JP3735614B2 - Transmission electron microscope observation base sample, transmission electron microscope measurement method, and transmission electron microscope apparatus - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a transmission electron microscope observation base sample, a transmission electron microscope measurement method, and a transmission electron microscope apparatus.
[0002]
[Prior art]
In general, various types of transmission electron microscope measurement samples (hereinafter also referred to as TEM measurement samples) for measurement using a transmission electron microscope (hereinafter also referred to as TEM (Transmission Electron Microscope)) and TEM measurement samples are prepared. The TEM observation method used is known. For example, a FIB (Focused Ion Beam) method and an ion milling method are widely known as methods for preparing a TEM measurement sample.
[0003]
In the FIB method, an observation target region having a thin film or a semiconductor pattern to be observed with a dicing saw is cut into a size of about 0.2 mm × 1.5 mm square, fixed to a jig for holding a sample, and then an acceleration voltage of 5 keV. This is a method for producing a TEM sample by thinning the thin film or semiconductor pattern to be observed to about 100 nm by focusing and sputtering a Ga ion beam of ˜30 keV.
[0004]
In the ion milling method, a sample and a dummy substrate are bonded to each other with an adhesive (glue), mechanically polished to a thickness of several μm in the cross-sectional direction, and then sputtered with Ar ions having an acceleration voltage of 2 keV to 5 keV to obtain a number of observation points. This is a method for producing a TEM sample by slicing from nm to several tens of nm (see, for example, Non-Patent Document 1).
[0005]
Also, a TEM sample is prepared by forming a thinned portion with the same width as the mask, leaving the area directly under the mask using lithography and reactive ion etching (hereinafter also referred to as RIE (Reactive Ion Etching)) using plasma. There is also a method (hereinafter also referred to as RIE method) (see, for example, Non-Patent Document 2).
[0006]
TEM observation is performed using the sample created using the above production method. In recent years, research on nanotechnology has been actively conducted, and so-called in-situ TEM observation, in which TEM observation is performed simultaneously with processing, is used for research on quantum properties.
[0007]
For example, a scanning tunneling microscope (Scanning Tunneling Microscope) is provided in the TEM device, and atomic images and quantized conductance are measured simultaneously (for example, see Non-Patent Document 3).
[0008]
[Non-Patent Document 1]
Masao Hirasaka, Kentaro Asakura, “FIB / Ion Milling Technique Q & A”, P.42-47 (2002)
[Non-Patent Document 2]
Hyun-Jin Cho, Peter B, Griffin, and James D. Plummer, Mat. Res. Soc. Symp. Proc. Vol. 480, 217 (1997)
[Non-Patent Document 3]
Quantized conductance through individual rows of suspended gold atoms, H. Ohnishi, Y. Kondo, K. Takayanagi, Nature, 395, 780-783 (1998)
[0009]
[Problems to be solved by the invention]
Although it is possible to prepare a sample for TEM observation and perform TEM observation by the above method, it is difficult to simply perform high-precision TEM observation. For example, since the FIB method uses a highly accelerated Ga ion beam, an amorphous layer containing Ga or an element contained in the observation sample is formed in the observation region where the electron beam is transmitted. The formed amorphous layer has a thickness of about 20 nm, which makes the TEM observation image unclear. Furthermore, since various elements are included in the formed amorphous layer, Energy Dispersive X-ray Spectrometer (EDX) and Electron Energy Loss Spectroscopy (EELS) are made difficult.
[0010]
In addition, the ion milling method can reduce the thickness of a TEM observation sample to about 10 nm, and the formation of an amorphous layer can be suppressed to about 5 nm. Therefore, an image with higher contrast than the FIB method can be obtained. However, the sample is easily bent, and it is difficult to evaluate defects and stress of the observation object.
[0011]
On the other hand, in the RIE method, since the resolution of lithography generally differs depending on the resist substrate, that is, the film type and film thickness of the object to be observed, each time a TEM observation sample is prepared by the RIE method, the focus and dose of the lithography are changed. It is necessary to make a condition. Also, in the RIE process, it is necessary to change the RIE conditions such as gas depending on the object to be shaved by RIE, that is, the type of TEM observation sample, and it takes a lot of time to prepare the TEM observation sample.
[0012]
In addition, when TEM observation is performed on fine particles having poor adhesion using a TEM sample prepared by these TEM sample preparation methods, it is necessary to pay particular attention to the preparation of the TEM sample. For example, when the above sample is observed by TEM after forming gold fine particles by sputtering (so-called gold coating) using a nitrogen target using a gold target, if a dicing saw is used during the preparation of the sample, the gold fine particles adhere to the substrate. The gold fine particles are often peeled off due to the poor quality. As described above, it is difficult to evaluate the particle size of the gold fine particles.
[0013]
Moreover, it is difficult for the once prepared TEM observation sample to perform TEM observation again after a certain process. In the case of being produced by the FIB method or ion milling method, it is often necessary to etch the paste region. Further, in many cases, the TEM observation sample formed by the RIE method cannot avoid the reaction from the side wall of the RIE process.
[0014]
Furthermore, since the TEM observation has so far required to prepare a sample for TEM observation by the above method, unlike the one-dimensional TEM observation such as the gold quantized conductance measurement mentioned in the above-mentioned literature, Reaction, especially TEM observation of the initial reaction process was virtually impossible.
[0015]
The present invention has been made in consideration of the above-described matters, and provides a transmission electron microscope observation ground sample, a transmission electron microscope measurement method, and a transmission electron microscope apparatus that can easily and accurately perform TEM observation. The purpose is to do.
[0016]
[Means for Solving the Problems]
The ground sample for transmission electron microscope observation according to the first aspect of the present invention is characterized by having a columnar protrusion having a partial region with a width of about 300 nm or less. Here, “about” means that an error in processing accuracy is included, or a fluctuation in the transmissive width of the electron beam is included.
[0017]
In the transmission electron microscope observation method according to the second aspect of the present invention, the transmission electron microscope measurement object is applied to a partial region having a width that allows transmission of the electron beam of the transmission electron microscope formed on the columnar protrusion. The formed transmission electron microscope observation sample is processed so as to fit in the holder of the transmission electron microscope, and the processed transmission electron microscope observation sample is introduced into the housing of the transmission electron microscope, and a part of the transmission electron microscope observation sample side A transmission electron microscope image is obtained by making an electron beam incident from a partial direction.
[0018]
Further, the transmission electron microscope observation method according to the third aspect of the present invention is for transmission electron microscope observation having a partial region having a width that allows transmission of an electron beam of a transmission electron microscope formed on a columnar protrusion. The base sample is processed so that it fits in the holder of the transmission electron microscope, and a transmission electron microscope observation sample is formed by forming a transmission electron microscope measurement object in a part of the processed base sample for transmission electron microscope observation. A transmission electron microscope observation sample is introduced into a housing of a transmission electron microscope, and an electron beam is incident from a side direction of a partial region of the transmission electron microscope observation sample to obtain a transmission electron microscope image.
[0019]
The transmission electron microscope observation sample from which the transmission electron microscope image was obtained was subjected to a predetermined treatment, and the transmission electron microscope observation sample subjected to the predetermined treatment was introduced into the transmission electron microscope housing, and the transmission electron microscope observation was performed. You may comprise so that an electron beam may be incident from the side part direction of the columnar projection part of a sample, and a transmission electron microscope image may be obtained.
[0020]
Note that the partial region may be a crystal region.
[0022]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
[0023]
(First embodiment)
A first embodiment of the present invention will be described with reference to FIGS.
First, the creation of a base sample for transmission electron microscope observation according to the present embodiment will be described. As shown in FIG. 1, an antireflection film 40 is formed on a silicon single crystal substrate 2 having a crystal orientation {100} as a plane orientation, and a resist 50 is applied on the antireflection film 40. Thereafter, as shown in FIG. 2, the resist 50 is patterned by an optical lithography process using KrF as a light source to form a fine line pattern 50a. Subsequently, as shown in FIG. 3, the antireflection film 40 is etched by reactive ion etching (RIE) using plasma with the fine line pattern 50a as a mask to form the fine line pattern 40a, and then the silicon substrate 1 is further deepened. The silicon substrate 2A having a single crystal projection region with a thin width (140 nm) is formed by etching about 200 nm. Thereafter, the fine line patterns 40a and 50a are peeled off, and the natural oxide film is removed by dilute hydrofluoric acid treatment, thereby forming the transmission electron microscope observation base sample 1 having a clean silicon single crystal projection region having a width of 140 nm. . The crystal plane orientation of the projection region upper surface 2a of the transmission electron microscope observation base sample 1 is {100}, and the crystal plane orientation of the side surface 2b is {011}.
[0024]
Next, as shown in FIG. 5, a 45 nm Hf silicate film 12 is deposited by a chemical vapor deposition method so as to cover the single crystal projection region. Thereafter, as shown in FIG. 6, the transmission electron microscope observation base sample 1 is processed with a dicing saw to a width of 250 μm so as to include the silicon single crystal protrusion region on which the Hf silicate film 12 is deposited, and the TEM observation sample is obtained. 10 is formed.
[0025]
Next, the TEM observation sample 10 is placed on a TEM sample holder (not shown) and introduced into the TEM casing. Then, as shown in FIG. 7, the electron beam is irradiated onto the TEM observation sample 10 from the <011> direction of the side surface of the silicon single crystal projection region, and an electron beam is imaged behind the TEM observation sample 10. A TEM observation image shown in FIG. 8 is obtained.
[0026]
Since the inside of the TEM housing into which the TEM observation sample 10 is introduced is a vacuum, as can be seen from the TEM observation image shown in FIG. 8, the surface of the Hf silicate film 12 can be easily identified. The film thickness can be calculated with high accuracy.
[0027]
Further, after depositing a 10 nm thick Hf silicate film so as to cover the single crystal protrusion region of the transmission electron microscope observation base sample 1 shown in FIG. 4, heat treatment was performed at 1000 ° C. for 10 minutes in an oxidizing atmosphere, When a TEM observation sample is prepared by performing dicing processing so as to fit in the TEM sample holder, and TEM observation is performed, a TEM observation image as shown in FIG. 9 is obtained. FIG. 9 shows that an interface layer made of substantially amorphous SiO2 is formed on a silicon substrate, and an Hf silicate film is formed on the interface layer.
[0028]
As can be seen from FIG. 9, not only the calculation of the thickness of the Hf silicate film and the information on the increase in the interface layer at the interface between the silicon substrate 2A and the Hf silicate film can be obtained, but also the upper part of the single crystal projection region of the silicon substrate 2A. Crystal fringes are observed in the Hf silicate film formed in 2a, and the crystallization of the Hf silicate film can be determined. That is, it is possible to evaluate at least as much as normal cross-sectional TEM observation.
[0029]
Further, as shown in FIG. 9, in the region of the Hf silicate film formed on the side surface 2b of the single crystal projection region of the silicon substrate 2A, the stripe pattern resulting from the crystallization of the Hf silicate film is the lattice stripe of the underlying silicon single crystal. Therefore, it is possible to make a sensitive determination of the crystallization of the film. That is, it is possible to evaluate at least as much as normal planar TEM observation.
[0030]
In the case of evaluating the film thickness and the substrate interface layer, as in this embodiment, the film thickness to be deposited is T, and T <D between the depth D of the silicon substrate 2A etched by RIE. A relationship is necessary.
[0031]
Each surface orientation of the silicon substrate is not limited to the above surface orientation, and includes, for example, the case where the surface orientation in the vertical direction of the substrate is {100} and the surface orientation of the side surface is {010}. In particular, when the vertical and side surface orientations are the same as in this case, it is possible to perform evaluation equivalent to the normal crystallinity evaluation of the epitaxial film, that is, cross-sectional TEM evaluation and planar TEM evaluation at once. is there. Usually, compared with the case where the TEM observation sample is separately prepared for the cross-sectional TEM evaluation and the planar TEM evaluation, the labor for preparing the TEM observation sample is reduced by half, and there is an advantage that the TEM observation cost is reduced.
[0032]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0033]
(Second Embodiment)
Next, a second embodiment of the present invention will be described with reference to FIGS.
First, the creation of a transmission electron microscope observation base sample according to the present embodiment will be described. As shown in FIG. 10, an oxide film is formed to a thickness of 0.6 nm on the silicon single crystal substrate 2 having the crystal orientation {100} as the plane orientation, and this oxide film is plasma-nitrided to form an oxynitride film 4. Thereafter, polysilicon 5 is deposited to a thickness of 200 nm on the oxynitride film 4, an antireflection film 40 is formed on the polysilicon 5, and a resist 50 is applied on the antireflection film 40 (see FIG. 10).
[0034]
Next, the resist 50 is patterned by an optical lithography process using KrF as a light source to form a fine line pattern 50a. Then, reactive ion etching using plasma is performed by using the fine line pattern 50a as a mask, and the antireflection film 40, the polysilicon 5, the oxynitride film 4, and the silicon substrate 2 are dug to a depth of about 200 nm. Etching is performed until it is filled (see FIG. 11). Thereafter, by a resist stripping step and a natural oxide film removing step, the silicon substrate 2A having a single crystal projection region with a thin width (60 nm), and the oxynitride film 4a and the polysilicon 5a laminated on the single crystal projection region are used. A transmission electron microscope observation base sample 1A having the laminated film is formed (see FIG. 11). The crystal plane orientation of the side surface 2b of the transmission electron microscope observation base sample 1A is {011}.
[0035]
Next, the transmission electron microscope observation ground sample 1A is processed with a dicing saw to a width of 250 μm. Then, as shown in FIG. 12, gold fine particles 13 are formed on a processed transmission electron microscope observation base sample 1A by a physical sputtering method using nitrogen plasma, thereby producing a TEM observation sample 10A.
[0036]
This TEM observation sample 10A is placed on the TEM sample holder and introduced into the transmission electron microscope casing, and the side surface of the TEM observation sample 10A, that is, the side surface direction of the silicon single crystal protrusion region of the silicon substrate 2A (the direction of the crystal orientation <011>) ) Is irradiated with an electron beam to form an image of the electron beam behind the TEM observation sample 10A to obtain a TEM observation image as shown in FIG. In FIG. 13, the thin and dark portions indicate gold fine particles 13, and the white dots in the silicon substrate region indicate regions (so-called lattice images) surrounded by Si atoms. And since the Si atoms in the crystal region are regularly arranged, the absolute scale of the TEM image obtained from the spacing of the white dots can be calculated, and the particle size of the thin blackened portion, that is, the gold fine particles can be measured. it can.
[0037]
When TEM evaluation is performed on a TEM evaluation sample that has poor adhesion to the ground sample that may be peeled off by water used during dicing, or a sample that reacts with water, as in this embodiment, the TEM evaluation target Before forming the object (gold fine particles 13 in this embodiment), the TEM observation ground sample 1A is processed to a size that can be introduced into the TEM sample holder, and then the TEM evaluation object is formed.
[0038]
In addition, when TEM evaluation of gold fine particles with poor adhesion is performed, the conventional TEM measurement method using FIB, ion milling, etc., uses a dicing saw to squeeze the sample to a certain size before processing the sample in advance. It was necessary to process. For this reason, in the conventional method, gold fine particles may be peeled off during dicing before TEM evaluation, and it is necessary to recreate a TEM evaluation sample.
[0039]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0040]
In general, substance A and substances B ₁ , B ₂ ,…., When examining the reactivity with the substance B first, as in this embodiment ₁ , B ₂ , ... are formed on the single crystal protrusion region of the silicon substrate 2A, reacted with the substance A after being subjected to RIE, and the reactivity with each substance can be examined at once. . For example, Si consisting of Si and Ge _x Ge _1-x After depositing Ti, Co, or Ni, which forms a silicidation reaction, on the projection area consisting of multiple layers and applying heat treatment to form silicide, each composition Si _x Ge _1-x The details of each silicidation reaction can be examined. Further, this composition may be changed in an inclined manner.
[0041]
(Third embodiment)
Next, a third embodiment of the present invention will be described with reference to FIGS.
First, the transmission electron microscope observation base sample according to the present embodiment is formed of a silicon single crystal whose crystal plane orientation {100} is the plane orientation of the substrate surface, and the shape of the transmission electron of the first embodiment shown in FIG. A ground sample 2A for microscopic observation, in which the width of a clean silicon single crystal protrusion region is 60 nm. Therefore, the crystal plane orientation of the upper surface of the silicon single crystal protrusion region is {100} and the side crystal plane orientation is {011}.
[0042]
Then, the surface of the silicon single crystal projection is oxidized by annealing the transmission electron microscope observation base sample 2A in a 1000 ° C. oxidizing atmosphere, and a silicon oxide film 14 is formed on the surface as shown in FIG. Then, a TEM observation sample 10B is obtained by processing the dicing saw to a width of 250 μm so as to include the silicon single crystal protrusion region.
[0043]
The TEM observation sample 10B is placed on the TEM sample holder and introduced into the transmission electron microscope casing, and as shown in FIG. 15, the TEM observation sample 10B is applied to the TEM observation sample 10B from the {011} direction of the side surface of the silicon single crystal projection region. An electron beam is irradiated and an electron beam is imaged behind the TEM observation sample 10B, whereby a TEM observation image of the silicon oxide film 14 is obtained. Thereby, as in the first and second embodiments, the film thickness of the silicon oxide film can be accurately evaluated.
[0044]
When the film thickness is evaluated, as shown in FIG. 14, if the film thickness to be deposited is T and the substrate depth D etched by RIE, the relationship of T <D is necessary.
[0045]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0046]
In the third embodiment, the surface of the silicon single crystal protrusion region of the transmission electron microscope observation base sample 2A is oxidized to form the silicon oxide film 14 on the surface, and then processed to a width of 250 μm with a dicing saw. In this way, the TEM observation sample 10B was obtained. Before forming the silicon oxide film 14, it was processed to a width of 250 μm with a dicing saw, and then the surface of the silicon single crystal region was oxidized to form a silicon oxide film on the surface. You may do it.
[0047]
(Fourth embodiment)
Next, a fourth embodiment of the present invention will be described with reference to FIGS. First, the transmission electron microscope observation base sample according to the present embodiment is formed of a silicon single crystal whose crystal plane orientation {100} is the plane orientation of the substrate surface, and the shape of the transmission electron of the first embodiment shown in FIG. A ground sample 2A for microscopic observation, in which the width of a clean silicon single crystal protrusion region is 60 nm. The crystal plane orientation of the upper surface of this silicon single crystal projection region is {100} and the side crystal plane orientation is {011}.
[0048]
SiH is deposited by chemical vapor deposition on the single-crystal projection area of the ground sample 2A for transmission electron microscope observation. _Four After depositing an amorphous silicon film at 600 ° C. using (silane) gas, the silane gas was stopped and N ₂ As shown in FIG. 16, the epitaxial growth of the amorphous silicon film using the substrate single crystal silicon as a seed is promoted, and the epitaxial growth film is formed on the silicon single crystal protrusion region as shown in FIG. 15 is formed. Then, by processing to a thickness of 250 microns with a dicing saw so as to include the silicon single crystal projection region, an observation sample for TEM 10C as shown in FIG. 16 is obtained.
[0049]
This TEM observation sample 10C was placed on a TEM sample holder and introduced into the transmission electron microscope casing, and as shown in FIG. 17, an electron beam was applied to the TEM observation sample 10C from the <011> direction of the side surface of the silicon single crystal projection region. Is irradiated to form an electron beam behind the TEM observation sample 10C to obtain a TEM observation image. As a result, as in the first and second embodiments, the film thickness evaluation, crystallinity evaluation, and evaluation of the interface layer with the substrate can be performed precisely.
[0050]
The film evaluation of the epitaxial growth can be applied not only to the solid phase epitaxial growth film as described above but also to a vapor phase epitaxial growth film.
[0051]
In the case of evaluating the film thickness and the substrate interface layer, as shown in FIG. 16, if the film thickness to be deposited is T and the substrate depth D etched by RIE, the relationship of T <D is necessary. .
[0052]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0053]
Note that the surface orientations of the substrate are not limited to the above-mentioned surface orientations. Other examples include the case where the surface orientation in the vertical direction of the substrate is (100) and the surface orientation of the side surface is (010). In particular, when the vertical and side surface orientations are the same as in this case, it is possible to perform evaluation equivalent to the crystallinity judgment of a normal epitaxial film, that is, cross-sectional TEM evaluation and planar TEM evaluation at a time. . Usually, compared with the case where the TEM sample is separately prepared for the cross-sectional TEM evaluation and the planar TEM evaluation, the labor for preparing the TEM sample is reduced by half, and there is an advantage that the TEM observation cost is reduced.
[0054]
(Fifth embodiment)
A fifth embodiment of the present invention will be described with reference to FIGS.
First, the creation of a base sample for transmission electron microscope observation according to the present embodiment will be described. As shown in FIG. 18, a silicon nitride film 6 is deposited on a silicon {100} substrate 2 having a surface Miller index of {100}. Thereafter, an antireflection film 40 is formed on the silicon nitride film 6, and a resist 50 is applied on the antireflection film 40.
[0055]
Next, as shown in FIG. 19, the resist 50 is patterned by a lithography process using KrF as a light source to form a fine line pattern 50a. Using the fine line pattern 50a as a mask, the antireflection film 40 and the silicon nitride film 6 are patterned by a reactive ion etching process using plasma to form the fine line pattern 40a and the nitride film 6a, and the silicon substrate 2 is processed to obtain a width. A silicon substrate 2A having a columnar portion of about 60 nm is formed (see FIG. 20). Note that the depth of digging the silicon substrate to form the columnar portion is about 200 nm.
[0056]
Then O ₂ After the resist ashing treatment by plasma and the resist 50a and the antireflection film 40a are peeled off by a mixed solution of sulfuric acid and hydrogen peroxide, the surface of the silicon substrate 2A is oxidized in an oxidizing atmosphere at 1000 ° C. As shown in FIG. A silicon oxide film 7 is formed on the side surface of the part. At this time, since the nitride film 6a is formed on the upper surface of the columnar portion, the upper surface of the columnar portion is not oxidized.
[0057]
Thereafter, the nitride film 6a that became a mask for oxidation is peeled off using hot phosphoric acid (see FIG. 22), the upper surface of the columnar portion of the silicon substrate 2A is exposed, and then silane gas is allowed to flow under a reduced pressure of 800 ° C. Silicon is epitaxially grown using the exposed surface of the columnar portion of the silicon substrate 2A as a seed to form a TEM observation sample 10D in which an epitaxial growth film 16 is formed on the upper surface of the columnar portion (see FIG. 23).
[0058]
This TEM observation sample 10D is processed into a size that can be accommodated in a TEM observation holder by using a dicing saw, and as shown in FIG. 24, TEM observation is performed by transmitting an electron beam from the lateral direction of the columnar portion.
[0059]
According to the present embodiment, the epitaxial growth is limited to the upper surface of the columnar portion of the silicon substrate 2A, and the side wall portion and the corner portion of the columnar silicon region can suppress the epitaxial growth. Limited TEM observation is possible. It is also possible to observe the crystallinity in the case where the oxide film 7 is grown on the oxide film 7 and epitaxially grown laterally. The plane index of the silicon substrate of the above embodiment is not limited to {100}, and a general plane index is possible. Further, the base substrate is not limited to a silicon single crystal, but can include single crystal and polycrystalline substrates of general compound semiconductors such as GaAs, GaN, and InGaN including SiGe and SiGeC.
[0060]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0061]
(Sixth embodiment)
A sixth embodiment of the present invention will be described with reference to FIGS.
First, the creation of a base sample for transmission electron microscope observation according to the present embodiment will be described. An antireflection film is formed on a silicon substrate having a mirror index of {100} on the surface, a resist is applied on the antireflection film, and silicon is formed by a lithography process using KrF as a light source and a reactive ion etching process using plasma. The substrate is processed to form a silicon substrate 2A having a columnar portion with a thickness of about 60 nm. Note that the depth of digging the silicon substrate is about 200 nm. O ₂ After the resist ashing treatment by plasma and the resist and the antireflection film are peeled off by a mixed solution of sulfuric acid and hydrogen peroxide, the entire surface of the silicon substrate is oxidized in an oxidizing atmosphere at 1000 ° C. to form a silicon oxide film 7 (see FIG. 25). .
[0062]
Subsequently, as shown in FIG. 26, a silicon nitride film 8 is deposited on the silicon oxide film 7, and then the silicon nitride film 8 is etched by reactive ion etching using plasma, and silicon is formed only on the side of the columnar portion. The nitride film 8a is left (see FIG. 27). Then, the surface of the silicon substrate 2A is treated with dilute hydrofluoric acid to form side walls made of the silicon oxide film 7a and the silicon nitride film 8a only on the side portions of the columnar portion, thereby obtaining a transmission electron microscope measurement sample 1C. (See FIG. 28).
[0063]
Thereafter, a silane gas is allowed to flow through the transmission electron microscope measurement sample 1C under a reduced pressure of 800 ° C., silicon is epitaxially grown using the exposed surface of the silicon substrate 2A as a seed, an epitaxial growth film 16 is formed, and a TEM observation sample 10E is formed. (See FIG. 29).
[0064]
The TEM observation sample 10E is processed into a size that fits into the TEM observation holder using a dicing saw (see FIG. 30), and TEM observation is performed by transmitting an electron beam from the lateral direction of the columnar portion of the TEM observation sample 10E ( (See FIG. 31).
[0065]
According to the present embodiment, the observed epitaxial growth is limited to the upper surface of the columnar part, and the epitaxial growth of the side wall part and the corner part of the columnar part can be suppressed. TEM observation is possible. In addition, it is possible to observe the crystallinity when the oxide film 7a is grown on the oxide film 7a and epitaxially grown laterally.
[0066]
The plane index of the silicon substrate is not limited to {100}, and a general plane index is possible. The base substrate is not limited to a silicon single crystal, but includes single crystal and polycrystalline substrates of general compound semiconductors such as GaAs, GaN, and InGaN including SiGe and SiGeC.
[0067]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0068]
(Seventh embodiment)
A seventh embodiment of the present invention will be described with reference to FIGS.
First, the creation of a base sample for transmission electron microscope observation according to the present embodiment will be described. As shown in FIG. 32, a silicon nitride film is formed on a silicon single crystal substrate having a crystal orientation of {100} as a plane orientation, and the silicon nitride film and the silicon single crystal substrate are etched using a lithography process. Transmission electron microscope observation base sample having a silicon substrate 2A having a columnar portion with a top surface orientation of {100} and a side surface orientation of {011}, and a silicon nitride film 6a formed on the top surface of the columnar portion Get 1D.
[0069]
Next, an Hf silicate film having a thickness of 4 nm is deposited on the transmission electron microscope observation base sample 1D, and is processed into a size that can be accommodated in a TEM observation holder by using a dicer to obtain a TEM observation sample 10F (see FIG. 10F). TEM observation is performed by transmitting an electron beam from the lateral direction of the columnar portion of the TEM observation sample 10F.
[0070]
In general, when an Hf silicate film is directly deposited on a silicon substrate, an interface layer is formed at the interface between the silicon substrate and the Hf silicate film. However, as in the present embodiment, an oxide resistant film is formed on the silicon substrate. The original heat resistance of the Hf silicate film can be evaluated by depositing it on the surface.
[0071]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0072]
(Eighth embodiment)
An eighth embodiment of the present invention will be described with reference to FIGS.
First, the creation of a base sample for transmission electron microscope observation according to the present embodiment will be described. Silicon nitride film patterned on the silicon substrate 2 by patterning the silicon nitride film on the silicon single crystal substrate having a crystal orientation of {100} in a 4 nm volume and patterning the silicon nitride film using a lithography process A ground sample 1E for transmission electron microscope observation on which the film 6a is formed is obtained (see FIG. 35).
[0073]
A 4 nm thick Hf silicate film 12 is deposited on the transmission electron microscope observation base sample 1E, and then processed into a size that can be accommodated in a TEM observation holder using a dicer to form a TEM observation sample 10G (see FIG. 35). . TEM observation is performed by transmitting an electron beam from the lateral direction of the columnar portion of the TEM observation sample 10G.
[0074]
Generally, the silicon nitride film and the apparatus for processing silicon are usually different, but if a base sample for transmission electron microscope observation is formed as in the present embodiment, the labor of processing can be saved.
[0075]
This embodiment can be used when it is desired to easily perform crystallinity evaluation such as heat resistance of a film rather than film thickness evaluation.
[0076]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0077]
(Ninth embodiment)
Next, a ninth embodiment of the present invention will be described with reference to FIGS. First, a silicon substrate is processed by a lithography process and an RIE method to form a transmission electron microscope observation base sample 1F composed of a silicon substrate 2A having a triangular columnar portion having a maximum width of 100 nm and a height of 200 nm (see FIG. 37).
[0078]
Thereafter, the silicon region on the triangular prism shape is cleaned by dilute hydrofluoric acid treatment of the silicon substrate 2A, and then the Hf silicate film 12 is deposited by 4 nm by the CVD method to obtain a TEM observation sample 10H (see FIG. 38). This TEM observation sample 10H is processed into a size that can be accommodated in a TEM holder using a dicing saw, and TEM observation is performed (see FIG. 38). Thereafter, the sample 10H for TEM observation is heat-treated in an oxidizing atmosphere at 1000 ° C. for 10 minutes, and then TEM observation is performed again.
[0079]
In general, it is known that when a TEM observation sample is made by digging up a substrate by RIE after deposition of an Hf silicate film, the Hf silicate film is wedge-oxidized.
[0080]
In the present embodiment, since the Hf silicate film 12 is deposited on the entire surface after the RIE process of the silicon substrate, it is possible to heat-treat the Hf silicate film 12 without the Hf silicate film 12 being wedge-oxidized. Furthermore, since the heat treatment and TEM observation can be repeated a plurality of times for the same sample, it is possible to save the trouble of preparing the TEM observation sample. Further, since the same sample can be observed by TEM, there is no variation between samples, and high-precision TEM evaluation can be performed at low cost.
[0081]
The present embodiment is not limited to heat treatment, and can be used for evaluating the resistance of a film to wet treatment such as dilute hydrofluoric acid treatment. In addition, an evaluation in which these different processes are appropriately combined is also possible.
[0082]
As described above, according to the present embodiment, a transmission electron microscope observation ground sample capable of easily performing highly accurate TEM observation, and a transmission electron microscope measurement method using the transmission electron microscope observation ground sample Can be obtained.
[0083]
Note that the transmission electron microscope observation base sample in the first to ninth embodiments is not limited to the shape shown in FIG. 37, and as shown in FIG. 39, a transmission electron microscope having a columnar columnar portion. The observation ground sample 1G may be used. Also in this case, the TEM observation sample 10I as shown in FIG. 40 can be obtained by depositing the Hf silicate film 12 on the entire surface of the transmission electron microscope observation base sample 1G. In addition, the RIE may have a shape (taper) with a side wall having an angle depending on conditions. By using this, it is possible to create a transmission electron microscope observation base sample 1H having a shape as shown in FIG. By depositing the Hf silicate film 12 on the entire surface of the transmission electron microscope observation base sample 1H, a TEM observation sample 10J as shown in FIG. 42 can be obtained. When these transmission electron microscope observation base samples are used, there are extremely thin regions as shown in FIGS. 37, 39, and 41. However, the higher the electron beam transmission thickness, the higher the resolution of the TEM image. There is an advantage that a high-resolution TEM observation image can be obtained in a thin region.
[0084]
In the first to ninth embodiments, the transmission electron microscope observation base sample having the projection region is formed using reactive ion etching, but is not limited to reactive ion etching. For example, as shown in FIG. 43, a mask 60 is formed on the silicon substrate 2, and wet etching is performed with a mixed solution of hydrofluoric acid and nitric acid, thereby observing a transmission electron microscope made of the silicon substrate 2E having the shape shown in FIG. A base sample base can be created. Further, as shown in FIG. 43, a mask 60 is formed on the silicon substrate 2, and an aqueous solution of ethylenediamine and pyrocatechol is used to anisotropically etch as shown in FIG. A base sample for transmission electron microscope observation made of a silicon substrate can be prepared. As shown in FIG. 46, it is also possible to form the mask 62 only in a predetermined region on the silicon substrate 2 and form the protrusion 20 in the region not covered with the mask 62 by using epitaxial growth.
[0085]
It is also effective to repeatedly perform etching or oxidation when forming the base substrate in the above embodiment. For example, after a silicon substrate 2A having a silicon protrusion region as shown in FIG. 47 is formed by the RIE method, as shown in FIG. 48, the entire surface of the silicon substrate 2A is oxidized to form an oxide film 22, and further diluted hydrofluoric acid. By performing the processing, a transmission electron microscope observation base sample made of the silicon substrate 2G having a protruding region having a shape as shown in FIG. 49 can be created. The width of the protruding region through which the electron beam is transmitted can be made equal to or smaller than a limit width that can be manufactured by a lithography process. Therefore, by forming an observation object on the transmission electron microscope observation base sample and performing TEM observation, a higher-resolution TEM observation image can be obtained.
[0086]
By the way, in the first to ninth embodiments, as shown in FIG. 50, the sample for TEM observation forms an observation film (not shown) on the R silicon substrate 2A having a plurality of protrusions. After that, it is formed by processing with a dicing saw 70 so as to fit in a TEM holder of a transmission electron microscope. Currently, the thickness Lds of the thinnest dicing saw 70 is 5 μm. Therefore, the distance Ls between the protrusions needs to be larger than the thickness Lds of the dicing saw 70. Further, the width Ll of the protrusion needs to be thin enough to transmit the electron beam, and Ll ≦ 300 nm. That is, the width Ll of the protrusion is about 300 nm or less. Here, “about” means that an error in processing accuracy is included, or a fluctuation in the transmissive width of the electron beam is included.
[0087]
In addition to dicing that fits in the TEM holder, additional RIE or wet etching methods, or simply by opening the walls, taking advantage of the characteristics of the silicon single crystal substrate being easily opened on the {111} plane In particular, it is also effective to draw a guide line having an appropriate curvature and open the wall to a very small width.
[0088]
(10th embodiment)
Next, a transmission electron microscope according to the tenth embodiment of the invention is illustrated. 51 Will be described with reference to FIG. Figure 51 These are block diagrams which show the structure of the transmission electron microscope apparatus 100 by this embodiment.
[0089]
The transmission electron microscope apparatus according to this embodiment includes a transmission electron microscope 110, an epitaxial film forming apparatus 140, and a load lock 150. The transmission electron microscope 110 includes an electron gun 112, a focusing lens 114, an objective lens 116, a limited field stop 118, an intermediate lens 120, a projection lens 122, and a fluorescent plate 124. Is provided in the housing.
[0090]
The epitaxial film forming apparatus 140 is in an ultra-high vacuum state (1 × 10 ^-6 An apparatus for depositing an epitaxial film on a base sample for transmission electron microscope observation (not shown) at about Pa), and is connected to the transmission electron microscope 110 via a load lock 150. In the epitaxial film forming apparatus 140, the ground sample for observation with a transmission electron microscope having the protrusions in the fifth embodiment or the sixth embodiment is introduced. Hydrogen gas, which is a reducing gas, is introduced into the epitaxial film forming apparatus 140 under an ultrahigh vacuum of 800 ° C., and the natural oxide film formed on the surface of the base sample for transmission electron microscope observation is removed. Subsequently, silane (SiH _Four ) Gas is introduced, and vapor phase epitaxial growth of silicon is performed by using the exposed silicon region as a seed, thereby producing a TEM observation sample 10 on which an epitaxial film is formed.
[0091]
Next, the created TEM observation sample 10 is conveyed to the load lock 150. The load lock 150 has a reduced pressure (1 × 10 10) compared to the transmission electron microscope 110 and the epitaxial film forming apparatus 140. ^-4 And a valve (not shown) is provided at the boundary between the transmission electron microscope 110 and the epitaxial film forming apparatus 140. In addition, when the TEM observation sample 10 is carried into the load lock 140 from the epitaxial film forming apparatus 140 or carried out to the transmission electron microscope 110, the pressure inside the load lock 140 is set to an ultra high vacuum state. A pump (not shown) is provided.
[0092]
The TEM observation sample 10 carried out from the load lock 150 to the transmission electron microscope 110 is disposed between the focusing lens 114 and the objective lens 116. The electron beam emitted from the electron gun 112 is focused by the focusing lens 114 and passes through the TEM observation sample 10. The electron beam transmitted through the TEM observation sample 10 enters the fluorescent plate 124 through the objective lens 116, the limited field stop 118, the intermediate lens 120, and the projection lens 122, and an electron microscope image of the TEM observation sample 10 is formed on the fluorescent plate 124. TEM observation is performed.
[0093]
In general, the crystallinity of an epitaxial film is important, and defects in the epitaxial film are often evaluated by TEM. Conventionally, the epitaxial film is once returned to room temperature and placed in the TEM. However, when the temperature is lowered from the high epitaxial temperature of 800 ° C. to room temperature, thermal stress is applied to the epitaxial film. When the existence of a defect is recognized in the epitaxial film, it is usually difficult to judge whether the defect is due to the growth of the epitaxial film or the thermal stress when the temperature is lowered.
[0094]
However, if the transmission electron microscope apparatus 100 of this embodiment is used, it is possible to observe “in-situ” during the growth of the epitaxial film. It is possible to determine the conditions.
[0095]
In the present embodiment, the transmission electron microscope 110 and the epitaxial film forming apparatus 140 are connected via the load lock 150, but may be configured to be in the same vacuum furnace.
[0096]
In the tenth embodiment, the epitaxial film forming apparatus 140 is provided with the transmission electron microscope. However, an ultrahigh vacuum chemical vapor deposition apparatus or the like may be provided. In-situ TEM observation such as crystallinity, film thickness, and particle size can be performed.
[0097]
Needless to say, TEM observation can be applied not only to taking a real image but also to various observation methods generally associated with TEM observation such as EELS, EDX, and electron diffraction.
[0098]
As described above, using the transmission electron microscope observation ground sample according to any one of the first to ninth embodiments of the present invention, the TEM observation target is the transmission electron microscope observation ground sample. The TEM observation sample is formed into a TEM observation sample, and the TEM observation sample only needs to be processed into a size that can be accommodated in the TEM observation holder.
[0099]
Further, according to the tenth embodiment of the present invention, TEM observation can be performed immediately after film formation, and the time required to obtain a TEM observation image can be further shortened. If the cleanness of the base does not satisfy the specifications of the cleanliness of the apparatus for forming the TEM observation object, it is necessary to prepare the TEM observation sample according to the first to ninth embodiments and perform the TEM observation. . In general, an apparatus for flowing a product in a clean room requires a high degree of cleanliness for a wafer to be put in the apparatus. When TEM observation is performed on the film quality and film thickness of a film forming apparatus in such a clean room, the first through The ninth embodiment may be used.
[0100]
Further, by forming the transmission electron microscope observation base sample with a general lithography apparatus and RIE, a large number of transmission electron microscope observation base samples of the first to ninth embodiments can be formed. For example, when a base sample for transmission electron microscope observation can be formed on each chip after opening a wall on each chip, if a TEM observation target is separately formed on each base sample, the TEM observation sample There is an advantage that the unit cost for sample preparation per unit can be lowered.
[0101]
According to an embodiment of the present invention, the initial state of reaction such as atomic surface diffusion and polymerization can be observed by TEM, and film growth and the like, which have been difficult until now, can be observed in situ.
[0102]
Further, according to one embodiment of the present invention, it is possible to easily calibrate the length of the TEM observation image from the crystal lattice spacing of the base region, and to accurately adjust the film thickness, grain size, etc. of the TEM observation target. Can be identified.
[0103]
Conventionally, glue or metal is usually attached to the surface of a TEM observation sample for the purpose of reinforcing the strength of the TEM observation sample. In some cases, it may react with the observation object. For example, when evaluating the thickness of the silicon oxide film, the boundary with the paste layer formed on the surface is unclear, and it is difficult to measure the accurate thickness. In general, it is difficult to remove the layer formed on this surface before TEM observation.
[0104]
On the other hand, according to each embodiment of the present invention, it is not necessary to attach glue or metal to reinforce the strength of the TEM observation sample, and an accurate film thickness can be measured. .
[0105]
Further, according to each embodiment of the present invention, the surface of the TEM observation sample at the time of TEM observation is easy to identify because the inside of the case of the transmission electron microscope is vacuum, and the TEM observation is easily and accurately performed. It is feasible.
[0106]
In addition, it is relatively easy to remove the TEM observation inhibition region formed on the surface of the base at the time of base preparation by performing appropriate processing, and high-precision TEM observation can be performed. For example, when a silicon substrate is etched by RIE in an oxygen atmosphere to form a region on a pillar having a thickness of about 50 nm and the resist is peeled off, RIE shavings adhere to the shaved sidewall, A natural oxide film is formed on the surface of the silicon substrate directly underneath, and this causes disturbance of TEM observation. However, these oxide film regions are not affected by the characteristics of the substrate before the TEM observation object is formed. It can be easily removed by dilute hydrofluoric acid treatment with high selectivity to the silicon substrate. Therefore, if the base according to each embodiment of the present invention is used, TEM observation can be performed after removing the disturbance factors other than the TEM observation object as much as possible, so that a highly accurate TEM image can be obtained. In addition, since the width of the base can be defined by lithography, it is easy to make the thickness of the electron beam transmitted in the TEM observation region, and it becomes possible to avoid uncertain factors due to the thickness as much as possible. For this reason, highly accurate TEM observation can be performed.
[0107]
Further, by subjecting the base to oxidation and etching, it is possible to relatively easily form a projection region below the lithography limit, and a high-resolution TEM image can be easily obtained.
[0108]
The light source used in the lithography process is not limited to KrF as described above. ArF, F ₂ And general light sources such as electron beams and X-rays. Alternatively, the patterned stencil mask may be made to adhere to or non-contact with the object to be etched and the base sample may be etched.
[0109]
【The invention's effect】
As described above, according to the present invention, high-accuracy TEM observation can be easily performed.
[Brief description of the drawings]
FIG. 1 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to a first embodiment of the present invention.
FIG. 2 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to the first embodiment of the present invention.
FIG. 3 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to the first embodiment of the present invention.
FIG. 4 is a cross-sectional view showing a configuration of a base sample for transmission electron microscope observation according to the first embodiment of the present invention.
FIG. 5 is a process cross-sectional view showing a TEM observation sample manufacturing process according to the first embodiment of the present invention.
FIG. 6 is a plan view showing a manufacturing process of a TEM observation sample according to the first embodiment of the present invention.
FIG. 7 is a perspective view for explaining a transmission electron microscope observation method according to the first embodiment of the present invention.
FIG. 8 is a photograph showing a TEM observation image observed by the transmission electron microscope observation method according to the first embodiment of the present invention.
FIG. 9 is a photograph showing a TEM observation image observed by the transmission electron microscope observation method according to the first embodiment of the present invention.
FIG. 10 is a process cross-sectional view showing a manufacturing process of a transmission electron microscope observation base sample according to a second embodiment of the present invention.
FIG. 11 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation ground sample according to a second embodiment of the present invention.
FIG. 12 is a sectional view showing a transmission electron microscope observation method according to a second embodiment of the present invention.
FIG. 13 is a photograph showing a TEM observation image observed by a transmission electron microscope observation method according to the second embodiment of the present invention.
FIG. 14 is a cross-sectional view showing a configuration of a TEM observation sample according to a third embodiment.
FIG. 15 is a perspective view showing a transmission electron microscope observation method according to a third embodiment.
FIG. 16 is a cross-sectional view showing a configuration of a TEM observation sample according to a fourth embodiment.
FIG. 17 is a perspective view showing a transmission electron microscope observation method according to a fourth embodiment.
FIG. 18 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to a fifth embodiment.
FIG. 19 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to a fifth embodiment.
FIG. 20 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to a fifth embodiment.
FIG. 21 is a sectional view showing the structure of a transmission electron microscope observation base sample according to a fifth embodiment.
FIG. 22 is a cross-sectional view showing a TEM observation sample manufacturing process according to the fifth embodiment.
FIG. 23 is a sectional view showing the structure of a TEM observation sample according to a fifth embodiment.
FIG. 24 is a perspective view for explaining a transmission electron microscope observation method according to a fifth embodiment.
FIG. 25 is a process cross-sectional view showing the manufacturing process of the transmission electron microscope observation base sample according to the sixth embodiment.
FIG. 26 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to the sixth embodiment.
FIG. 27 is a process cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to the sixth embodiment.
FIG. 28 is a sectional view showing the structure of a transmission electron microscope observation base sample according to the sixth embodiment.
FIG. 29 is a sectional view showing the structure of a TEM observation sample according to a sixth embodiment.
FIG. 30 is a plan view showing a TEM observation sample manufacturing process according to the sixth embodiment.
FIG. 31 is a perspective view for explaining a transmission electron microscope observation method according to a sixth embodiment.
FIG. 32 is a cross-sectional view showing the configuration of a transmission electron microscope observation base sample according to a seventh embodiment.
FIG. 33 is a sectional view showing the structure of a TEM observation sample according to a seventh embodiment.
FIG. 34 is a perspective view for explaining a transmission electron microscope observation method according to a seventh embodiment.
FIG. 35 is a sectional view showing the structure of a TEM observation sample according to an eighth embodiment.
FIG. 36 is a perspective view for explaining a transmission electron microscope observation method according to an eighth embodiment.
FIG. 37 is a sectional view showing the structure of a transmission electron microscope observation base sample according to the ninth embodiment.
FIG. 38 is a perspective view for explaining a transmission electron microscope observation method according to a ninth embodiment.
FIG. 39 is a cross-sectional view showing the configuration of a transmission electron microscope observation base sample according to a modification of the ninth embodiment.
FIG. 40 is a perspective view illustrating a transmission electron microscope observation method according to a modification of the ninth embodiment.
41 is a cross-sectional view showing the configuration of a transmission electron microscope observation base sample according to another modification of the ninth embodiment. FIG.
FIG. 42 is a perspective view for explaining a transmission electron microscope observation method according to another modification of the ninth embodiment.
FIG. 43 is a cross-sectional view illustrating a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 44 is a cross-sectional view for explaining a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 45 is a cross-sectional view for explaining a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 46 is a cross-sectional view for explaining a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 47 is a cross-sectional view for explaining a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 48 is a cross-sectional view for explaining a manufacturing process of a transmission electron microscope observation base sample according to an embodiment of the present invention.
FIG. 49 is a cross-sectional view showing the configuration of a base sample for observation with a transmission electron microscope according to one embodiment of the present invention.
FIG. 50 is a view for explaining the width of the protrusions and the limit of the interval between the protrusions of the transmission electron microscope observation base sample according to the embodiment of the present invention.
FIG. 51 is a block diagram showing a configuration of a transmission electron microscope apparatus according to a tenth embodiment of the present invention.
[Explanation of symbols]
1 Ground sample for transmission electron microscope observation
2 Silicon substrate
4 Silicon oxynitride film
5 Polysilicon film
6 Silicon nitride film
7 Silicon oxide film
8 Silicon nitride film
10 TEM observation sample
12 Hf silicate membrane
13 Gold fine particles
14 Silicon oxide film
15 Epitaxial growth film
16 Epitaxial growth film
40 Anti-reflective coating
50 resists
60 mask
70 dicing saw
100 Transmission electron microscope apparatus
110 Transmission electron microscope
112 electron gun
114 focusing lens
116 Objective lens
118 Restricted field stop
120 Intermediate lens
122 Projection lens
124 fluorescent screen
140 Epitaxial film deposition system
150 Load lock

Claims (5)

  A base sample for observation with a transmission electron microscope, comprising a columnar protrusion having a partial region with a width of about 300 nm or less.   A transmission electron microscope observation sample in which a transmission electron microscope measurement object is formed in a partial region having a width that allows transmission of an electron beam of a transmission electron microscope formed on a columnar projection so as to fit in the holder of the transmission electron microscope. The processed transmission electron microscope observation sample is introduced into the case of the transmission electron microscope, and an electron beam is incident from the side of the partial region of the transmission electron microscope observation sample to obtain a transmission electron microscope image. And a transmission electron microscope observation method.   Processing a transmission electron microscope observation ground sample provided with a partial region having a width that allows transmission of an electron beam of a transmission electron microscope formed on a columnar projection so as to fit in the holder of the transmission electron microscope. A transmission electron microscope measurement object is formed on the partial region of the transmitted transmission electron microscope observation base sample to create a transmission electron microscope observation sample, and the transmission electron microscope observation sample is placed in the casing of the transmission electron microscope. A transmission electron microscope observation method comprising introducing an electron beam from a side direction of the partial region of the transmission electron microscope observation sample to obtain a transmission electron microscope image.   The transmission electron microscope observation sample from which the transmission electron microscope image was obtained is subjected to a predetermined treatment, and the transmission electron microscope observation sample subjected to the predetermined treatment is introduced into a case of the transmission electron microscope, and the transmission electron microscope 4. The transmission electron microscope observation method according to claim 2, wherein an electron beam is incident from a side direction of the columnar protrusion of the microscope observation sample to obtain a transmission electron microscope image.   5. The transmission electron microscope observation method according to claim 2, wherein the partial region is a crystal region.

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