WO2016047829A1 - Support de microscope électronique pour observation d'échantillons en phase gazeuse ou liquide - Google Patents

Support de microscope électronique pour observation d'échantillons en phase gazeuse ou liquide Download PDF

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Publication number
WO2016047829A1
WO2016047829A1 PCT/KR2014/009012 KR2014009012W WO2016047829A1 WO 2016047829 A1 WO2016047829 A1 WO 2016047829A1 KR 2014009012 W KR2014009012 W KR 2014009012W WO 2016047829 A1 WO2016047829 A1 WO 2016047829A1
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WO
WIPO (PCT)
Prior art keywords
grid
window film
receiving space
electron microscope
seated
Prior art date
Application number
PCT/KR2014/009012
Other languages
English (en)
Korean (ko)
Inventor
정종만
천성식
김윤중
김진규
Original Assignee
한국기초과학지원연구원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 한국기초과학지원연구원 filed Critical 한국기초과학지원연구원
Priority to PCT/KR2014/009012 priority Critical patent/WO2016047829A1/fr
Publication of WO2016047829A1 publication Critical patent/WO2016047829A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/2002—Controlling environment of sample
    • H01J2237/2003—Environmental cells
    • H01J2237/2004—Biological samples

Definitions

  • the present invention relates to an electron microscope holder equipped with a wet-cell for injecting gas or liquid into a sample so that a reaction occurring under a complex dynamic environment can be observed in real time in an electron microscope requiring high vacuum. .
  • the electron microscope sample holder equipped with a special device called a wet-cell is used to observe the moisture in the sample or inject gas or liquid into the sample. Should be used.
  • Japanese Patent JP 2781320 is a sample holder having a sample stand, in which a sample is embedded between a pair of sheet meshes having a thin film sealing material, and a sample paper placed on the sample stand and a mesh paper for pressing the sample mesh from above .
  • a sample holder comprising a sealing member for sealing between a strip and a sheet mesh periphery-sample stage, a sheet mesh-mesh support, and a sample stand-mesh support is disclosed.
  • U.S. Patent No. 7807979 is a sample kit in which a pair of substrates having a thin portion of an electron beam passing through (observation window) are disposed to face each other, and a sample is embedded therein by interposing a gap material and a sealing material in the periphery therebetween. (cell) is disclosed (FIGS. 3 and 4).
  • a sample set can be produced quickly and easily by using a simple material for observing the TEM, and a sample containing moisture can be observed in the TEM, but a change in the sample due to the injection of gas or liquid cannot be observed. .
  • US Patent Publication US 2013/0264476 proposes an observation cell in which a gas or a liquid can flow while having a cell structure as shown in US Pat. No. 7,077,979 (Fig. 6).
  • Such a device allows electron microscope to observe the change of a sample while supplying gas or liquid, but it is not universal because it requires a substrate having a special structure having a viewing window and a holder having a corresponding structure. Although not shown, considerable skill is required to set up the cell and mount it in the holder because it must allow gas or liquid to flow while maintaining the space between the substrates.
  • a silicon O-ring is used for sealing, and grooves are formed in the corresponding portions, and in case of repeated use, fine silicon particles that are dropped may affect the sample, and fine impurities may be caught in the O-ring grooves. There is a lot of room for care.
  • the present invention uses a material required for normal electron microscope observation and has a very simple structure, so that a sample set-up and maintenance is easy to configure a wet-cell to maintain a liquid state or a gaseous state or a gas or a liquid state. To provide an electron microscope holder to observe the sample by flowing into the cell.
  • the present invention for achieving the above object is (A) a cylindrical accommodating space in which the step is formed so that the following cell is inserted into the tip portion in one direction; Electron microscope holder tip including an inlet and outlet formed toward the receiving space: (B) 1 the diameter corresponding to the receiving space is seated on the stepped, a predetermined number of beam through holes formed in the center Lower grid ; A lower window film seated on the upper surface of the lower grid to cover all of the through holes; 3 The outer diameter corresponds to the receiving space, the hollow portion is formed so that the through hole of the lower grid is exposed, the through passage corresponding to the inflow passage and the outlet passage is formed on the side, it is seated on the outer periphery of the lower grid Spacer ; 4 an upper window film seated on the lower surface of the upper grid to cover all of the through holes; 5 and a diameter corresponding to the receiving space, the upper grid, which is formed through-holes corresponding to the through hole of the lower grid, at the center; A: wet-cell containing;
  • the present invention it is possible to observe not only the state containing the gas or liquid but also the change state of the sample due to the change of the input of the gas or the liquid with an electron microscope, so that the bio, chemical, medicine, In the field of materials, research and development can be made from a new perspective.
  • 1 to 6 is a view showing the structure of a wet-cell holder according to the prior art.
  • FIG. 7 is a conceptual perspective view of the end portion of a wet-cell holder for an electron microscope according to the present invention.
  • FIG. 8 is a conceptual partial cross-sectional perspective view showing a receiving space area in the wet-cell holder for electron microscope according to the present invention.
  • FIG. 9 is a conceptual partial cross-sectional exploded perspective view showing a receiving space area in the wet-cell holder for electron microscope according to the present invention.
  • FIG. 10 is a conceptual vertical cross-sectional view of a receiving space region in a wet-cell holder for an electron microscope according to the present invention.
  • the present invention relates to an electron microscope holder for including a holder tip 10 and a wet-cell 20 to observe a sample in a gas phase or a liquid phase.
  • 7 is a conceptual perspective view of an electron microscope holder end portion according to the present invention.
  • a conceptual partial cross-sectional perspective view showing an area of the accommodation space 11 in FIG. 8 a conceptual partial cross-sectional exploded perspective view showing an area of the accommodation space 11 in FIG. 9, and a conceptual vertical cross-sectional view of an area of the accommodation space 11 in FIG. 10, respectively. Shown.
  • the holder tip 10 is a part for introducing gas or liquid into the wet-cell 20 while the wet-cell 20 is hermetically sealed, and the tip of the wet-cell 20 at the tip portion thereof.
  • a cylindrical accommodating space 11 having a stepped portion 12 formed therein so that the component part is inserted and mounted in one direction, and an inflow path and an outflow path for inflow and outflow of gas or liquid formed toward the accommodating space 11.
  • the inflow path and the outflow path are preferably formed horizontally in the center of the holder tip 10 when viewed in a vertical section, and are in communication with a predetermined connection pipe, a pump and a storage tank. In the drawings, the inlet and outlet, the connection pipe, the pump and the storage tank are not shown.
  • the wet-cell 20 is in the order to be accommodated in the receiving space 11, the lower grid 21, the lower window film 22, the spacer 23, the upper window film 24, the upper grid 25 and a fixed cap 26 are included.
  • the lower grid 21 has a diameter corresponding to the accommodation space 11 and is seated on the step 12, and a predetermined number of beam passing through holes 21a are formed in the center thereof.
  • the material of the lower grid 21 may be a conductive and nonmagnetic material such as copper, gold, nickel, aluminum, molybdenum, titanium, berliumlium, carbon, or a mixture or alloy thereof. It is preferable that it is a copper material normally used by an electron microscope. Such a material may be used as a material of other components except for the lower window film 22 and the upper window film 24.
  • the diameter of the lower grid 21 is generally about 3.0 mm and the thickness is about 50 ⁇ m (see http://www.tedpella.com/grids_html/Pelco-TEM-Grids.htm ).
  • the number of the through holes 21a of the lower grid 21 is not limited, but is formed in the center, which is an area through which the electron beam can pass.
  • the diameter of the through hole 21a should be small enough that the lower window film 22 does not suck out by the vacuum pressure, and should be large enough not to affect the straightness of the electron beam, but preferably around 100 ⁇ m.
  • the lower window film 22 While the lower window film 22 is in contact with the lower grid 21 and passes through the electron beam and prevents leakage of air or moisture in the wet-cell 20, the lower window film 22 is in contact with the lower grid 21. It serves to settle (attach) the sample on the opposite surface (ie, the upper surface).
  • the lower window film 22 various kinds of synthetic resin films that do not affect the straightness of the electron beam may be applied.
  • the lower window film 22 is preferably a carbon film. There is no big restriction
  • the lower window film 22 covers all of the through holes 21a but is not sized in contact with the spacer 23
  • the bottom window film 22 is larger than the bottom of the spacer 23. Even if it comes in contact with, it is obvious.
  • the wet-cell 20 according to the present invention When the wet-cell 20 according to the present invention is mounted and observed on the holder tip 10, a strong adhesion force naturally occurs on the lower grid 21 and the lower window film 22 because the outside (electron microscope barrel) is a vacuum. do. Therefore, in the present invention, the lower grid 21 and the lower window film 22 need not be adhered to each other by an adhesive or the like, but only enough to be in close contact with each other so as not to be separated during the assembly process.
  • the spacer 23 is interposed on the outer periphery between the lower grid 21 and the upper grid 25 to be mounted oppositely to maintain a gap between the lower grid 21 and the upper grid 25. While serving to seal the inside and at the same time serves to communicate the inlet and outlet of the holder tip 10 and the inside of the wet-cell (20). That is, the spacer 23 has an outer diameter corresponding to the accommodating space 11, and a hollow part is formed to expose the through hole 21a of the lower grid 21. Through passages (23a) is formed, it is seated on the outer periphery of the lower grid (21). The through passage may be formed in a size corresponding to a position corresponding to the inflow passage and the outflow passage.
  • the accommodation space 11 and the spacer 23 may be easily matched with the inflow passage, the outflow passage and the through passage. It is preferable to form predetermined positioning means (not shown) in between.
  • the through passage may be formed on the side of the spacer 23 so that the through passage and the inflow passage and the outflow passage may be in contact with each other, or three or more passage passages may be provided so that any passage may communicate with the inflow passage and the outflow passage. It is also good. In FIG. 10, six through paths are illustrated.
  • the thickness of the spacer 23 eventually determines the distance between the lower grid 21 and the upper grid 25 (the height of the space in which the sample is seated).
  • the thickness of the spacer 23 is about 50 to 500 ⁇ m. It is good to be.
  • the material of the spacer 23 may be a metal, such as the material of the lower grid 21, or may be a synthetic resin having appropriate strength.
  • the upper window film 24 is mounted on the lower surface of the upper grid 25 so as to cover all the through holes 25a, and the upper grid 25 has a diameter corresponding to the receiving space 11, and the center portion of the upper window 25 is The through hole 25a corresponding to the through hole 21a of the lower grid 21 is formed.
  • the size, material, and characteristics thereof are the same as those of the lower window film 22 and the lower grid 21 described above. May be the same.
  • the lower grid 21 and the upper grid 25 have the lower window film 22 and the upper window film 24 attached to the inner surface thereof, respectively, and the through holes 21a and 25a are vertically attached.
  • the electron beams are opposed to each other so as to pass through holes 21a and 25a formed in the lower grid 21 and the upper grid 25. Since the components according to the present invention have a very fine size (the lower grid 21 and the upper grid 25 are about 3 mm), the through holes 21a, when the lower grid 21 and the upper grid 25 are opposed to each other, are formed. It may not be easy to vertically match 25a).
  • a predetermined position (direction) determining means (not shown) in contact with the lower grid 21, the spacer 23, the upper grid 25 and the receiving space (11).
  • a portion of the outer circumference of the lower grid 21, the spacer 23, and the upper grid 25 may be a straight line, or a groove is formed on the outer circumference, and a portion of the accommodating space 11 corresponding thereto is a straight line.
  • the fixing cap 26 serves to press and fix the lower grid 21, the spacer 23, and the upper grid 25 seated in order, and the diameter of the accommodation space ( 11) and has a hollow portion in which a hollow part is formed to expose the through hole 25a of the upper grid 25.
  • the outer periphery of the fixing cap 26 and the receiving space 11 corresponding thereto have a screw structure (not shown) corresponding to each other, so that the screw can be fixed in a screwing manner.
  • the second step 12a is formed in the portion corresponding to the upper grid 25 of the accommodation space 11, Side of the upper grid 25 may be a structure corresponding to the second step (12a).
  • the upper grid 25 is pressed down by the fixing cap 26 and is strongly adhered to the receiving space 11 at the second step 12a so that there is no fear of leakage of gas or liquid therein.
  • Electron microscope wet-cell holder 20 according to the present invention made of the above components, for example, can be assembled in a state where the sample is seated through the following process.
  • the lower window film 22 or the upper window film 24 is floated on a liquid such as distilled water, and (B) the lower grid 21 or the upper grid 25 is held with a forceps or the like.
  • the lower window film 22 or the upper window film 24 is lifted up from the bottom of the lower window 21 or the upper window 25 on the lower window film 22 or the upper window film 24, through-holes It is settled and dried so that all (21a, 25a) may be covered.
  • the lower window film 22 having the lower window film 22 seated on the upper surface is inserted into the receiving space 11 of the holder tip 10 and seated on the step 12.
  • FIGS. 8 and 9 A partial cross-sectional perspective view of the assembled state is illustrated in FIGS. 8 and 9 (sample not shown).
  • loading the sample on the surface of the lower window film 22 before or after the step (C); may be further added.
  • the holder for the electron microscope wet-cell 20 according to the present invention thus assembled is used to observe the change over time of the sample while being inserted into the barrel of the electron microscope and applying a predetermined gas or liquid.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

La présente invention concerne un support de microscope électronique équipé d'un micro-dispositif (cellule humide), destiné à permettre à un microscope électronique, nécessitant un vide poussé, d'observer, en temps réel, une réaction ayant lieu dans un environnement dynamique complexe, en injectant un gaz ou un liquide dans un échantillon. Selon la présente invention, un échantillon contenant de l'humidité, tel qu'un organisme ou un minéral, peut être observé de manière simple et économique dans l'état naturel où il se trouve, une atmosphère d'air ou une atmosphère d'eau étant maintenue, par l'intermédiaire du microscope électronique.
PCT/KR2014/009012 2014-09-26 2014-09-26 Support de microscope électronique pour observation d'échantillons en phase gazeuse ou liquide WO2016047829A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/KR2014/009012 WO2016047829A1 (fr) 2014-09-26 2014-09-26 Support de microscope électronique pour observation d'échantillons en phase gazeuse ou liquide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2014/009012 WO2016047829A1 (fr) 2014-09-26 2014-09-26 Support de microscope électronique pour observation d'échantillons en phase gazeuse ou liquide

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WO2016047829A1 true WO2016047829A1 (fr) 2016-03-31

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876234A (zh) * 2017-04-17 2017-06-20 南京大学 一种用于矿物相自动识别分析的样品台
WO2019010390A1 (fr) * 2017-07-06 2019-01-10 Protochips, Inc. Gestion de fluide de porte-échantillon de microscope électronique à commande de pression et de débit indépendante

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080179518A1 (en) * 2004-09-13 2008-07-31 Jan Fredrik Creemer Microreactor for a Transmission Electron Microscope and Heating Element and Method of Manufacture Thereof
US20110079710A1 (en) * 2007-05-09 2011-04-07 Protochips, Inc. Microscopy support structures
US20120017415A1 (en) * 2009-02-04 2012-01-26 Marsh Charles P Method of use of reusable sample holding device permitting ready loading of very small wet samples
WO2013132906A1 (fr) * 2012-03-09 2013-09-12 株式会社 日立製作所 Porte-échantillon liquide pour microscope électronique et son procédé de fabrication
US20130264476A1 (en) * 2010-08-02 2013-10-10 Protochips, Inc. Electron microscope sample holder for forming a gas or liquid cell with two semiconductor devices

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080179518A1 (en) * 2004-09-13 2008-07-31 Jan Fredrik Creemer Microreactor for a Transmission Electron Microscope and Heating Element and Method of Manufacture Thereof
US20110079710A1 (en) * 2007-05-09 2011-04-07 Protochips, Inc. Microscopy support structures
US20120017415A1 (en) * 2009-02-04 2012-01-26 Marsh Charles P Method of use of reusable sample holding device permitting ready loading of very small wet samples
US20130264476A1 (en) * 2010-08-02 2013-10-10 Protochips, Inc. Electron microscope sample holder for forming a gas or liquid cell with two semiconductor devices
WO2013132906A1 (fr) * 2012-03-09 2013-09-12 株式会社 日立製作所 Porte-échantillon liquide pour microscope électronique et son procédé de fabrication

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876234A (zh) * 2017-04-17 2017-06-20 南京大学 一种用于矿物相自动识别分析的样品台
CN106876234B (zh) * 2017-04-17 2018-06-26 南京大学 一种用于矿物相自动识别分析的样品台
WO2019010390A1 (fr) * 2017-07-06 2019-01-10 Protochips, Inc. Gestion de fluide de porte-échantillon de microscope électronique à commande de pression et de débit indépendante
US11222765B2 (en) 2017-07-06 2022-01-11 Protochips, Inc. Electron microscope sample holder fluid handling with independent pressure and flow control
US11869744B2 (en) 2017-07-06 2024-01-09 Protochips, Inc. Electron microscope sample holder fluid handling with independent pressure and flow control

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