JP2001124676A - Sample support member for electron microscopic observation - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample support member for electron microscopic observation capable of easily fixing and safely treating an extracted minute sample piece when extracting a more minute sample piece from a sample by FIB working and working it into a TEM sample. SOLUTION: In this sample support member for electron microscopic observation, the thickness of a minute sample piece fixing part is set to the thickness of a minute sample piece or more, and projection parts having a thickness and height larger than those of the minute sample piece are provided on both sample fixing-side ends of the sample support member. Further, the irregularities of the part for fixing the sample piece of the sample support member is set to 5 μm or less.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preparing a sample for observation with an electron microscope, and more particularly, to extracting a finer sample piece from the sample with a focused ion beam (hereinafter, FIB) processing apparatus, and using a transmission electron microscope. The present invention relates to a sample support member for electron microscope observation, which can easily fix and handle the micro sample piece that is extracted when processing into a sample for (hereinafter, TEM).

[0002]

2. Description of the Related Art A conventional micro-sample piece is formed by cleaving from a silicon wafer or using a dicing saw as the electron-microscope observation sample support member when the micro-sample piece is fixed to the electron microscope observation sample support member. The micro sample piece was fixed to one end of the silicon piece.

As a well-known example, as described in JP-A-11-108813, only a sample piece including a desired specific region is extracted from a bulk sample and a 1 mm × 2.5 mm × 0.1 mm knife-edged silicon is obtained. There is a sample preparation method and a sample preparation method in which a (Si) piece is fixed using a deposition film formed by FIB irradiation, and is fixed to a sample stage of an analyzer.

[0004]

However, in the above prior art, when the sample piece is fixed to the sample fixing portion and the sample piece is fixed and then removed from the analyzer and observed again, the sample piece portion is There is a risk of damaging the sample because it has a shape that allows easy contact.

In addition, when the sample support member formed by using a cleavage or a dicing saw has irregularities, there is a problem that the micro sample piece cannot be fixed securely.

An object of the present invention is to remove a finer sample piece from a sample by FIB processing and process it into a TEM sample.
It is an object of the present invention to provide an electron microscope observation sample support member that can easily fix and safely handle the extracted micro sample piece.

[0007]

The object of the present invention is to make the thickness of the micro sample piece fixing portion of the sample support member for electron microscope observation equal to or greater than the thickness of the micro sample piece, and to mount the micro sample pieces on both ends of the sample support member on the sample fixing side. This is achieved by providing a projection having a thickness and a height.

Further, in the sample support member for electron microscopic observation, the unevenness of a portion of the sample support member for fixing the sample piece is set to 5 μm or less.

[0009]

FIG. 1 is a perspective view of a sample supporting member 1 for an electron microscope according to an embodiment of the present invention.

[0010] A micro sample piece 2 is fixed to a sample support member 1 for an electron microscope by a deposition film 3. Both ends of the sample support member 1 are thicker than the portion where the sample piece 2 is fixed, and have a shape protruding larger than the fixed sample piece 2. The fixing portion 4 of the sample piece 2 has a surface irregularity of 5 μm.
It is as follows. When fixing the sample piece 2 to the fixing part 4,
Scan FIB while flowing out deposition gas,
The deposition film 3 is formed in the FIB irradiation area, and the sample piece 2 is fixed. The fixing film 4 can easily form the deposition film 3 in the FIB irradiation area without the deposition gas being blocked by the unevenness of the fixing member 4. Further, since the fixing portion 4 is flat, the bottom of the sample piece 2 is in close contact with the fixing portion 4 and can be fixed securely by the deposition film 3. Since the unevenness of the surface is 5 μm or less, the deposition film 3 can be formed on the side surface of the sample piece 2 when there is a gap between the sample piece 2 and the fixing portion 4. Therefore, the sample piece 2 can be reliably fixed to the fixing portion 4 by filling the gap.

FIG. 2 shows the shape and general size of a sample piece 2 which has been processed into a wedge shape by the FIB and extracted. The sample piece 2 needs to be processed into a wedge shape in order to extract it from the bulk sample, but the bottom of the sample piece 2 is processed so as to be horizontal with respect to the fixed part 4 during the inclined groove processing step. It has a shape that can be fixed securely. Although the size does not depend on this, in order to reduce the processing time of the thin film processing step for observation with the extraction processing step and the transmission electron microscope, as long as the area where the observation of the target portion can be sufficiently observed with the electron microscope remains, Make it as small as possible.

FIG. 3A shows a conventional sample supporting member 5 in FIG.
FIG. 2B shows the sample supporting member 1 in which the sample piece 2 of the present invention is fixed to the fixing portion 4. FIG. 3A shows that the sample piece 2 is exposed and easily damaged when the sample support member 5 is handled. In FIG. 3B, the sample support member 1 is provided with a protruding portion having a thickness and height greater than that of the sample piece 2. For example, a sample support member 1 with a sample piece 2 attached to a sample holder for an electron microscope
When the sample support member 1 is dropped or hit when attaching or removing the sample piece, the sample piece 2 is held in a state where it is not damaged.

FIG. 4 is a perspective view of a sample support member 6 for an electron microscope according to another embodiment. Although the sample piece 2 is fixed to the fixing part 4, it is difficult to visually confirm the sample piece 2 because the sample piece 2 is minute, and if the fixing part 4 is pinched with the tweezers 7, the sample piece 2 may be damaged. Protrusions were provided at one end of the support member 6 to facilitate handling with the tweezers 7. Further, a groove 8 was provided in the protrusion, so that the sample supporting member 6 could be securely held by the tweezers 7. In FIG. 4, the projection of the sample support member 6 has only one end, but when the sample support member 6 is inserted into the FIB processing observation device, the sample piece 2 is attached to the fixing portion 4 depending on the direction in which the sample support member is inserted. This is because the deposition gas during fixing may be blocked.
The protrusion and the groove 8 may be provided at both ends.

[0014]

By using the sample supporting member for an electron microscope according to the present invention, the sample piece can be protected from impact and the like, and handling becomes easy.

[Brief description of the drawings]

FIG. 1 is a perspective view of a sample support member for an electron microscope according to one embodiment.

FIG. 2 is a diagram showing one embodiment of the present invention.

FIG. 3 is a diagram showing one embodiment of the present invention.

FIG. 4 is a diagram showing an embodiment of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... sample support member, 2 ... sample piece, 3 ... deposition film,
4 ... fixed part, 5 ... sample support member, 6 ... sample support member, 7
... tweezers, 8 ... grooves.

Continued on the front page (72) Inventor Norie Yaguchi 1040 Ma, Ichiki, Hitachinaka City, Ibaraki Prefecture Inside Hitachi Science Systems Co., Ltd. (72) Inventor Hidemi Koike 882 Mao, Oita, Hitachinaka City, Ibaraki Prefecture Measuring Instruments, Hitachi, Ltd. Within the group (72) Inventor Kaoru Umemura 1-280 Higashi Koigakubo, Kokubunji-shi, Tokyo Inside Central Research Laboratory, Hitachi, Ltd.

Claims (3)

[Claims] 1. A focused ion beam processing apparatus, comprising:
When a smaller sample piece is extracted and processed into a sample for transmission electron microscope, in the support member for fixing the extracted small sample piece, the thickness of the small sample piece fixing portion is equal to or greater than the thickness of the small sample piece. A sample support member for electron microscopic observation, comprising a projection having a thickness and a height equal to or greater than the minute sample piece at both ends on a fixed side. 2. The sample support member for electron microscope observation according to claim 1, wherein the unevenness of a portion of the sample support member for fixing a sample piece is 5 μm or less. . 3. The electron microscope according to claim 1, wherein at least one end on the sample fixing side has a protruding portion having a height that can be pinched with tweezers or the like. An observation sample support member.