JP5674126B2 - Sample for transmission electron microscope and method for producing the same - Google Patents

Description

  The present invention relates to a sample for a transmission electron microscope and a manufacturing method thereof.

  In observation of a transmission electron microscope (TEM), it is known that a sample for a TEM is prepared by thinning using a focused ion beam (FIB). For example, FIGS. 1A to 1C, FIGS. 2A to 2B, and FIGS. 3A to 3B are schematic diagrams illustrating a method for preparing a TEM sample by a general FIB.

  As shown in FIG. 1A, first, FIB_B0 is irradiated from above the sample 101 to scrape the sample 101. Thereby, as shown to FIG. 1B, the 1st main-body part 102 and the thin-body part 103 are formed. The thin body portion 103 extends laterally from the first main body portion 102 and has a shape thinner than that of the first main body portion 102. The first main body portion 102 is a remaining portion of the sample 101 when the thin body portion 103 is cut out. The thin body portion 103 is coupled to the thin body portion 103 on the lateral side and the lower side thereof.

  Subsequently, as shown in FIG. 1C, FIB_C0 is irradiated from the upper side of the sample 101 to scrape the thin body portion 103, thereby forming the second main body portion 103a and the thin piece portion 104. The thin piece portion 104 extends laterally from the second main body portion 103a and has a shape thinner than that of the second main body portion 103a. The second main body portion 103a is a remaining portion of the thin body portion 103 when the thin piece portion 104 is cut out. The thin piece portion 104 is coupled to the thin piece portion 104 on the lateral side and the lower side thereof. FIG. 2A to FIG. 2B show the enlarged process of FIG. 1C.

  Here, as shown in FIG. 3A (enlargement of the P0 portion in FIG. 2B), the thin piece portion 104 is further shaved by FIB_C0. Thereby, as shown in FIG. 3B, the third main body portion 104a and the thin film portion 111 are formed. The thin film portion 111 extends laterally from the third main body portion 104a and has a shape thinner than that of the third main body portion 104a. The third main body portion 104a is a remaining portion of the thin piece portion 104 when the thin film portion 111 is cut out. The thin film part 111 is coupled to the thin film part 111 on the lateral side and the lower side. An analysis object 113 by TEM is present at a predetermined location of the thin film portion 111.

  In the thinning of the sample by FIB, when the beam is incident from the upper side of the sample, the polishing rate varies depending on the material depending on the configuration in the sample. Therefore, there may be a variation in film thickness within the sample. In such a case, when the elemental analysis is quantified, the accuracy of the analysis is greatly lowered due to the variation in the film thickness. This phenomenon is called cartaining. It is desirable to prevent curtaining.

  As a related technique, Japanese Patent Laid-Open No. 9-145567 (Patent Document 1) discloses a method for preparing a sample for observation with a transmission electron microscope. The method for preparing a sample for observation with a transmission electron microscope is that a carbon film is formed by irradiating an electron beam on the surface of a sample in a vacuum chamber in which an organic molecular gas mainly composed of hydrocarbons is present. By irradiating with an Ar ion beam, the sample surface other than the carbon film covering portion is etched away, and a columnar observation portion perpendicular to the sample surface is formed in the carbon film covering portion.

  Japanese Patent Laid-Open No. 2007-292507 (Patent Document 2) discloses a transmission electron microscope sample preparation method and a focused ion beam apparatus. In this transmission electron microscope sample preparation method, after processing a sample, a thin piece portion including a desired observation position by the transmission electron microscope is formed, and a thin film is formed on the sample surface including the thin piece portion. Then, the thin piece portion is processed with a focused ion beam to remove a part of the thin film of the thin piece portion, and to be an observation sample of the transmission electron microscope.

  In addition, “Recent damage reduction technique at the time of FIB sample preparation” in the proceedings of the 26th Analytical Electron Microscope Symposium discloses that the cutting is suppressed by irradiating the FIB from the back side of the sample.

JP-A-9-145567 JP 2007-292507 A

Masabayashi Masahiro, “Recent Damage Reduction Techniques in FIB Sample Preparation”, Proceedings of the 26th Analytical Electron Microscope Discussion Meeting (2010)

  It has been clarified for the first time by the inventor's research that the above-described general method for preparing a TEM sample by FIB has the following problems. 4A and 4B are schematic diagrams showing problems in thinning. When the thin film portion 111 is formed, if a beam is incident from above the sample 1, the thinned portion may collapse from two directions. For example, as shown in FIG. 4A, when the thin film portion 111 is thinned to have a desired thickness, the thinned portion collapses from above (indicated by K1 in the figure), It begins to collapse from the side (indicated by K2 in the figure). In this case, since the thin film portion 111 collapses from two directions, the area of the thin film portion 111a becomes small as shown in FIG. 4B. That is, thinning over a wide range is difficult, and in the worst case, a certain part of the analysis object 113 may be broken. Therefore, control of collapse is extremely important when making the thinnest (example: film thickness 30 nm-100 nm).

  Hereinafter, means for solving the problem will be described using the numbers and symbols used in the embodiments for carrying out the invention. These numbers and symbols are added with parentheses in order to clarify the correspondence between the description of the claims and the mode for carrying out the invention. However, these numbers and symbols should not be used for interpreting the technical scope of the invention described in the claims.

  The sample for a transmission electron microscope of the present invention includes a sample body (4a), a thin film portion (11), and a protective film (8). The thin film portion (11) extends from the sample body (4a) in the first direction (-Y) and is thinner than the sample body (4a). The protective film (8) is continuously provided on the upper surface of the sample body (4a) and the thin film portion (11), and is harder than the main material of the thin film portion (11). The thin film part (11) includes an ultrathin film part (12) in contact with the lower side of the protective film (8) and a remaining part (11a) in contact with the lower side of the ultrathin film part (12). The ultrathin film portion (12) is thinner than the remaining portion (11a). The ultrathin film portion (12) has a triangular or quadrangular flake shape with the first side being the portion in contact with the protective film (8). The ultrathin film portion (12) has an angle (α) formed by a second side that intersects the first side and is exposed to the outside and a third side that intersects the second side and is coupled to the remaining portion (11a). , Greater than 0 ° and less than 180 °.

  In the transmission electron microscope sample of the present invention, the protective film (8) harder than the main material of the thin film part (11) is provided on the ultrathin film part (12). Therefore, when the ultrathin film portion (12) having a predetermined shape is formed by processing with a beam from the side, that is, the angle (α) formed by the second side and the third side is greater than 0 ° and greater than 180 °. Even in the case of having an extremely thin film portion (12) having a small predetermined shape, the collapse of the ultrathin film portion (12) can be suppressed and the shape can be maintained while curving is suppressed. Thereby, thin film sampling in a large area becomes possible.

  The method for producing a sample for a transmission electron microscope of the present invention comprises: a step of forming a protective film (8); a step of forming a sample body (4a) and a thin film portion (11); and an ultra thin film portion (12). Forming the process. The step of forming the protective film (8) forms a protective film (8) harder than the main material of the sample (1) on the upper surface of the sample (1). The step of forming the sample body (4a) and the thin film portion (11) includes irradiating an ion beam to scrape the sample (1), and a sample body (4a) provided with a protective film (8) on the upper surface. A film (8) is provided on the upper surface, extends from the sample body (4a) in the first direction (-Y), and forms a thin film portion (11) thinner than the sample body (4a). The step of forming the ultrathin film portion (12) is performed by irradiating an ion beam from the side of the thin film portion (11) opposite to the sample main body (4a) and shaving the thin film portion (11) so as to be thin. An ultrathin film part (12) in contact with the lower side of the film (8) is formed.

  In the method for preparing a sample for a transmission electron microscope of the present invention, in the step of forming the ultrathin film portion (12), protection on the ultrathin film portion (12) is harder than the main material of the thin film portion (11) in advance. A membrane (8) is provided. Therefore, even when the ultra-thin film portion (12) having a predetermined shape is formed by processing with a beam from the side, the collapse of the ultra-thin film portion (12) can be suppressed and the shape can be maintained while curving is suppressed. . Thereby, thin film sampling in a large area becomes possible.

  According to the present invention, in a sample for an over-type electron microscope and a manufacturing method thereof, collapse of a thin film portion in the vicinity of an analysis object can be suppressed while curving is suppressed.

FIG. 1A is a schematic diagram showing a method for producing a TEM sample by a general FIB. FIG. 1B is a schematic view showing a method for producing a TEM sample by a general FIB. FIG. 1C is a schematic diagram showing a method for producing a TEM sample by a general FIB. FIG. 2A is a schematic view showing a method for producing a TEM sample by a general FIB. FIG. 2B is a schematic diagram showing a method for producing a TEM sample by a general FIB. FIG. 3A is a schematic diagram showing a method for preparing a TEM sample by a general FIB. FIG. 3B is a schematic view showing a method for producing a TEM sample by a general FIB. FIG. 4A is a schematic diagram showing problems in thinning. FIG. 4B is a schematic diagram showing problems in thinning. FIG. 5A is a perspective view showing a configuration of a transmission electron microscope sample according to the embodiment of the present invention. FIG. 5B is a side view showing the configuration of the transmission electron microscope sample according to the embodiment of the present invention. FIG. 6A is a schematic view showing a method for producing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 6B is a schematic view showing a method for manufacturing a transmission electron microscope sample according to the embodiment of the present invention. FIG. 6C is a schematic diagram showing a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 6D is a schematic diagram illustrating a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 7A is a schematic view showing a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 7B is a schematic diagram showing a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 8A is a schematic view showing a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention. FIG. 8B is a schematic view showing a method for manufacturing a transmission electron microscope sample according to the embodiment of the present invention. FIG. 9 is a schematic diagram showing a method for producing a transmission electron microscope sample according to an embodiment of the present invention.

  Embodiments of a transmission electron microscope sample of the present invention and a method for manufacturing the same will be described below with reference to the accompanying drawings.

  The configuration of the transmission electron microscope sample according to the embodiment of the present invention will be described. 5A and 5B are a perspective view and a side view showing a configuration of a transmission electron microscope sample according to the embodiment of the present invention. A sample 1 for a transmission electron microscope has a shape in which, for example, a part of a substantially rectangular parallelepiped sample is cut out thinly enough to allow TEM observation using a focused ion beam (FIB) or the like. The sample 1 includes a third main body portion 4a, a thin film portion 11, an ultrathin film portion 12, and a protective film 8. Furthermore, you may comprise the 1st main-body part 2 and the 2nd main-body part 3a.

  The first main body 2 has a step structure (step up) in the + Y direction. The step structure is provided with a second main body 3a. The second main body 3 a extends in the lateral direction (−Y direction) from the top of the first main body 2 and has a plate-like shape that is thinner than the first main body 2. The first main body 2 is coupled to the second main body 3a on the lateral side (+ Y side) and the lower side (−Z side) of the second main body 3a.

  The second main body 3a has a step structure (ascending step) in the + Y direction. In the step structure, a third main body portion 4a is provided. The third main body 4a extends in the horizontal direction (−Y direction) from the top of the second main body 3a, and has a plate-like shape that is thinner than the second main body 3a. The second main body portion 3a is coupled to the third main body portion 4a on the lateral side (+ Y side) and the lower side (−Z side) of the third main body portion 4a.

  The third main body 4a has a step structure (ascending step) in the + Y direction. The thin film portion 11 is provided in the step structure. The thin film portion 11 extends in the lateral direction (−Y direction) from the upper portion of the third main body portion 4a, and has a plate shape thinner than the third main body portion 4a. The third main body portion 4 a is coupled to the thin film portion 11 on the lateral side (+ Y side) and the lower side (−Z side) of the thin film portion 11.

  The protective film 8 is provided so as to continuously cover at least the upper surface (+ Z side) of the thin film portion 11 and the third main body portion 4a. Furthermore, it may be provided so as to continuously cover the upper (+ Z side) surfaces of the second main body 3a and the first main body 2.

  The thin film portion 11 includes an ultrathin film portion 12 and a remaining portion 11a. The ultrathin film portion 12 is in contact with the lower side of the protective film 8. The remaining portion 11 a is in contact with the lower side of the ultrathin film portion 12. The remaining portion 11a may partially be in contact with the lower side of the protective film 8. The ultrathin film portion 12 is thinner than the remaining portion 11a. The ultrathin film portion 12 includes an analysis object 13 for TEM observation.

  The ultrathin film portion 12 has a triangular or quadrangular thin piece shape with a portion in contact with the protective film 8 as a first side (Y direction). FIG. 5B illustrates a case where the solid line is a triangle and a case where the two-dot chain line is a rectangle. The ultrathin film portion 12 includes an analysis object 13 for TEM observation inside the triangle or the rectangle. The angle α formed between the second side (side in the Z direction) that intersects the first side and is exposed to the outside and the third side that intersects the second side and is coupled to the remaining portion 11a is greater than 0 ° and 180 °. Less than °. Further, in order to increase the area of the ultrathin film portion 12, the angle α is more preferably 45 ° or more. In order to sufficiently maintain the strength of the thin film portion 11 (suppress the area of the ultrathin film portion 12), each α is preferably 135 ° or less.

  The protective film 8 is formed of a material that is harder than at least the main material of the thin film portion 11. Here, the main material of the thin film portion 11 is the material having the largest amount in the thin film portion 11. Further, it may be formed of a material whose hardness is harder than the main material of the third main body portion 4a and the second main body portion 3a. In this case, the main material is the material having the largest amount among the thin film portion 11, the third main body portion 4a, and the second main body portion 3a. Such a protective film 8 is less likely to be cut than the thin film portion 11 and the ultrathin film portion 12 even when the thin film portion 11 and the ultrathin film portion 12 are thinned. Therefore, even if the thin film portion 11 and the ultrathin film portion 12 are cut and become extremely thin, the thin film portion 11 and the ultra thin film portion 12 are held and supported by the protective film 8 that has a relatively small amount to be cut, and thus are not easily broken. That is, the protective film 8 is preferable because it can prevent the thin film portion 11 and the ultrathin film portion 12 from collapsing. Since the protective film 8 is hard to be cut compared to the thin film portion 11 and the ultrathin film portion 12, the width in the X direction is equal to the thickness (X direction) of the thin film portion 11 and the ultrathin film portion 12, or large.

  For example, when the main material such as the thin film portion 11 is silicon, since the hardness of silicon is 4.0, the hardness of the protective film 8 is preferably larger than 4.0. Thereby, when the thin film part 11 and the ultra-thin film part 12 are shaved thinly, the situation where the protective film 8 is similarly shaved and lost can be prevented. Examples of the material having high hardness include materials containing at least one of Pt, W, Ni, SiC, and DLC (Diamond-Like Carbon). In particular, these materials are materials having a hardness greater than 4.0, and are also suitable when the main material is silicon.

  The thickness of the protective film 8 is preferably 0.1 μm or more and 3 μm or less. This is because if the thickness is less than 0.1 μm, the function as the protective film 8 cannot be performed. The upper limit of the film thickness is not particularly limited, but is about 3 μm or less in consideration of ease of handling.

  In addition, the observation target position (position of the analysis target 13) in the ultrathin film portion 12 is preferably greater than 0 μm and less than or equal to 5 μm from the first side (protective film 8). As will be described later, when aiming at the effect of reducing the curtaining (the effect of reducing the influence of the unevenness of the sample), the effect is large when the analysis target 13 is near the sample surface (example: within 5 μm from the surface). It is possible. Thereby, thin film sampling in a wide area can be made possible while reducing the curtaining.

  Next, a method for manufacturing a transmission electron microscope sample according to an embodiment of the present invention will be described. FIGS. 6A to 6D, FIGS. 7A to 7B, FIGS. 8A to 8B, and FIG. 9 are schematic diagrams illustrating a method for producing a transmission electron microscope sample according to an embodiment of the present invention.

  As shown in FIG. 6A, first, a protective film 8 is formed on the upper surface of the sample 1. For example, a Pt or W target for the protective film is sputtered A1, and a Pt film or a W film is formed as the protective film 8.

  Next, as shown in FIG. 6B, FIB_B1 is irradiated from above the sample 1 to scrape the sample 1 on which the protective film 8 is formed. Thereby, as shown to FIG. 6C, the 1st main-body part 2 and the thin-body part 3 are formed. The thin body portion 3 includes a protective film 8 on the surface, extends in the lateral direction (−Y direction) from the first main body portion 2, and has a shape thinner than that of the first main body portion 2. The 1st main-body part 2 is the remainder part of the sample 1 when the thin body part 3 is cut out, and is provided with the protective film 8 on the surface. The thin body 3 is coupled to the thin body 3 on the lateral side (+ Y side) and the lower side (−Z side).

  Subsequently, as shown in FIG. 6D, the sample 1 has a component in the + Y direction from the side of the sample 1 (the side opposite to the coupling portion with the first main body portion 2 with respect to the thin body portion 3; the −Y side). In the direction, FIB_C1 is irradiated to cut the thin body portion 3. Thereby, the 2nd main-body part 3a and the thin piece part 4 are formed. The thin piece portion 4 includes a protective film 8 on the surface, extends in the lateral direction (−Y direction) from the second main body portion 3a, and has a shape thinner than the second main body portion 3a. The 2nd main-body part 3a is a remaining part of the thin-body part 3 when the thin piece part 4 is cut out, and is provided with the protective film 8 on the surface. The thin piece portion 4 is coupled to the thin piece portion 4 on the lateral side (+ Y side) and the lower side (−Z side). FIG. 7A to FIG. 7B show the process of FIG. 6D in an enlarged manner.

  Here, the reason why the FIB is irradiated from the side of the sample 1 is to solve the problem of degradation in analysis accuracy (effect of unevenness of the sample) due to the cutting. According to the inventors' research, it has been found that the curtaining that occurs when the FIB is irradiated from the upper side of the sample can be significantly reduced by irradiating the FIB from the lateral side of the sample. Therefore, at least after the step of FIG. 6D, the cutting can be significantly suppressed by irradiating the FIB from the side.

  Further, as shown in FIG. 8A (enlargement of the P1 portion in FIG. 7B), FIB_C1 is irradiated from the lateral side (−Y side) of the sample 1 in a direction having a component in the + Y direction, and the thin piece portion 4 is shaved. . Thereby, as shown to FIG. 8B, the 3rd main-body part 4a and the thin film part 11 are formed. The thin film portion 11 includes a protective film 8 on the surface, extends in the lateral direction (−Y direction) from the third main body portion 4a, and has a shape thinner than that of the third main body portion 4a. The 3rd main-body part 4a is a remaining part of the thin piece part 4 when the thin film part 11 is shaved, and is provided with the protective film 8 on the surface. The thin film part 11 is coupled to the thin film part 11 on the lateral side (+ Y side) and the lower side (−Z side).

  Further, as shown in FIG. 9 (enlargement of the Q1 portion in FIG. 8B), the thin film portion 11 is shaved by irradiating FIB_C1 from the lateral side (−Y side) of the sample 1 in a direction having a component in the + Y direction. . Thereby, the ultrathin film portion 12 and the remaining portion 11a are formed. The ultrathin film portion 12 is in contact with the lower side of the protective film 8, extends in the lateral direction (−Y direction) from the remaining portion 11a, and has a shape thinner than the remaining portion 11a. The remaining portion 11a is a remaining portion of the thin film portion 11 when the ultrathin film portion 12 is cut out, and may have a protective film 8 on the surface. The ultrathin film portion 12 is coupled to the ultrathin film portion 12 on the lateral side (+ Y side) and the lower side (−Z side). A predetermined portion of the ultrathin film portion 12 becomes an analysis target 13 by TEM.

  At this time, since the protective film 8 is difficult to be cut compared to the thin film portion 11 and the ultrathin film portion 12, the width in the X direction is compared with the thickness (X direction) of the thin film portion 11 and the ultrathin film portion 12, Equal or larger. That is, the protective film 8 may protrude in the ± X direction on the upper side (+ Z side) of the ultrathin film portion 12. Further, the protective film 8 is not necessarily formed at the stage shown in FIG. 6A, and may be formed at the stage shown in FIGS. 6C and 6D as long as it does not affect other portions.

  Here, the horizontal direction of irradiation with FIB_C1 has at least a component in the + Y direction (lateral direction) in any case. Further, the elevation angle is 0 ° to less than 90 ° (0 ° to less than 90 ° on the upper side (+ Z side)), or the depression angle is 0 ° to less than 90 ° (0 ° to less than 90 ° on the lower side (−Z side)). ) Is preferable. At this time, FIB_C1 is moved in parallel on the X-axis, and is irradiated in the predetermined angle range in the YZ plane. For example, as shown in FIG. 9, the direction in which FIB_C11 is irradiated has a component in the −Y direction, and the depression angle is 0 ° or more and less than 90 ° (0 ° or more and less than 90 ° on the lower side (−Z side)). Is the angle range. The direction of irradiating FIB_C12 has a component in the −Y direction and is in an angle range of an elevation angle of 0 ° (or a depression angle of 0 °). The direction of irradiating FIB_C13 has a component in the −Y direction, and has an elevation range of 0 ° or more and less than 90 ° (0 ° or more and less than 90 ° on the upper side (+ Z side)).

  At this time, the shape of the ultrathin film portion 12 illustrated in FIG. 9 (solid line and two-dot chain line; angle α formed between the second side and the third side) is a horizontal to upward FIB such as FIB_C12 to FIB_C13. Can be formed by irradiation. The FIB irradiation angle range is more preferably an elevation angle of 45 ° or less in order to increase the area of the ultrathin film portion 12. In addition, in order to sufficiently maintain the strength of the thin film portion 11 (suppress the area of the ultrathin film portion 12), the depression angle is preferably 45 ° or less.

  As described above, the method for manufacturing the sample for the transmission electron microscope according to the embodiment of the present invention is performed. That is, the ultrathin film portion 12 is thinner than the remaining portion 11a of the thin film portion 11 that is in contact with the lower side of the ultrathin film portion 12, and has a triangular or quadrangular flake shape with a portion in contact with the protective film 8 as a first side. The angle formed by the second side that intersects the first side and is exposed to the outside and the third side that intersects the second side and joins the remaining portion 11a is larger than 0 ° and smaller than 180 °. A sample for a scanning electron microscope is produced.

  In the present embodiment, the protective film 8 is formed in advance at a position (the surface of the ultrathin film portion 12) that does not inhibit the FIB irradiation in the process of thinning. Therefore, when the FIB is irradiated, the protective film 8 supports and holds the ultrathin film portion 12 even if the vicinity of the ultrathin film portion 12 becomes extremely thin. That is, the protective film 8 functions as a support that suppresses the collapse of the film in the ultrathin film portion 12. Accordingly, when the FIB is incident and processed from this lateral direction (+ Y direction or side surface direction), the film collapse at the ultrathin film portion 12 is only from this lateral direction (−Y direction or side surface direction). Accordingly, the region of the ultrathin film portion 12 can be formed and maintained widely. As a result, wide area thin film sampling is possible.

  Further, in this embodiment, when a thin film of a TEM sample (example: ultrathin film portion 12) is manufactured using FIB, a beam is incident from the lateral direction (+ Y direction or side surface direction) to reduce the curtaining. It aims at effect (reduction of the influence of unevenness of the sample). At this time, if there is an analysis target 13 near the sample surface (example: within 5 μm from the surface), the corner portion needs to be thinned (example: similar to the case of FIG. 4A), and the film breaks down at the time of thinning. There is a possibility that the target 13 is destroyed (example: same as in FIG. 4B). However, in this embodiment, the film collapse can be suppressed as described above by forming the protective film 8 on the sample surface in advance. That is, thin film sampling in a wide area can be achieved while reducing the curtaining.

  The present invention is not limited to the embodiments described above, and it is obvious that the embodiments can be appropriately modified or changed within the scope of the technical idea of the present invention.

DESCRIPTION OF SYMBOLS 1,101 Sample 2,102 1st main-body part 3,103 Thin body part 3a, 103a 2nd main-body part 4,104 Thin piece part 4a, 104a 3rd main-body part 8 Protective film 11,111 Thin-film part 111a Thin-film part 11a Residual part 12 Ultrathin film part 13 Analytical object

Claims (7)

(A) preparing a sample having a surface and a side surface intersecting with the surface and containing the analyte;
(B) after the step (a), forming a protective film having a hardness higher than that of the main material of the sample on the surface of the sample;
(C) After the step (b), the surface of the sample is irradiated with an ion beam, the first surface, the second surface opposite to the first surface, and the remaining portion of the protective film Forming a first protective film surface comprising a part of the first protective film surface, a first side surface comprising a part of the remaining part of the side surface, and forming a first sample part containing the analysis object;
(D) After the step (c), the first main surface is irradiated with an ion beam toward the first side surface of the first sample portion, and the first main surface and the second main surface opposite to the first main surface When, and a second protective layer surface consisting of a portion of the remaining portion of the first protective film surface, a second side surface consisting of a portion of the remaining portion of the first side surface, the enclosing the analysis object 2 Forming a sample portion;
(E) After the step (d), an ion beam is irradiated toward the second side surface of the second sample portion, and the first region containing the analysis target in the second sample portion and the analysis target Forming a second region that does not contain an object,
In the step (e), the thickness of the first region is made thinner than the thickness of the second region in a cross-sectional view. In the manufacturing method of the sample for transmission electron microscopes of Claim 1 ,
In the step (e), the irradiation direction of the ion beam is an ion beam in an angle range of an elevation angle of 0 ° to less than 90 ° or a depression angle of 0 ° to less than 90 ° with respect to the second side surface of the second sample portion. Including the step of irradiating,
A method for producing a sample for a transmission electron microscope. In the manufacturing method of the sample for transmission electron microscopes of Claim 2 ,
The step (e)
The first region is
It has a triangular or quadrangular flake shape whose first side is a portion in contact with the protective film,
A second side exposed to the outside of the first side and the intersection, the angle formed between the third side is to bind to a second side and intersects the second region, said to be smaller than 180 ° greater than 0 ° A method for producing a sample for a transmission electron microscope, including a step of forming a first region. In the manufacturing method of the sample for transmission electron microscopes as described in any one of Claims 1 thru | or 3 ,
A method for producing a sample for a transmission electron microscope, wherein the hardness of the protective film is greater than the hardness of the first sample portion. In the manufacturing method of the sample for transmission electron microscopes of Claim 4 ,
The thickness of the protective film is 0.1 μm or more and 3 μm or less. A method for manufacturing a sample for a transmission electron microscope. In the manufacturing method of the sample for transmission electron microscopes of Claim 1 ,
The method for manufacturing a sample for a transmission electron microscope, wherein the protective film includes at least one of Pt, W, Ni, SiC, and DLC (Diamond-Like Carbon). In the manufacturing method of the sample for transmission electron microscopes as described in any one of Claims 1 thru | or 6 ,
The second sample portion is located on the opposite side to the third side, connected to the second side surface, and has a fourth side intersecting the first side and the second side,
The position of the analysis object in the first region is located between the first side and the second side of the second sample part, and is arranged closer to the second side than the first side. And the manufacturing method of the sample for transmission electron microscopes located between the said 3rd side and the said 4th side, and arrange | positioned near the said 3rd side rather than the said 4th side.

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