopy (EDS) is performed. Even when the constituent elements of the sample fixing part 20 are detected during the composition analysis by X-rays, the influence is small. That is, system noise can be reduced during composition analysis. Moreover, when using an alloy as a metal which comprises the sample fixing | fixed part 20, age-hardening type alloys, such as beryllium copper, are preferable. In a normal metal or alloy, when processing such as rolling or annealing is performed, crystal grains may grow greatly, resulting in a decrease in strength or cracking. On the other hand, the age-hardening type alloy can improve the hardness by heat treatment after rolling.

The sample stage 100 is formed by cutting a predetermined shape from a plate-shaped rolled material using a technique such as etching. The support part 10 and the sample fixing part 20 are cut out from one rolled material and formed integrally. That is, in the sample stage 100, the support part 10 is comprised with the metal which has a rolling structure similarly to the sample fixing | fixed part 20. As shown in FIG.

2. Sample Processing Method Next, a sample processing method using the sample stage 100 will be described with reference to the drawings.

  FIG. 6 is a flowchart showing an example of the flow of the sample processing method using the sample stage 100. Here, a sample processing method for producing a transmission electron microscope sample using the sample stage 100 will be described.

  First, the sample stage 100 is prepared (step S10).

  Next, the sample fixing unit 20 of the sample stage 100 is thinned using a broad ion beam (step S12).

  Thinning of the sample fixing unit 20 is performed using a broad ion beam apparatus. The broad ion beam apparatus is an apparatus for processing a sample by irradiating the sample with an ion beam having a diameter of about several millimeters that is not emitted from the ion gun and is not subjected to the focusing action by the lens system.

  7 to 10 are diagrams schematically showing a step (step S12) of thinning the sample fixing unit 20 using a broad ion beam. 10 is a cross-sectional view taken along the line XX of FIG.

  In the broad ion beam apparatus 2, as shown in FIGS. 7 and 8, the ion beam is directed from the ion guns 2 a and 2 b toward the tip 24 while rotating the sample stage 100 around the tip 24 of the sample fixing unit 20. Can be irradiated. The broad ion beam apparatus 2 includes two ion guns 2a and 2b arranged at positions facing each other with the sample stage 100 interposed therebetween.

  The broad ion beam device 2 can irradiate the broad ion beam IB in synchronization with the rotation of the sample stage 100. Therefore, it is possible to irradiate the sample stage 100 (the tip portion 24 of the sample fixing unit 20) with the broad ion beam IB from a desired direction in plan view.

In this step, the broad ion beam IB is irradiated from the root portion 22 side of the sample fixing portion 20 to the tip portion 24 of the sample fixing portion 20. For example, as shown in FIG. 9, when the Z axis passing through the center of the tip 24 of the sample fixing portion 20 and extending in the direction opposite to the first direction A is 0 degree (rotation angle θ _R = 0 degree), the sample The broad ion beam IB is irradiated to the distal end portion 24 of the fixed portion 20 in a range where the rotation angle θ _R is −30 degrees to +30 degrees (−30 ° ≦ θ _R ≦ + 30 °). By synchronizing the irradiation of the broad ion beam IB with the rotation of the sample stage 100, the broad ion beam IB is irradiated to the distal end portion 24 of the sample fixing unit 20 in a range of the rotation angle θ _R of −30 degrees to +30 degrees. can do.

Further, in this step, as shown in FIG. 10, by irradiating a broad ion beam IB plus elevation theta _E from the ion gun 2a, irradiating broad ion beam IB from an ion gun 2b minus elevation theta _E. In this step, the broad ion beam IB is irradiated with an elevation angle θ _E (that is, a shallow angle) smaller than the elevation angle θ _E of the broad ion beam IB in the broad ion beam processing step (step S18) for the sample S described later. For example, the elevation angle θ _E of the broad ion beam IB in this step is about half the elevation angle θ _E in step S18. The elevation angle θ _E of the broad ion beam IB irradiated from the ion gun 2a is, for example, θ _E = + 3 degrees, and the elevation angle θ _E of the broad ion beam IB irradiated from the ion gun 2b is θ _E = −3 degrees. is there.

  In this step, for example, the sample fixing portion 20 having a thickness of about 5 μm is thinned to a thickness of about 1 μm to 3 μm.

  Here, as described above, the sample fixing part 20 of the sample stage 100 protrudes in the first direction A, and is formed of crystal grains having a longitudinal direction in the second direction B intersecting the first direction A in plan view. It consists of a metal with a texture. Therefore, in this process, the broad ion beam IB is irradiated from the base portion 22 side of the sample fixing portion 20 to the tip portion 24 of the sample fixing portion 20, so that the sample fixing portion 20 protrudes in a plan view. Compared with the case where the longitudinal direction of the crystal grains is the same direction, the effect of shadowing can be increased, and the unevenness formed on the sample fixing portion 20 can be reduced. The reason for this will be described later.

  Thus, in this process, since the unevenness formed on the sample fixing part 20 can be reduced, the unevenness of the sample fixing part 20 is processed, for example, in the process of processing the sample S described later with a broad ion beam (step S18). Therefore, the thickness unevenness formed in the sample S can be reduced. Further, since the unevenness formed on the end surface 25 of the sample fixing portion 20 can be reduced, it is difficult to fix the sample S in the step of fixing the sample S to the distal end portion 24 of the sample fixing portion 20 described later (step S14). Can be prevented.

  Next, the sample S is fixed to the sample fixing part 20 of the sample stage 100 (step S14).

  FIG. 11 is a perspective view schematically showing the sample S fixed to the sample fixing portion 20 of the sample stage 100. The sample S is fixed to the sample fixing unit 20 in a state of a sample piece processed to have a thickness of about 1 μm, a width of 10 μm, and a length of about 20 μm with an FIB apparatus, for example. In this step, the sample S is fixed to the tip 24 of the sample fixing part 20 so that the tip (observation region S1) side of the sample S protrudes from the end surface 25 of the sample fixing part 20. The sample S is fixed using a pickup device or the like. The sample S is fixed to the sample fixing unit 20 with an adhesive or the like.

  Next, the sample S fixed to the sample fixing unit 20 is processed into a thickness of about 0.1 μm in the observation region of the sample S using a focused ion beam (FIB) (step S16).

  As shown in FIG. 11, the sample S is processed so as to have an observation region S1 having a thickness of 0.1 μm or less and a buffer portion S2 having a thickness of about 0.3 μm and a length of 10 μm or more. The buffer portion S2 is provided to prevent the observation region S1 from being a shadow of the sample fixing portion 20 due to the thickness of the sample fixing portion 20 in the step of processing the sample S to be described later with a broad ion beam (step S18).

  In this step, an unnecessary portion (at least a portion of the tip portion 24 excluding the portion to which the sample S is bonded) is further removed using the focused ion beam. May be. In the illustrated example, the corner of the tip 24 is removed so that the width of the tip 24 of the sample fixing unit 20 is reduced.

  Next, the sample S fixed to the sample fixing unit 20 is processed using the broad ion beam IB (step S18).

  12 and 13 are diagrams schematically illustrating a process (step S18) of processing the sample S using a broad ion beam. In this step, a broad ion beam apparatus is used to irradiate the sample S with a low-acceleration broad ion beam to perform processing for removing the damaged layer.

Removal of the damaged layer of the sample S is performed using a broad ion beam apparatus as in the step of thinning the sample fixing unit 20 (step S12). In this step, the sample S, irradiating broad ion beam IB the sample fixing portion 20 at a large angle of elevation theta _E to the step of thinning (step S12). Specifically, the elevation angle θ _E of the broad ion beam IB irradiated from the ion gun 2a is, for example, θ _E = + 10 degrees, and the elevation angle θ _E of the broad ion beam IB irradiated from the ion gun 2b is θ _E = −10 degrees.

Further, in this step, the broad ion beam IB is irradiated from the base portion 22 side of the sample fixing portion 20 to the sample S fixed to the tip portion 24 of the sample fixing portion 20 as in step S12 described above. For example, the sample S fixed to the distal end 24 of the sample fixing portion 20, the rotation angle theta _R irradiates the broad ion beam IB in a range of -30 degrees to + 30 degrees.

  In this way, by irradiating the sample S fixed to the tip 24 of the sample fixing unit 20 with the broad ion beam IB from the root 22 side of the sample fixing unit 20, the traveling direction of the broad ion beam IB In the (irradiation direction), the sample stage 100 does not exist ahead of the sample S. Therefore, it is possible to prevent the material sputtered by the broad ion beam IB from adhering to the sample S (observation region S1) (hereinafter also referred to as “reattachment”).

  For example, although not shown, when the sample S is irradiated with a broad ion beam from the direction opposite to the traveling direction of the broad ion beam IB shown in FIG. The sample stage 100 (for example, the end face 25) exists ahead of S. Therefore, the broad ion beam sputters the sample stage 100 (for example, the end face 25), and the sputtered material adheres to the sample S.

  Further, by irradiating the sample S fixed to the tip 24 of the sample fixing unit 20 with the broad ion beam IB from the root 22 side of the sample fixing unit 20, as in the above-described step S12, a plan view is obtained. Thus, the shadowing effect can be increased and the unevenness formed on the sample fixing portion 20 can be reduced as compared with the case where the protruding direction of the sample fixing portion 20 and the longitudinal direction of the crystal grains are the same direction. it can. Therefore, a sample with small thickness unevenness can be obtained.

  Through the above process, a sample for an electron microscope can be produced.

  The sample stage 100 has the following features, for example.

  In the sample stage 100, the sample fixing unit 20 is made of a metal having a rolled structure. Therefore, for example, it is easier to handle than the case where the sample fixing unit 20 is made of a material such as silicon or ceramics. For example, when the sample fixing part is made of a material such as silicon or ceramics, it may be cracked or chipped when fixing the sample to the sample fixing part or carrying the sample table with tweezers. Caution must be taken. On the other hand, when the sample fixing part 20 is made of metal, it is not cracked or chipped when the sample S is fixed to the sample fixing part 20 or when the sample stage 100 is carried with tweezers. Easy to handle. In addition, since the rolled material is inexpensive, the sample stage can be provided at a low cost.

  In the sample stage 100, the sample fixing unit 20 protrudes from the support unit 10 in the first direction A, and has a rolled structure composed of crystal grains having a longitudinal direction in the second direction B that intersects the first direction A in plan view. It is comprised with the metal which has. Therefore, when processing a sample with an ion beam (for example, step S18 described above), compared to a case where the protruding direction of the sample fixing portion and the longitudinal direction of the crystal grains are the same in a plan view while preventing reattachment. A sample with small thickness unevenness can be obtained. The reason will be described below.

  When a sample fixed to the sample stage is processed with an ion beam, irregularities reflecting the crystal grains of the metal constituting the sample stage may be formed on the sample stage (crystal anisotropic sputtering). The reason is as follows.

  The ion beam sputtering phenomenon includes a phenomenon in which ions enter a material, and when ions enter the material, atoms collide with each other continuously in the material (collision cascade), and atoms are desorbed from the surface. It can be divided into phenomena. 14 to 16 are diagrams for explaining the sputtering phenomenon when ions are incident on the same crystal from different directions.

  First, the phenomenon that ions enter a substance will be described. When the surface of the material is irradiated with the ion beam I, some of the ions collide with atoms on the surface of the material, but many ions pass through the surface and enter the material, so-called channeling phenomenon occurs. Collisions with constituent atoms. The ions have a smaller scattering cross section, and the deeper the interatomic distance of the substance viewed from the ion beam I, the deeper the ions enter. The scattering cross section of ions depends on the ion species and acceleration, and the interatomic distance of the material viewed from the ions depends on the interplanar spacing and direction of the crystal. For this reason, the depth at which the ions and the atoms constituting the substance collide changes depending on the orientation of the crystal (see FIGS. 14 and 15).

  Next, collision cascade and desorption from the surface will be described. When an ion with momentum collides with an atom that constitutes a substance, part of the momentum that the ion has is transmitted to the atom, and the ion loses part of the momentum and changes its direction. The ion whose direction has been changed repeatedly collides until its momentum disappears, and continues to give momentum in various directions to the atoms constituting the material. Atoms that have received momentum more than the energy that keeps the atoms at the lattice points are separated from the lattice points, are blown off in the direction of the received momentum, collide with other atoms, and repeat collisions in the same way as ions. When ions with momentum enter the material, an avalanche-type atomic collision phenomenon is caused (collision cascade). When a momentum greater than the desorption energy is given to an atom near the surface in the direction of desorption from the surface, the atom desorbs from the substance. This is a sputtering phenomenon. The probability that the atoms collide with each other is related to the lattice plane density seen from the ejected atoms, and the probability that the momentum is converted in the desorption direction is related to the atomic position of the crystal (see FIGS. 15 and 16). That is, the crystal plane and the incident direction of ions, and the orientation of the crystal plane and surface correlate with the desorption yield.

  As described above, the ion penetration depth varies depending on the orientation of the crystal. And, ions that have entered deeper require more collisions for sputtering than ions that have entered shallower. Therefore, when compared with ions having the same momentum, the sputtering yield (the number of atoms desorbed per incident ion) is smaller for ions that have entered deeper than ions that have entered shallower. That is, the sputtering yield depends on the crystal orientation. Further, as described above, the crystal plane and the incident direction of ions, and the orientation of the crystal plane and surface correlate with the yield of desorption.

  Therefore, when a polycrystalline material is thinly sputtered to a crystal grain size with a uniform ion beam I, irregularities corresponding to the crystal grains are formed.

  FIG. 17 is a perspective view schematically showing the distal end portion 24A of the sample fixing portion 20A of the sample stage 100A according to the reference example. In the sample stage 100A, the direction in which the sample fixing portion 20A protrudes is the same direction as the longitudinal direction of the crystal grains.

As shown in FIG. 17, when the sample stage 100A is thinly sputtered to a crystal grain size with a uniform ion beam, unevenness in the thickness direction is formed at the tip portion 24A of the sample fixing portion 20A, and further, the end face 25A. Irregularities are also formed. When unevenness in the thickness direction is formed on the sample fixing portion 20A, the ion beam I is not uniformly irradiated on the sample S due to the unevenness, and streaky thickness unevenness is formed on the sample S. In addition, when unevenness is formed on the end surface 25A of the sample stage 100A, it becomes difficult to fix the sample S to the sample fixing portion 20A.

  Here, by irradiating the ion beam I with a small elevation angle (shallow angle) to a sample stage made of a polycrystalline material, the unevenness can be reduced by the effect of shadowing.

  FIG. 18 is a diagram for explaining the effect of shadowing. As shown in FIG. 18, by irradiating the ion beam I at a small elevation angle, the crystal grains 3 having a small height are shaded by the adjacent crystal grains 3 having a large height and are not processed until the heights are approximately the same. . Thereby, a processed surface with small unevenness can be obtained. Since the ion beam I has a feature of diverging, the effect of shadowing is reduced when the length L3 of the concave portion is large. For this reason, the shadowing effect is sufficiently exhibited when the length L3 of the concave portion is several μm or less.

  Therefore, when processing the rolled material with the ion beam I, the ion beam I is irradiated from a direction intersecting the second direction B which is the longitudinal direction of the crystal grains constituting the rolled structure in a plan view. As a result, the unevenness formed on the rolled material due to the effect of shadowing can be reduced compared to the case of irradiating the ion beam I from the same direction as the second direction B, which is the longitudinal direction of the crystal grains constituting the rolled structure. can do. In particular, when the ion beam I is irradiated from a direction orthogonal to the second direction B, which is the longitudinal direction of the crystal grains constituting the rolled structure, the effect of shadowing is maximized and formed on the rolled material. The unevenness to be made can be made smaller.

  Therefore, as described above, in the sample stage 100, the sample fixing portion 20 is a crystal grain that protrudes from the support portion 10 in the first direction A and has a longitudinal direction in the second direction B that intersects the first direction A in plan view. Since it is composed of a metal having a structured rolled structure, when the sample is processed with an ion beam (for example, step S18 described above), the sample is fixed to the sample S fixed to the tip portion 24 of the sample fixing unit 20. By irradiating the ion beam from the root portion 22 side of the fixing portion 20, it is possible to prevent reattachment, and in comparison with the case where the protruding direction of the sample fixing portion and the longitudinal direction of the crystal grains are the same direction in plan view. A sample with small unevenness can be obtained.

  In the sample stage 100, the angle formed by the first direction A and the second direction B in plan view is more preferably 45 degrees or more and 90 degrees or less, and further preferably 90 degrees. When the angle formed by the first direction A and the second direction B in the plan view is in the above range, as described above, the effect of shadowing can be increased, so that the thickness unevenness is prevented while preventing reattachment. A small sample can be obtained.

  In the sample stage 100, since the sample fixing part 20 protrudes from the support part 10 in the first direction A, even when a twist is applied to the support part 10 when the support part 10 is sandwiched between tweezers, the stress is It concentrates on the root portion 22 of the sample fixing portion 20 and hardly transmits to the tip portion 24. Therefore, in the sample stage 100, by fixing the sample S to the distal end portion 24 of the sample fixing part 20, it is possible to make the sample S less likely to be detached or broken when the sample stage 100 is sandwiched with tweezers. The sample stage 100 can be easily handled.

  In the sample stage 100, the sample fixing part 20 has a root part 22 connected to the support part 10 and a tip part 24 having a smaller width than the root part 22. Therefore, it is possible to prevent the sample fixing part 20 from being bent or rounded and deforming its shape, and for example, subjecting the tip 24 of the sample fixing part 20 to FIB processing in the focused ion beam processing step (step S16). In this case, the processing amount can be reduced.

  The sample processing method according to the present embodiment includes a step of preparing the sample stage 100 (step S10), a step of fixing the sample S to the sample fixing unit 20 (step S14), and a sample S fixed to the sample stage 100. And processing using an ion beam (step S18). Thus, in this embodiment, since the sample fixing | fixed part 20 of the sample stand 100 is comprised with the metal which has a rolling structure | tissue, it is easy to handle. Further, in the present embodiment, in the step of processing the sample with an ion beam, while preventing re-adhesion, compared to the case where the direction in which the sample fixing portion protrudes and the longitudinal direction of the crystal grains are the same direction in plan view, A sample with small unevenness can be obtained.

  In addition, the sample processing method according to the present embodiment includes a step of thinning the sample fixing unit 20 using an ion beam before the step of fixing the sample S to the sample fixing unit 20. Therefore, reattachment to the sample S can be prevented in the step of processing the sample S with a broad ion beam (step S18). Further, since the thickness of the sample fixing unit 20 can be reduced, system noise can be reduced when the sample S fixed to the sample stage 100 is introduced into an electron microscope or the like for analysis. When composition analysis such as EDS analysis is performed with an electron microscope or the like, a part of the electron beam is irradiated to the sample fixing unit 20 by scattering or the like, and characteristic X-rays are generated from the sample fixing unit 20 and detected as system noise. There is a case. In particular, when the thickness of the sample fixing unit 20 is large, the system noise increases. In this embodiment, since the thickness of the sample fixing unit 20 can be reduced, system noise can be reduced.

3. Experimental Examples Hereinafter, the present invention will be specifically described with reference to experimental examples, but the present invention is not limited to the following experimental examples.

  In this experimental example, a transmission electron microscope sample was produced according to the flowchart shown in FIG.

  A sample stage having the same shape as the sample stage 100 shown in FIGS. 1 to 3 was produced using a 5 μm-thick molybdenum foil produced by cold roll rolling. Specifically, the first direction A that is the extending direction of the sample fixing portion and the second direction B that is the longitudinal direction of the crystal grains of the rolled material constituting the sample fixing portion are orthogonal to each other in plan view. Formed as follows. Further, a part of the outer edge of the support portion has an arc shape in plan view, and the tip end portion of the sample fixing portion is formed so as to be located at the center of the arc. The length of the sample fixing part was 150 μm, and the width of the tip part of the sample fixing part was 50 μm. The protrusion of the support portion was shaped according to the shape of the sample holding mechanism of the broad ion beam device (PIPSII MODEL 695 manufactured by Gatan).

  Next, the prepared sample stage was processed with an ion beam using a broad ion beam apparatus (PIPSII MODEL695 manufactured by Gatan). Specifically, an Ar ion beam having an ion energy of 8 kV and an ion current of 140 μA is applied to a sample stage rotating at 0.5 rpm, with an elevation angle of +3 degrees and −3 degrees, and a rotation angle of −30 degrees to +30 degrees. Irradiated in the range of.

  When the ion beam was irradiated for 18 minutes, the tip of the sample fixing part had a thickness of 1 μm and was processed into a flat surface with small irregularities.

  Next, a sample processed to a width of 10 μm, a height of 22 μm, and a thickness of 1 μm with an FIB apparatus was fixed to the sliced sample fixing portion with an adhesive using a pickup apparatus.

  Next, using the FIB apparatus, the sample fixed to the sample fixing unit is 10 μm in length, the buffer is 0.3 μm in thickness, and the observation region is 0.1 μm in thickness. Was processed as follows.

  When TEM observation was performed in this state, detailed observation could not be performed because the damaged layer formed on the sample was thick.

  Next, the sample held on the sample stage was processed using a broad ion beam apparatus (PIPSII MODEL695 manufactured by Gatan). Specifically, an Ar ion beam having an ion energy of 0.3 kV is applied to a sample fixed on a sample stage rotating at 0.5 rpm, with an elevation angle of +10 degrees and −10 degrees, and a rotation angle of −30 degrees. Irradiation was in the range of ˜ + 30 degrees.

  When the ion beam was irradiated for 15 minutes and TEM observation was performed, detailed observation was able to be performed compared with before performing this process. In addition, no reattachment to the sample was observed.

  In addition, when the sample stage was twisted, the root part of the sample fixing part was deformed, but the tip part of the sample fixing part was hardly deformed, and the sample fixed to the tip part was not detached or broken. There wasn't.

4). Modified example 4.1. First Modification Next, a first modification of the sample stage according to the present embodiment will be described with reference to the drawings. FIG. 19 is a perspective view schematically showing a sample stage 200 according to the first modification. Hereinafter, in the sample stage 200 according to the first modification of the present embodiment, members having the same functions as those of the constituent members of the sample stage 100 described above are denoted by the same reference numerals, and detailed description thereof is omitted.

  In the sample stage 100 described above, as shown in FIGS. 1 to 3, the support portion 10 has a uniform thickness.

  On the other hand, in the sample stage 200, as shown in FIG. 18, the support portion 10 is provided along the thin plate portion 13 connected to the sample fixing portion 20 and the outer edge having the arc shape of the support portion 10. A thick plate portion 14. The thickness of the thin plate portion 13 is, for example, 5 μm, and the thickness of the thick plate portion 14 is, for example, 30 μm.

  The sample stage 200 can be formed, for example, by etching a rolled material in two stages.

  The sample processing method using the sample table 200 is the same as the sample processing method using the sample table 100 described above, and the description thereof is omitted.

  The sample stage 200 can achieve the same effects as the sample stage 100 described above. Furthermore, in the sample stage 200, since the support unit 10 includes the thin plate unit 13 and the thick plate unit 14, the sample unit 200 is sandwiched with tweezers while preventing the support unit 10 from blocking the ion beam. Desorption and destruction of the sample S can be made difficult, and the sample stage 200 can be made easier to handle.

  Hereinafter, the present invention will be specifically described with reference to experimental examples, but the present invention is not limited to the following experimental examples.

  In this experimental example, a transmission electron microscope sample was produced according to the flowchart shown in FIG.

A beryllium copper foil with a thickness of 30 μm produced by cold roll rolling was etched in two stages to produce a sample stage having the same shape as the sample stage 200 shown in FIG. Specifically, the first direction A that is the extending direction of the sample fixing portion and the second direction B that is the longitudinal direction of the crystal grains of the rolled material constituting the sample fixing portion are orthogonal to each other in plan view. Formed as follows. Further, a part of the outer edge of the support portion has an arc shape in plan view, and the tip end portion of the sample fixing portion is formed so as to be located at the center of the arc. The length of the sample fixing part was 150 μm, and the width of the tip part of the sample fixing part was 50 μm. Further, the thickness of the thin plate portion was 5 μm, and the thickness of the thick plate portion was 30 μm. The protrusion of the support portion was shaped according to the shape of the sample holding mechanism of the broad ion beam device (PIPSII MODEL 695 manufactured by Gatan).

  Next, the prepared sample stage was processed with an ion beam using a broad ion beam apparatus (PIPSII MODEL695 manufactured by Gatan). Specifically, an Ar ion beam having an ion energy of 8 kV and an ion current of 140 μA is applied to a sample stage rotating at 0.5 rpm, with an elevation angle of +3 degrees and −3 degrees, and a rotation angle of −30 degrees to +30 degrees. Irradiated in the range of.

  When the ion beam was irradiated for 22 minutes, the tip portion of the sample fixing portion had a thickness of 1 μm and was processed into a flat surface with small unevenness.

  Next, a sample processed to a width of 10 μm, a height of 22 μm, and a thickness of 1 μm with an FIB apparatus was fixed to the sliced sample fixing portion with an adhesive using a pickup apparatus.

  Next, using the FIB apparatus, the sample fixed to the sample fixing part is adjusted so that the buffer part has a length of 10 μm, the buffer part has a thickness of 0.3 μm, and the observation region has a thickness of 0.1 μm. processed.

  When TEM observation was performed in this state, detailed observation could not be performed because the damaged layer formed on the sample was thick.

  Next, the sample fixed to the sample fixing portion was processed using a broad ion beam apparatus (PIPSII MODEL 695 manufactured by Gatan). Specifically, an Ar ion beam having an ion energy of 0.3 kV is applied to a sample fixed on a sample stage rotating at 0.5 rpm, with an elevation angle of +10 degrees and −10 degrees, and a rotation angle of −30 degrees. Irradiation was in the range of ˜ + 30 degrees.

  When the ion beam was irradiated for 15 minutes and TEM observation was performed, detailed observation was able to be performed compared with before performing this process. In addition, no reattachment to the sample was observed.

  In addition, when this sample stage was twisted, the deformation was small due to the thick plate part, and a slight deformation occurred at the base of the sample fixing part for fixing the sample. Was hardly deformed, and the sample fixed to the tip part was not detached or broken.

4.2. Second Modified Example Next, a second modified example of the sample stage according to the present embodiment will be described with reference to the drawings. FIG. 20 is a plan view schematically showing a sample stage 300 according to the second modification. FIG. 21 is a plan view schematically showing the sample fixing portion 20 of the sample stage 300 according to the second modification. Hereinafter, in the sample stage 300 according to the second modification of the present embodiment, members having the same functions as those of the constituent members of the sample stage 100 described above are denoted by the same reference numerals, and detailed description thereof is omitted.

  In the sample table 100 described above, as shown in FIGS. 1 to 3, the sample fixing unit 20 protrudes from the support unit 10.

  On the other hand, in the sample stage 300, the sample fixing unit 20 does not protrude from the support unit 10 as shown in FIGS. 20 and 21. In the illustrated example, a part of the outer edge of the support portion 10 has an arc shape in plan view, and the sample fixing portion 20 is located at the center of the arc.

  As shown in FIG. 21, the sample S is fixed so that the tip of the sample S protrudes from the end surface 25 of the sample fixing unit 20 in plan view. The base side of the sample S is fixed to the sample fixing unit 20, and the tip side of the sample S is an open end. That is, in the sample stage 300, the sample S is supported in a cantilever shape.

  The sample fixing part 20 is made of a metal having a rolling structure made up of crystal grains having a longitudinal direction in a direction intersecting the direction of the perpendicular P of the end face 25 of the sample fixing part 20 in plan view. That is, in a plan view, the second direction B, which is the longitudinal direction of the crystal grains constituting the rolled structure, is a direction that intersects the perpendicular P of the end face 25. In the illustrated example, the end surface 25 of the sample fixing unit 20 is a surface (surface flush) that is continuous with the cutout surface 11 of the support unit 10.

  Note that the sample processing method using the sample stage 300 includes the sample processing method using the sample stage 100 shown in FIG. 6, the step of preparing the sample stage 300 in the step of preparing the sample stage (Step S <b> 10), and the sample In the step of processing S using a broad ion beam (step S18), the sample S is different in that the ion beam is irradiated from the sample fixing unit 20 side. Other steps are the same as those of the sample processing method using the sample table 100 described above.

  Hereinafter, the sample processing method using the sample table 300 will be described with respect to differences from the sample processing method using the sample table 100 described above, and description of similar points will be omitted.

  FIG. 22 is a diagram schematically showing a process (step S18) of processing the sample S using the broad ion beam IB.

In this step, as shown in FIG. 22, with respect to the sample S fixed to the sample fixing unit 20 of the sample stage 300 so that the front end side of the sample S protrudes from the end surface 25 of the sample fixing unit 20 in plan view. A broad ion beam IB is irradiated from the sample fixing unit 20 side. For example, for a fixed sample S on the sample fixing part 20, the rotation angle theta _R irradiates the broad ion beam IB in a range of -30 degrees to + 30 degrees. Thereby, in this process, as in the example of the sample stage 100 described above, while preventing reattachment, compared to the case where the direction of the perpendicular to the end surface of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view Thus, a sample with small thickness unevenness can be obtained.

  In the sample processing method using the sample table 300, the first direction A in the sample processing method using the sample table 100 described above corresponds to, for example, the direction of the perpendicular P of the end surface 25.

  The sample stage 300 is made of a metal having a rolling structure composed of crystal grains having a longitudinal direction in a direction intersecting with the direction of the perpendicular P of the end surface 25 of the sample fixing portion 20 in plan view. Therefore, as in the sample table 100 described above, when processing a sample with an ion beam, the perpendicular direction of the end surface of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view while preventing reattachment. Compared with the case where it is, a sample with small thickness nonuniformity can be obtained.

  In addition, embodiment mentioned above and a modification are examples, Comprising: It is not necessarily limited to these. For example, each embodiment and each modification can be combined as appropriate.

For example, in the example of the sample stage 100 according to the first embodiment described above, the example in which the sample fixing unit 20 is configured by a rolled material has been described. However, in the sample stage according to the present invention, the sample fixing unit 20 is configured. The material is not limited to rolled material. In the sample stage according to the present invention, the sample fixing part 20 is a material composed of crystal grains having a longitudinal direction in the second direction B intersecting the first direction A which is the direction in which the sample fixing part 20 protrudes. Also good. Even in such a case, as in the case of the sample stage 100, while preventing re-adhesion, the thickness is larger than the case where the direction in which the sample fixing portion 20 protrudes and the longitudinal direction of the crystal grains are the same in plan view. A sample with small unevenness can be obtained.

  Further, for example, the same applies to the example of the sample stage 300 according to the second modified example described above, and in the sample stage according to the present invention, the sample fixing unit 20 has the direction of the perpendicular P of the end surface 25 of the sample fixing unit 20. You may be comprised with the material comprised by the crystal grain which has a longitudinal direction in the direction which cross | intersects. Even in such a case, as in the sample table 300, while preventing reattachment, compared to the case where the direction of the perpendicular to the end surface of the sample fixing portion and the longitudinal direction of the crystal grains are the same in plan view, A sample with small thickness unevenness can be obtained.

  The present invention includes configurations that are substantially the same as the configurations described in the embodiments (for example, configurations that have the same functions, methods, and results, or configurations that have the same objects and effects). In addition, the invention includes a configuration in which a non-essential part of the configuration described in the embodiment is replaced. In addition, the present invention includes a configuration that exhibits the same operational effects as the configuration described in the embodiment or a configuration that can achieve the same object. Further, the invention includes a configuration in which a known technique is added to the configuration described in the embodiment.

DESCRIPTION OF SYMBOLS 2 ... Broad ion beam apparatus, 2a ... Ion gun, 2b ... Ion gun, 3 ... Crystal grain, 10 ... Support part, 11 ... Notch surface, 12 ... Projection part, 13 ... Thin plate part, 14 ... Thick plate part, 20 Sample fixing portion, 21a ... main surface, 21b ... main surface, 22 ... root portion, 24 ... tip portion, 25 ... end surface, 100 ... sample stand, 200 ... sample stand, 300 ... sample stand

Claims (14)

A sample stage for processing an ion beam used for holding the sample when processing the sample by irradiating the sample with an ion beam,
A sample fixing part to which the sample is fixed;
A support part supporting the sample fixing part;
Including
The sample fixing portion is made of a metal having a rolling structure that is protruded from the support portion in a first direction and that is composed of crystal grains having a longitudinal direction in a second direction that intersects the first direction in a plan view. , Sample stage. In claim 1,
The sample fixing part has a base part connected to the support part and a tip part having a width smaller than the base part. In claim 1 or 2,
At least a part of the outer edge of the support portion has an arc shape in plan view,
The tip of the sample fixing portion is a sample stage located in the center of the arc in plan view. In any one of Claims 1 thru | or 3,
The angle between the first direction and the second direction in a plan view is a sample stage that is not less than 45 degrees and not more than 90 degrees. In any one of Claims 1 thru | or 4,
The sample stage, wherein an angle formed by the first direction and the second direction in a plan view is 90 degrees. In any one of Claims 1 thru | or 5,
A sample stage, wherein the metal constituting the sample fixing part is copper, molybdenum, rhodium, ruthenium, rhenium, beryllium, titanium, or an alloy containing at least one of these metals. A sample stage for processing an ion beam used for holding the sample when processing the sample by irradiating the sample with an ion beam,
A sample fixing part to which the sample is fixed;
A support part supporting the sample fixing part;
Including
The sample holder is made of a material made of crystal grains that protrude from the support portion in a first direction and have a longitudinal direction in a second direction that intersects the first direction. A sample stage for ion beam processing, having a sample fixing part to which a sample is fixed, and fixed in a plan view so that the tip side of the sample protrudes from the end surface of the sample fixing part,
The sample fixing part is made of a metal having a rolling structure composed of crystal grains having a longitudinal direction in a direction intersecting with a direction of a normal to an end surface of the sample fixing part in a plan view. A sample fixing part to which the sample is fixed, and a support part supporting the sample fixing part, wherein the sample fixing part protrudes from the support part in a first direction and intersects the first direction. Preparing a sample stage composed of a metal having a rolled structure composed of crystal grains having a longitudinal direction in two directions;
Fixing the sample to the sample fixing part;
Processing the sample fixed to the sample stage using an ion beam;
A sample processing method. In claim 9,
In the step of fixing the sample to the sample fixing portion, the sample is fixed to the tip portion of the sample fixing portion so that the tip side of the sample protrudes from the sample fixing portion. In claim 9 or 10,
In the step of processing the sample fixed to the sample stage using an ion beam, the ion beam is applied to the sample fixed to the tip of the sample fixing unit from the base side of the sample fixing unit. Irradiation, sample processing method. In any one of claims 9 to 11,
A sample processing method comprising a step of thinning the sample fixing part using an ion beam before the step of fixing the sample to the sample fixing part. A sample fixing part to which the sample is fixed, and a support part supporting the sample fixing part, wherein the sample fixing part protrudes from the support part in a first direction and intersects the first direction. Preparing a sample stage composed of a material composed of crystal grains having a longitudinal direction in two directions;
Fixing the sample to the sample fixing part;
Processing the sample fixed to the sample stage using an ion beam;
A sample processing method. A sample fixing portion to which the sample is fixed; Preparing a sample stage made of metal;
Fixing the sample to the sample fixing portion so that the tip side of the sample protrudes from the end surface of the sample fixing portion in plan view;
Processing the sample fixed to the sample stage using an ion beam;
A sample processing method.