JPH0614461B2 - Gas atmosphere sample holder for electron microscope - Google Patents

Description

TECHNICAL FIELD The present invention relates to a side entry type sample holder used in an electron microscope, and particularly to a gas atmosphere sample in an electron microscope adapted to observe a biological sample or the like under atmospheric pressure. Regarding the holder.

[Prior Art] In observing a sample with an electron microscope, it is often the case that a chemical change in the sample is observed, or a biological sample or the like is placed in various gas atmospheres for observation. As a sample holder used for such sample observation, a sample holder as shown in FIG. 4 is used. In FIG. 4, 1 is a sample holder inserted from a direction orthogonal to the electron beam optical axis Z, and 2 is a sample chamber formed in the sample holder 1. Reference numeral 3 denotes a vacuum packing arranged at the bottom of the sample chamber 2, and 4 denotes a lower mesh arranged via the vacuum packing 3, and the upper mesh 6 is arranged so as to face the lower mesh 4 with the frame body 5 interposed therebetween.
Are arranged. Reference numeral 7 is a vacuum packing, and 8 is a cap having an electron beam passage hole 8a. Reference numerals 9 and 10 denote thin films stretched so as to close the pores 4a and 6a of the mesh, and a sample 11 is placed on the thin film 9 stretched on the lower mesh 4. As shown in FIG. 5, reference numerals 12 and 13 denote a pair of gas introduction pipes arranged so as to pass through the sample holder 1, and the pipes 12 and 13 are formed by the frame 5 and are an atmospheric pressure sample chamber. It communicates with 2A.

In the apparatus configured as described above, the sample holder 1 is inserted from a direction orthogonal to the electron beam optical axis Z, and the sample 11 is supplied with a gas by, for example, a pipe 12 communicating with the atmospheric pressure sample chamber 2A. It can be placed underneath for observation.

[Problems to be Solved by the Invention] In the sample holder thus configured, when the atmospheric pressure sample chamber 2A is formed in the sample holder 1 to set the sample, first, the lower mesh 4 and the thin film 9 are arranged. After that, the sample 11 is placed on the thin film 9, and then the frame 5, the upper mesh 6, the vacuum packing 7, and the cap 8 are attached in this order to set the sample. Therefore, in the case of a biological sample or the like that is observed in a wet state, it takes a relatively long time to set the sample, so that the sample dries and an accurate electron beam image cannot be obtained. Further, even if an electric signal from the sample is to be taken out, there is a drawback that the electric signal from the sample cannot be taken out because the structure is not such.

The present invention has been made in view of the above points, and has a structure in which a sample can be set from any of the upper and lower directions, and shortens the time required for setting the sample to obtain an accurate electron beam of a wet sample such as a biological sample. It is an object of the present invention to provide a device capable of obtaining an image and taking out an electric signal from a sample.

[Means for Solving the Problems] In order to achieve the above object, the present invention has an electron microscope which has a sample chamber holding a sample at its tip and is inserted from a direction orthogonal to the electron beam optical axis. In the sample holder, the block for the sample chamber, which is attached to the tip of the sample holder and which forms the sample chamber, has a hole for the sample chamber, and the electron beam passage hole which is arranged so as to face the hole for the sample chamber. Having the upper and lower caps, and the upper and lower meshes arranged on the opposing surfaces of the upper and lower caps with a frame interposed therebetween, and on the opposing surfaces of both meshes so as to close the pores of the upper and lower meshes. A thin film to be arranged and an atmospheric pressure sample chamber formed by the frame between the both caps are provided, and means for introducing gas into the atmospheric pressure sample chamber from the atmosphere side is provided. .

[Embodiment] An embodiment of the present invention will be described in detail below with reference to the accompanying drawings.

1 and 2 are cross-sectional views of an embodiment of the present invention,
FIG. 1 is a vertical cross-sectional view from the direction in which the sample holder is inserted, and FIG. 2 is a horizontal cross-sectional view from the electron beam optical axis direction. In FIGS. 1 and 2, 20 is a sample holder, and 21 is a screw 22a, 22b, 22 at the tip of the sample holder 20.
It is the block for the sample chamber attached by c and 22d. The sample chamber block 21 is provided with a sample chamber hole 21a for forming an atmospheric pressure sample chamber described later,
Four gas holes 21b, 21c, 21d for supplying and discharging the gas communicating with the hole 21a are provided in the hole 21a.
21e (holes 21c and 21e for gas are not shown) are formed, and these holes for gas are formed above the center C of the sample holder as shown by the broken line 21b in FIG.
Also, as shown in the perspective view of FIG. 3, four pipes 24, 25, 26, 27 are connected to the gas holes 21b, 21c, 21d, 21e through a vacuum seal 23, and the gas chambers for the sample chamber are connected. The block 21 and the pipe are removable. Reference numerals 28 and 29 are an upper cap and a lower cap, respectively, which are arranged so as to face the sample chamber hole 21a and have electron beam passage holes 28a and 29a. The upper cap 28
An upper mesh 31 and a lower mesh 32 are arranged on opposite surfaces of the lower cap 29 with the frame 30 interposed therebetween. Reference numerals 33 and 34 denote thin films stretched so as to close the pores 31a and 32a of the mesh. Therefore, in the sample holder thus configured, the frame body 30 forms the atmospheric pressure sample chamber 35. A sample 36 is placed on the thin film 34 stretched over the lower mesh 32a.
Reference numerals 37 and 38 are vacuum seals, and 39 and 40 are ring-shaped corners for setting the electron beam optical axis Z and the center of the sample holder 1 when the sample holder is assembled. 41 and 42 are screws for fixing the upper cap 28 and the lower cap 29 to the sample chamber block 21. Reference numeral 43 is a liquid retention pipe connected to a gas introduction pipe used when the sample is wetted with a liquid for observation.

The sample holder configured as described above is used by being inserted from the direction orthogonal to the electron beam optical axis Z, and the case of setting various samples and the like in the atmospheric pressure sample chamber will be described below. In the vertical cross-sectional view of FIG. 1, the right side of the drawing with the optical axis Z as the center, when the electric signal from the sample is extracted,
The left side of the paper shows the arrangement of each component when a wet sample is set and observed.

First, when extracting the electric signal from the sample 36,
Connect an electrode and an electric wire (not shown) to 6, and take out the electric wire through the gas introducing pipe.
This is because it is more convenient for the sample 36 to be set first. Therefore, when setting such a sample, the corner 39, the vacuum seal member 38, the lower cap 29, and the lower mesh 32 are arranged in this order, and the sample 36 is set on the thin film 34 stretched over the lower mesh 32. To do. Then, the above-mentioned electrode is attached to the sample 36, an electric wire is connected, and the electric wire is taken out through the gas introducing pipe. Next, the frame 30, the upper mesh 31, the corners 40, and the vacuum seal 37 are arranged, and finally the upper cap 28 is attached, whereby the electric signal from the sample 36 can be taken out of the sample holder.

Next, when the wet sample 36 is set in the atmospheric pressure sample chamber 35 for observation, it is necessary to observe it before the wet sample 36 is dried. Therefore, first, the liquid retention pipe 43 in which the liquid is retained is attached to the pipe 24. Then, the corner 40 ', the vacuum seal member 37, the upper cap 28, and the mesh 31 are arranged in this order. Next, the frame 30 is put in. At this time, the sample chamber block 2
The notch 30a of the frame body 30 is aligned with the gas hole No. 1 and the frame body 30 is set so that the tip of the liquid retention pipe 43 is located in the atmospheric pressure sample chamber 35. Then, the lower mesh 32 on which the sample 36 is placed, the corner 39 ', the vacuum seal 38, and the lower cap 29 are arranged. After setting the sample 36 in this way, the sample holder 20 is inserted from the lens barrel, and the atmospheric pressure sample chamber 35 is evacuated by the pipe 26 so as to have a negative pressure. The flowing liquid flows into the atmospheric pressure sample chamber 35,
The liquid can be applied to the sample 36, and the sample 36 can be made wet.

Therefore, in the sample holder configured in this way,
The shape and components of the sample holder allow the sample to be set from either the top or bottom direction, making it easier to set the sample than before and observing electrical signals from the sample while it is wet. It becomes possible to do it.

Further, the thickness of the frame body 30 forming the atmospheric pressure sample chamber 35 is selected to be, for example, 1 mm to use the atmospheric pressure sample chamber for introducing liquid, or the thickness of the frame body 30 is selected to be 0.5 mm. Used for electrical signal extraction, and the thickness of the frame 30 is 0.05m
Since it can be selected for m and used for gas introduction, it can be an atmospheric pressure sample chamber according to the purpose of observing the sample.

Further, in the conventional sample holder, two gas introduction pipes are connected to the atmospheric pressure sample chamber, but in the apparatus of this embodiment, four gas introduction pipes are provided in the atmospheric pressure sample chamber 35. Since the number of pipes has been increased by communicating with each other, it is possible to simultaneously supply a plurality of types of gas or liquid to be supplied to the atmospheric pressure sample chamber and observe the sample under these atmospheres.

Furthermore, the sample set can be performed even when the sample chamber block 21 is still attached to the sample holder 20, or the sample chamber block 2 is used.
Since the sample can be set in a state in which 1 is removed from the sample holder 20, it is possible to prepare various sample chamber blocks and to observe various samples simply by exchanging the sample chamber blocks. It is not necessary to prepare many sample holders.

[Effects of the Invention] As described in detail above, according to the present invention, the shape and configuration of the sample holder are set so that the sample can be set from any of the upper and lower directions. Provided is a gas atmosphere sample holder in an electron microscope that can be accurately observed and can extract an electric signal from a sample.

[Brief description of drawings]

1 and 2 are cross-sectional views of an embodiment of the present invention, FIG. 3 is a perspective view of an essential part of the present invention, and FIGS. 4 and 5 are cross-sectional views for explaining a conventional technique. . 20: sample holder, 21: block for sample chamber, 22a,
22b, 22c, 22d: screws, 23: vacuum seal,
24, 25, 26, 27: pipe, 28: upper cap, 29: lower cap, 30: frame body, 31: upper mesh, 32: lower mesh, 33, 34: thin film, 35:
Atmospheric pressure sample chamber, 36: sample, 37, 38: vacuum seal member, 39, 40: ring-shaped corner, 41, 42: screw,
43: Liquid retention pipe.

Claims (1)

[Claims] 1. A sample holder in an electron microscope having a sample chamber for holding a sample at its tip and inserted from a direction orthogonal to an electron beam optical axis, the sample being attached to the tip of the sample holder. A sample chamber block having holes for sample chambers forming a chamber, an upper and lower caps arranged to face the sample chamber hole and having electron beam passage holes, and a facing surface of the upper and lower caps. Formed between the upper and lower meshes with the frame body sandwiched between them, thin films arranged on the opposing surfaces of both meshes so as to close the pores of the upper and lower meshes, and the frame body. Atmospheric pressure sample chamber, and means for introducing gas into the atmospheric pressure sample chamber from the atmosphere side are provided.