KR20170050250A - Specimen Multi-loading Device for Grid of TEM - Google Patents

Specimen Multi-loading Device for Grid of TEM Download PDF

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Publication number
KR20170050250A
KR20170050250A KR1020150151571A KR20150151571A KR20170050250A KR 20170050250 A KR20170050250 A KR 20170050250A KR 1020150151571 A KR1020150151571 A KR 1020150151571A KR 20150151571 A KR20150151571 A KR 20150151571A KR 20170050250 A KR20170050250 A KR 20170050250A
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South Korea
Prior art keywords
grid
sample
tem
loading
opening
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KR1020150151571A
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Korean (ko)
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KR101748824B1 (en
Inventor
권용은
김정균
정종만
김윤중
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한국기초과학지원연구원
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2204—Specimen supports therefor; Sample conveying means therefore
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/079—Investigating materials by wave or particle radiation secondary emission incident electron beam and measuring excited X-rays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/309—Accessories, mechanical or electrical features support of sample holder
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/40—Imaging
    • G01N2223/418—Imaging electron microscope

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention relates to a multi-specimen loading device for a grid for a transmission electron microscope (TEM) enabling a plurality of specimens to be observed by setting TEM equipment once by loading the plurality of specimens on a single grid when observing the specimens with the TEM and, more specifically, relates to a multi-specimen loading device for a grid for a transmission electron microscope comprising: (A) a base unit; (B) a rotary unit mounted on the base unit to be able to rotate, having a grid seating hole in a rotary shaft, and automatically or manually rotated; (C) a partial blocking unit mounted on the rotary unit to be separated to be spaced from a top surface of the grip when the grid is seated in the grid seating hole having an opening to pass specimen fume in a part corresponding to a specimen loading area, except for a center of the grip (might be in contact with the center) when the grid is seated in the grid seating hole.

Description

(Specimen Multi-loading Device for Grid of TEM for TEM Grid)

The present invention relates to a sample loading apparatus that allows a plurality of samples to be observed by setting one TEM apparatus by loading a plurality of samples on one grid when the sample is observed with a TEM.

Conventionally, in order to observe a sample with a TEM, the following sample preparation process and sample observation process are performed.

① Sample preparation process (process of loading sample on grid)

First, the sample is well dispersed in a dispersion medium (for example, alcohol) and allowed to stand or centrifuge to precipitate large particles. Then, the sample is loaded into the grid by grasping the grid with a predetermined tweezer, immersing it in the upper layer of the dispersion medium, and taking it out. The dispersion medium is dried naturally or is removed by filter paper and dried.

② Sample Observation Process (The process of observing and loading a sample loaded grid on TEM)

The prepared sample grid (sample-loaded grid) was attached to a TEM holder according to a conventional method, and the holder was placed in a column (column) of a TEM through an air lock, the column was evacuated and the holder was moved to the sample stage .

However, in the sample observation process, only one sample grid can be observed at one time, and it takes a long time to complete the observation after the holder is inserted into the column, and then prepare for the next sample grid mounting. It takes a considerable amount of time to observe all the samples.

Patent No. 10-1214985 filed by the inventors of the present invention has a support portion 10 in which n vertical fine penetration grooves 11 are uniformly formed with respect to the center a; A partitioning part (20) having a vertical blocking plate (21) formed uniformly with respect to the center (b); The vertical separator 20 is positioned at the center of the support 10 so that the vertical micro through grooves 11 and the vertical shutoff plate 21 are aligned with the centers a and b, And a vertically moving means (30) for vertically shifting the vertical axis with respect to one vertical axis (see Figs. 1a and 1b). However, according to this, there is a disadvantage that the sample liquid is moved to the neighboring region (compartment) by the capillary phenomenon through the contact surface of the grid G and the vertical blocking plate 21 indicated by the red line in FIG. .

In order to solve such a problem, the inventors of the present invention have proposed (A) a method of manufacturing a semiconductor device, comprising: (A) Horizontally mounting a mask having one or a plurality of openings therein; (B) horizontally mounting the ultrasonic vibrator at a predetermined height above the mask opening so that the mist plate faces downward; (C) loading a sample liquid on the upper surface of the ultrasonic vibrator and operating the ultrasonic vibrator; (D) replacing or washing the ultrasonic vibrator and the mask in another region not overlapping one region of the grid, and repeating the steps (A) to (C) with another sample liquid A method of loading a plurality of samples onto a grid for observation of the TEM and a sample loading apparatus therefor are disclosed (see Figs. 1C and 1D). However, according to the above-described technique, the concept of loading the sample on the grid by the sample mist by ultrasonic vibration has been proposed. However, since a plurality of samples are loaded depending on the operator's sense, very care has to be taken so that the samples are not cross- .

Patent No. 10-1214985 Patent Document 10-2015-0054428

An object of the present invention is to provide a sample loading apparatus which can accurately observe a plurality of samples in a short period of time by loading a plurality of samples on one grid without cross contamination by mounting the sample grid once.

According to an aspect of the present invention, there is provided a semiconductor device comprising: (A) a base portion; (B) an automatic or manually rotating rotating part rotatably mounted on the base part and having a grid in-hole formed on the rotating shaft; (C) is detachably mounted on the rotary part so as to be spaced apart from the upper surface of the grid when the grid is seated in the grid, and wherein when the grid is seated in the grid, the grid does not include the center of the grid And a part blocking part having an opening hole for passing the sample mist through the part corresponding to the part in the sample loading area. The present invention relates to a sample multi-loading mechanism for a TEM grid.

As described above, according to the present invention, loading of the sample liquid by spraying, loading of the sample liquid at a fixed position and range, and loading of the sample liquid are prevented, 6) of different samples can be accurately observed by TEM.

FIGS. 1A and 1B are conceptual diagrams showing a grid sample multi-loading auxiliary mechanism according to the prior art;
1C and 1D are conceptual diagrams showing an example of a grid sample loading method according to still another prior art, and a photograph of a sample loading device for this purpose.
Figures 2a and 2b are an external perspective view and a partially enlarged perspective view of the device according to the invention.
3 is an enlarged view of the rear surface of the blocking plate in the device according to the present invention.
FIG. 4 is a photograph of a production example of a sample loading device according to the present invention. FIG.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail with reference to the accompanying drawings. It should be understood, however, that the appended drawings illustrate only the contents and scope of technology of the present invention, and the technical scope of the present invention is not limited thereto. It will be apparent to those skilled in the art that various changes and modifications can be made within the scope of the technical idea of the present invention based on these examples.

In order to accomplish the above object, the present invention relates to a sample multi-loading mechanism for a grid for TEM comprising a base portion (10), a rotating portion (20) and a partial blocking portion (30). FIGS. 2A and 2B are an external perspective view and a partially enlarged perspective view of the device according to the present invention, FIG. 3 is an enlarged view of the back surface of the blocking plate in the device according to the present invention and FIG. 4 is a photograph showing the sample loading device according to the present invention Respectively. The following description will be made with reference to the drawings.

In the present invention, the base portion 10 serves as a support on which other components are seated. At least a portion corresponding to the grid or the open hole 31 may be opened in the base portion 10 so that excessive sample mist can be easily discharged to the outside.

In the present invention, the rotary part 20 is rotatably mounted on the base part 10, and a grid inner hole 21 is formed on the rotation axis, so that a grid ultimately seated on the inner grid hole 21 It can rotate automatically or manually. The rotary part 20 has a grid inner hole 21 on which a grid to be loaded is placed, and serves to rotate the grid mounted on the inner grid hole 21. The grid in-hole may be actually 'open' or may be a groove in which the grid can be seated. At this time, the rotation unit may rotate the 'grid only' without rotating, or may rotate the grid with itself. The rotation of the grid or the rotary part may be automatically performed by a predetermined driving part and a control part, or manually by a worker. The drawings illustrate by manual.

In the present invention, the partial cut-off portion 30 is detachably mounted on the rotary portion 20 so as to be spaced apart from the upper surface of the grid by an appropriate distance when the grid is seated in the grid in-hole 21, 21, there is formed an opening hole 31 for passage of the sample mist in a portion corresponding to the site in the sample loading region which does not include (can touch) the center of the grid when the grid is seated. The blocking portion functions so that the sample mist can be loaded only on a limited portion of the sample loading area of the grid. The open hole 31 should not include the center of the grid, otherwise cross contamination of the sample mist will occur at the center of the grid. The apparatus illustrated in the drawing is made to have an arc shape in which the open hole 31 is 1/4 of the grid.

The sample multi-loading mechanism according to the present invention can be used, for example, in the following manner. First, the partial cut-off portion 30 is opened in the mechanism and the empty grid is placed on the grid in-hole 21 of the rotary portion 20. [ And then covers the partial blocking portion 30 on the grid. In this state, for example, the grid is opened up to 1/4 of the open space 31 of the partial cut-off portion 30 (assuming that it is an arc shape which is 1/4 of the grid). The experimenter puts the sample liquid into a mist state by a predetermined method (for example, using the ultrasonic vibrator described below) and injects a small amount onto the opening hole 31. [ Then, the sample mist is raised to the open 1/4 size grid area. Then, the experimenter automatically or manually rotates the rotary part 20 by 1/4 to newly open 1/4 of the grid and raise new sample mist. After four sample fogs are put on the grid, the partial cutoff portion 30 is opened and a grid on which different samples are placed in the 1/4 region is taken out and observed with an electron microscope through a normal method. Therefore, it is possible to observe four kinds of samples by attaching the grid once to the electron microscope.

In the present invention, it is preferable that a diffusion preventing tuck 32 for preventing the diffusion of the sample mist is formed on the entire outer periphery of the lower outer periphery of the opening portion 31 of the partial blocking portion 30. 3 is an enlarged view of the lower portion of the partial cut-off portion 30. As shown in Fig.

It is preferable to load each sample at a predetermined interval on the grid when using the sample loading mechanism according to the present invention. For this purpose, the open hole 31 is sized to be included or inscribed in an arc which is uniformly radially divided into n (n > = 2) with respect to the center of the grid, It is preferable to rotate by 1 / n. At this time, it is preferable that 2? N? 6, and n = 4 in the example produced by way of example.

When the sample multi-loading mechanism according to the present invention is used, the constituent elements and the grid are sequentially stacked, the sample mist is loaded, and the rotating unit 20 is rotated. In this process, the stacked components may be shaken. In order to prevent this, it is preferable to add a fixing portion 40 for fixing the base portion 10, the rotating portion 20 and the partial blocking portion 30 which are stacked and mounted.

The sample multi-loading mechanism according to the present invention intends to load the sample liquid into the grid in a mist state. Therefore, it is better to integrate the parts to make the sample liquid to be fogged. For example, the sample multi-loading mechanism according to the present invention may further include an ultrasonic transducer 50 horizontally mounted on the upper portion of the opening 31 of the partial cut-off portion 30 (see FIG. 4). At this time, the ultrasonic transducer 50 is preferably fixed to the upper and lower coaxial axes so that the height of the ultrasonic transducer 50 can be appropriately adjusted (see FIG. 4).

10. Base portion
20. Rotation part
21. Grid construction
30. Partial cut-
31. Opening Ball 32. Diffusion Bottom
40. Higher government
50. Ultrasonic vibrator

Claims (7)

(A) a base portion;
(B) an automatic or manually rotating rotating part rotatably mounted on the base part and having a grid in-hole formed on the rotating shaft;
(C) is detachably mounted on the rotating portion so as to be spaced apart from the upper surface of the grid when the grid is seated in the grid opening,
A part blocking part formed with an opening hole for passing the sample mist through a part corresponding to a part of the sample loading area not containing (touching) the center of the grid when the grid is seated in the grid opening,
A sample multi-loading mechanism for a grid for TEM.
The method according to claim 1,
And a diffusion barrier for preventing spread of the sample mist is formed on the entirety or a part of the outer periphery of the open lower end of the partial shielding portion.
The method according to claim 1,
The open hole is sized to be included or inscribed in an arc that is uniformly radially spaced from the center of the grid by n (where n > = 2)
Wherein the rotation unit is rotated at a rate of 1 / n per one click.
The method of claim 3,
2 ≤ n ≤ 6.
5. The method of claim 4,
and n is 4. 4. A sample multi-loading mechanism for a TEM grid.
The method according to claim 1,
Further comprising a fixing portion for fixing the base portion, the rotating portion, and the partial blocking portion, which are stacked and attached, to the TEM multi-loading mechanism.
The method according to claim 1,
Further comprising an ultrasonic vibrator horizontally mounted on the upper portion of the partial cut-off portion opening.
KR1020150151571A 2015-10-30 2015-10-30 Specimen Multi-loading Device for Grid of TEM KR101748824B1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109444195A (en) * 2018-12-27 2019-03-08 中建材蚌埠玻璃工业设计研究院有限公司 A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder
CN113192816A (en) * 2021-04-26 2021-07-30 中国科学院物理研究所 Electron microscope carrier net, preparation method thereof and microscope product
CN113484545A (en) * 2021-07-19 2021-10-08 中科合成油技术有限公司 Transmission electron microscope multi-sample grid, matched sample preparation table thereof, preparation method and use method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101214985B1 (en) * 2011-11-21 2012-12-24 한국기초과학지원연구원 Aids for sample loading on grid for observing tem

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109444195A (en) * 2018-12-27 2019-03-08 中建材蚌埠玻璃工业设计研究院有限公司 A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder
CN113192816A (en) * 2021-04-26 2021-07-30 中国科学院物理研究所 Electron microscope carrier net, preparation method thereof and microscope product
CN113192816B (en) * 2021-04-26 2023-11-17 中国科学院物理研究所 Electron microscope carrier net, preparation method thereof and microscope product
CN113484545A (en) * 2021-07-19 2021-10-08 中科合成油技术有限公司 Transmission electron microscope multi-sample grid, matched sample preparation table thereof, preparation method and use method

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