WO2016047829A1 - Electron microscope holder for sample observation in gas or liquid phase - Google Patents

Electron microscope holder for sample observation in gas or liquid phase Download PDF

Info

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
Authority
WO
WIPO (PCT)
Prior art keywords
grid
window film
receiving space
electron microscope
seated
Prior art date
Application number
PCT/KR2014/009012
Other languages
French (fr)
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/en
Publication of WO2016047829A1 publication Critical patent/WO2016047829A1/en

Links

Images

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.

Landscapes

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

Abstract

The present invention relates to an electron microscope holder equipped with a micro-device (a wet cell), for allowing an electron microscope, requiring high vacuum, to observe, in real time, a reaction occurring under a complex dynamic environment, by injecting a gas or liquid into a sample. According to the present invention, a sample containing moisture, such as an organism or mineral, can be simply and economically observed in the natural state as it is, in which an air atmosphere or water atmosphere is maintained, through the electron microscope.

Description

기상 또는 액상에서의 시료관찰을 위한 전자현미경 홀더Electron microscope holder for sample observation in gas phase or liquid phase
본 발명은 시료에 가스나 액체를 주입하여 복합적인 동적환경 아래에서 일어나는 반응을 고진공을 요구하는 전자현미경에서 실시간으로 관찰할 수 있도록 하는 미세장치(wet-cell)가 장착된 전자현미경 홀더에 관한 것이다.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. .
전자현미경에 의한 시료의 관찰은 고진공 상태에서 이루어진다. 따라서 전자현미경 내부에 장착되는 시료는 고진공 분위기에 노출되기 때문에 시료 중에 수분이 있거나, 시료에 가스나 액체를 주입하면서 관찰하기 위해서는 소위 wet-cell이라는 특수한 구조의 미세장치를 장착한 전자현미경 시료홀더를 이용해야 한다.Observation of the sample by electron microscope is performed under high vacuum. Therefore, because the sample mounted inside the electron microscope is exposed to high vacuum atmosphere, 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.
일본등록특허 JP 2781320에는, 시료대를 가지는 시료홀더로서, 박막 밀봉재가 붙어있는 한 쌍의 시트 메쉬 사이에 시료를 내장하고 있고 상기 시료대에 올려지는 시료메쉬, 상기 시료메쉬를 위에서 눌러주는 메쉬지지구 및 시트메쉬주변부-시료대, 시트메쉬-메쉬지지구 및 시료대-메쉬 지지구 사이를 밀봉하는 밀봉부재로 이루어진 시료홀더를 개시하고 있다.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.
이러한 종래기술에 의하면 액상 또는 기상 상태를 유지할 수 있으므로 수분이 함유된 상태 그대로의 생물, 광물 등의 시료를 전자현미경으로 관찰할 수 있게 된다. 그러나 이에 의하면 ① 시트메쉬의 제작이 어렵고(종래기술 문헌 문단0009 ; 구멍의 크기가 100㎛정도의 금속성의 시트메쉬에 구멍 지름이 수㎛정도의 프로그래머블컴퓨터 그리드를 붙이고, 그 위에 폴리비닐 박막소자를 얹고 카본를 증착하여 제작) ② 시료를 홀더에 밀봉하여 장착하는 과정이 복잡하고(도 1 참조) ③ 무엇보다도 특수한 전용홀더(도 2 참조)를 사용해야 하는 어려움이 있다.According to such a prior art, it is possible to maintain a liquid state or a gaseous state, so that samples of living organisms, minerals, and the like in a state containing water can be observed with an electron microscope. However, according to this method, it is difficult to manufacture sheet mesh (Prior art document 0009; attaching a programmable computer grid having a hole diameter of several μm to a metallic sheet mesh having a hole size of about 100 μm, and placing a polyvinyl thin film device thereon. The process of mounting the sample sealed to the holder is complicated (see Fig. 1). ③ Above all, it is difficult to use a special dedicated holder (see Fig. 2).
미국특허 US 7807979는, 전자빔이 통과하는 부위(관찰창)를 얇게 제작한 기판 한쌍을 마주보게 배치하고 그 사이의 주변부에 간극재 및 밀봉재를 개재시켜 내부에 시료를 내장할 수 있도록 한 시료용키트(cell)를 개시하고 있다(도 3, 4).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).
이에 의하면 전술한 일본특허보다 편리하고 간단하게 액상 또는 기상 상태를 유지할 수 있게 된다. 그러나 관찰창을 가지는 특수한 구조의 기판이 필수적이기 때문에 범용성이 없다는 단점이 있다. This makes it possible to maintain a liquid or gaseous state more conveniently and simply than the above-described Japanese patent. However, there is a disadvantage in that it is not versatile because a special structure substrate having an observation window is essential.
본 발명의 발명자들이 발명한 국제출원(PCT/KR2013/10219, 수분을 함유하고 있는 샘플을 TEM에서 관찰할 수 있도록 TEM 홀더에 장착되는 미세장치)에는 (A) 중앙부에 소정 개수의 관통공이 형성되어 있는 하부그리드; (B) 상기 하부그리드의 관통공을 모두 덮도록 안착되고, 상면에 시료가 로딩되는 윈도우필름; (C) 상기 하부원판의 외주변에 안착되는 밀폐디스크; (D) 상기 하부원판의 관통공에 대응되는 관통공이 형성되어 있고 상기 밀폐디스크에 안착되는 상부그리드; 및 (E) 상기 하부그리드의 하면에, 관통공을 모두 덮도록 부착되는 윈도우필름;을 포함하는, 수분을 함유하고 있는 샘플을 TEM에서 관찰할 수 있도록 TEM 홀더에 장착되는 미세장치가 개시되어 있다(도 5).In the international application invented by the inventors of the present invention (PCT / KR2013 / 10219, a micro device mounted on the TEM holder to observe a sample containing water in the TEM), a predetermined number of through holes are formed in the center of (A). Lower grid; (B) a window film seated to cover all the through holes of the lower grid, the sample film is loaded on the upper surface; (C) a closed disk seated on the outer periphery of the lower disc; (D) an upper grid is formed in the through hole corresponding to the through hole of the lower disc and seated on the closed disk; And (E) a window film attached to a lower surface of the lower grid so as to cover all of the through holes, and a micro device is mounted on the TEM holder to observe a water-containing sample in the TEM. (FIG. 5).
이에 의하면 TEM 관찰시에 간단한 재료를 사용하여 간편하고 신속하게 시료세트를 제작하여 수분을 함유하고 있는 샘플을 TEM에서 관찰할 수 있지만, 가스 또는 액체의 투입에 따른 시료의 변화상을 관찰할 수는 없다.According to this, 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. .
미국특허공개 US 2013/0264476는 위의 미국특허 US 7807979가 제시한 것과 같은 cell 구조를 가지면서 가스나 액체가 유동할 수 있는 관찰용 cell을 제안하고 있다(도 6).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).
이러한 장치는 가스 또는 액체를 공급하면서 시료의 변화를 전자현미경으로 관찰할 수 있도록 하지만, 관찰창을 가지는 특수한 구조의 기판과 그에 대응되는 구조를 가지는 홀더가 필수적이기 때문에 범용성이 없으며, 명세서에 언급되거나 도시되지 않았지만, 기판 사이의 공간을 유지하면서 가스 또는 액체가 유동할 수 있도록 해야 하기 때문에 cell을 세팅하고 홀더에 장착하는데 상당한 숙련성이 요구되고 있다. 또한 밀봉을 위해 실리콘 재질의 O-링을 이용하며 그에 대응되는 부위에 홈을 형성하게 되는데, 반복 사용시에 탈락된 미세 실리콘 입자가 시료에 영향을 줄 수도 있고, O-링 홈에 미세불순물이 끼어들 여지가 있어 관리에 매우 주의해야 한다.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. In addition, 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.
본 발명은 통상의 전자현미경 관찰을 위해 필요한 재료를 이용하며 매우 단순한 구조로 되어 있어 시료 세팅이 간편하고 유지관리가 편리한 미세장치(wet-cell)를 구성하여 액상 또는 기상 상태를 유지하거나 기체 또는 액체를 cell 내로 유동시켜 시료를 관찰할 수 있도록 하는 전자현미경 홀더를 제공하고자 한다.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.
전술한 목적을 달성하기 위한 본 발명은 (A) 팁 부위에 하기 cell이 한 방향으로 삽입 장착되도록 단턱이 형성되어 있는 원통형상의 수용공간; 상기 수용공간을 향하여 형성된 유입로 및 유출로;를 포함하는 전자현미경용 홀더팁: (B) ① 직경이 상기 수용공간에 대응되어 상기 단턱에 안착되며, 중앙부에 소정 개수의 빔 통과용 관통공이 형성되어 있는 하부그리드; ② 상기 하부그리드의 상면에, 관통공을 모두 덮도록 안착되는 하부윈도우필름; ③ 외경이 상기 수용공간에 대응되고, 상기 하부그리드의 관통공이 노출되도록 중공부가 형성되어 있고, 측면에 상기 유입로 및 유출로에 대응되는 관통로가 형성되어 있으며, 상기 하부그리드의 외주변에 안착되는 스페이서; ④ 하기 상부그리드의 하면에, 관통공을 모두 덮도록 안착되는 상부윈도우필름; ⑤ 직경이 상기 수용공간에 대응되며, 중앙부에 상기 하부그리드의 관통공에 대응되는 관통공이 형성되어 있는 상부그리드; ⑥ 직경이 상기 수용공간에 대응되고, 상기 상부그리드의 관통공이 노출되도록 중공부가 형성되어 있으며, 안착된 상기 하부그리드-스페이서-상부그리드를 압박하여 고정하는 고정캡;을 포함하는 wet-cell:을 가지는 전자현미경용 wet-cell 홀더에 관한 것이다.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; fixing cap for fixing the pressure on the upper grid ⑥ a diameter corresponding to the receiving space and the and the upper grid portion a hollow so that the through-hole is exposed is formed of, wherein the lower grid rests - - spacer The branch relates to a wet-cell holder for electron microscopy.
이상과 같이 본 발명에 의하면, 수분을 함유하고 있는 생물, 광물 등의 시료를 공기 분위기 또는 물 분위기가 유지되는 자연 상태그대로, 간단하면서 경제적으로 전자현미경에서 관찰하는 것이 가능하게 된다.As described above, according to the present invention, it is possible to observe samples such as biological matters and minerals containing water in an electron microscope in a simple and economical manner in a natural state in which an air atmosphere or a water atmosphere is maintained.
또한 본 발명에 의하면 취급하기 쉬운 간단한 구조로 되어 있으면서 도 가스 또는 액체를 함유한 상태 뿐 아니라 가스 또는 액체의 투입의 변화에 따른 시료의 변화상을 전자현미경으로 관찰할 수 있게 됨으로써 바이오, 화학, 의약, 재료 등의 분야에서 새로운 관점에서의 연구개발이 이루어질 수 있게 된다.In addition, according to 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.
도 1~6은 종래기술에 의한 wet-cell 홀더의 구조를 보여주는 도면.1 to 6 is a view showing the structure of a wet-cell holder according to the prior art.
도 7은 본 발명에 의한 전자현미경용 wet-cell 홀더 말단 부분의 개념적 사시도.7 is a conceptual perspective view of the end portion of a wet-cell holder for an electron microscope according to the present invention.
도 8은 본 발명에 의한 전자현미경용 wet-cell 홀더에서 수용공간 영역을 보여주는 개념적 부분단면 사시도.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.
도 9는 본 발명에 의한 전자현미경용 wet-cell 홀더에서 수용공간 영역을 보여주는 개념적 부분단면 분해사시도.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.
도 10은 본 발명에 의한 전자현미경용 wet-cell 홀더에서 수용공간 영역의 개념적 수직단면도.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.
- 부호의 설명 -Description of the sign
10. 홀더팁10. Holder tip
11. 수용공간 12. 단턱 12a. 제2단턱11. receiving space 12. step 12a. 2nd step
20. wet-cell20. wet-cell
21. 하부그리드 21a. 관통공21. Lower grid 21a. Through hole
22. 하부윈도우필름 23. 스페이서22. Lower Window Film 23. Spacer
23a. 관통로 24. 상부윈도우필름23a. Throughway 24. Upper Window Film
25. 상부그리드 25a. 관통공25. Upper grid 25a. Through hole
26. 고정캡26. Fixed cap
이하 첨부된 도면을 참조하여 본 발명을 보다 상세히 설명한다. 그러나 첨된 도면은 본 발명의 기술적 사상의 내용과 범위를 쉽게 설명하기 위한 예시일 뿐, 이에 의해 본 발명의 기술적 범위가 한정되거나 변경되는 것은 아니다. 이러한 예시에 기초하여 본 발명의 기술적 사상의 범위 안에서 다양한 변형과 변경이 가능함은 당업자에게는 당연할 것이다. Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings. However, the accompanying drawings are only examples for easily describing the content and scope of the technical idea of the present invention, and thus the technical scope of the present invention is not limited or changed. It will be apparent to those skilled in the art that various modifications and variations are possible within the scope of the present invention based on these examples.
전술하였듯이 본 발명은 기상 또는 액상에서 시료를 관찰할 수 있도록 하는 홀더팁(10)과 wet-cell(20)을 포함하는 위한 전자현미경 홀더에 관한 것이다. 도 7에 본 발명에 의한 전자현미경 홀더 말단 부분의 개념적 사시도를 도시하였다. 도 8에 수용공간(11) 영역을 보여주는 개념적 부분단면 사시도를, 도 9에 수용공간(11) 영역을 보여주는 개념적 부분단면 분해사시도를, 도 10에 수용공간(11) 영역의 개념적 수직단면도를 각각 도시하였다.As described above, 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.
본 발명에서 상기 홀더팁(10)은 wet-cell(20)을 기밀하게 내장하면서 wet-cell(20) 내부로 가스 또는 액체를 유입시키기 위한 부분으로서, 팁 부위에 wet-cell(20)의 각 구성부가 한 방향으로 삽입 장착되도록 단턱(12)이 형성되어 있는 원통형상의 수용공간(11)과 상기 수용공간(11)을 향하여 형성된 가스 또는 액체의 유입 및 유출을 위한 유입로 및 유출로;를 가진다. 상기 유입로 및 유출로는 수직단면으로 볼 때 홀더팁(10)의 중앙에 수평으로 형성되는 것이 바람직하며, 소정의 연결관, 펌프 및 저장탱크와 연통되어 있다. 도면에서는 유입로 및 유출로, 연결관, 펌프 및 저장탱크의 도시를 생략하였다.In the present invention, 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. And 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.
본 발명에서 상기 wet-cell(20)은 상기 수용공간(11)에 수용되는 순으로, 하부그리드(21), 하부윈도우필름(22), 스페이서(23), 상부윈도우필름(24), 상부그리드(25) 및 고정캡(26)을 포함하고 있다.In the present invention, 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.
하부그리드(21)는, 직경이 상기 수용공간(11)에 대응되어 상기 단턱(12)에 안착되며, 중앙부에 소정 개수의 빔 통과용 관통공(21a)이 형성되어 있다. 하부그리드(21)의 재질로는 구리(Copper), 금(Gold), 니켈(Nickel), Aluminum, Molybdenum, Titanium, Beryllium, Carbon 또는 이들의 혼합물이나 합금처럼 전도성이며 비자성인 특성을 가진 것이면 족하며, 전자현미경에서 통상 사용되는 구리 재질인 것이 바람직하다. 이러한 재질은 하부윈도우필름(22)과 상부윈도우필름(24)을 제외한 다른 구성요소의 재질로도 이용될 수 있다. 하부그리드(21)의 직경은 통상 3.0㎜ 전후, 두께는 50㎛ 정도인 것이 바람직하다(참조 : http://www.tedpella.com/grids_html/Pelco-TEM-Grids.htm). 하부그리드(21)의 관통공(21a) 수는 제한이 없으나 전자빔이 통과할 수 있는 영역인 중앙부에 형성된다. 관통공(21a)의 직경은 진공압에 의해 내부의 하부윈도우필름(22)이 빨려나가지 않을 정도로 작고, 전자빔의 직진성에 영향을 주지 않을 정도로 커야 하는데 대략 100㎛ 전후인 것이 바람직하다. 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. It is preferable that the diameter of the lower grid 21 is generally about 3.0 mm and the thickness is about 50 µm (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 μm.
하부윈도우필름(22)은, 하부그리드(21)와 접해 있으면서 전자빔은 통과하고 wet-cell(20) 내부의 공기나 수분 등의 누출을 방지하는 기능을 함과 동시에, 하부그리드(21)와 접하는 반대면(즉, 상면)에 시료를 안착(부착)시키는 기능을 하는 것이다. 하부윈도우필름(22)으로는 전자빔의 직진성에 영향을 주지 않는 다양한 종류의 합성수지 필름을 적용할 수 있다. 다만 TEM 관찰을 위해서 상기 하부윈도우필름(22)은 카본필름인 것이 바람직하다. 필름의 두께는 큰 제한이 없으며, 대략 5~10㎛ 정도의 것으로 충분하다. 하부윈도우필름(22)의 크기는 하부그리드(21)에 형성된 관통공(21a) 모두를 충분히 덮을 수 있을 정도의 크기 이상이다. 본 발명에 의한 전자현미경 홀더를 도시한 도면에서는 하부윈도우필름(22)이 관통공(21a)을 모두 덮지만 스페이서(23)와는 접하지 않는 크기로 예시되어 있지만, 더 커서 스페이서(23)의 하면과 접하게 되더라도 관계없음은 명백하다. 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). As the lower window film 22, various kinds of synthetic resin films that do not affect the straightness of the electron beam may be applied. However, in order to observe the TEM, the lower window film 22 is preferably a carbon film. There is no big restriction | limiting in the thickness of a film, and about 5-10 micrometers is enough. The size of the lower window film 22 is larger than the size enough to cover all of the through holes 21a formed in the lower grid 21. In the drawing showing the electron microscope holder according to the present invention, although 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.
본 발명에 의한 wet-cell(20)이 홀더팁(10)에 장착되어 관찰될 때, 외부(전자현미경 경통)가 진공이므로 하부그리드(21)와 하부윈도우필름(22)에 강한 밀착력이 자연스럽게 발생한다. 따라서 본 발명에서 하부그리드(21)와 하부윈도우필름(22)은 굳이 접착제 등으로 접착될 필요는 없고 조립과정에서 분리되지 않을 정도로만 밀착되어 있으면 충분하다. 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.
본 발명에서 상기 스페이서(23)는, 대향되어 장착되는 상기 하부그리드(21)와 상부그리드(25) 사이의 외주변에 개재되어 상기 하부그리드(21)와 상부그리드(25) 사이의 간격을 유지하면서 내부를 밀폐하는 기능을 함과 동시에 상기 홀더팁(10)의 유입로 및 유출로와 wet-cell(20) 내부를 연통시키는 역할을 한다. 즉, 스페이서(23)는 외경이 상기 수용공간(11)에 대응되고, 상기 하부그리드(21)의 관통공(21a)이 노출되도록 중공부가 형성되어 있고, 측면에 상기 유입로 및 유출로에 대응되는 관통로(23a)가 형성되어 있으며, 상기 하부그리드(21)의 외주변에 안착된다. 상기 관통로는 상기 유입로 및 유출로에 대응되는 위치에 대응되는 크기로 형성될 수 있는데, 이 경우 유입로, 유출로와 관통로를 쉽게 일치시키기 위해 상기 수용공간(11)과 스페이서(23) 사이에 소정의 위치결정수단(도시 생략)을 형성하는 것이 바람직하다. 또는 상기 관통로를 스페이서(23)의 측면에 넓게 형성하여 관통로와 유입로, 유출로가 여유있게 접하도록 하거나, 세 개 이상의 관통로를 두어 임의의 관통로가 유입로, 유출로와 연통되도록 하는 것도 좋다. 도면(도 10)에서는 6개의 관통로를 둔 것이 예시되어 있다. 스페이서(23)의 두께는 결국 상기 하부그리드(21)와 상부그리드(25) 사이의 간격(시료가 안착되는 공간의 높이)을 결정하게 되는데, 조립작업의 편의성을 위해 50~500㎛ 정도의 두께인 것이 좋다. 스페이서(23)의 재질은 상기 하부그리드(21)의 재질처럼 금속이거나, 적절한 강도를 가진 합성수지일 수 있다.In the present invention, 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. In this case, 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. Alternatively, 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 μm. 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.
상부윈도우필름(24)은 상부그리드(25)의 하면에, 관통공(25a)을 모두 덮도록 안착되는 것이며, 상부그리드(25)는 직경이 상기 수용공간(11)에 대응되며, 중앙부에 상기 하부그리드(21)의 관통공(21a)에 대응되는 관통공(25a)이 형성되어 있는 것인데, 그 규격, 재질, 특성 등은 전술한 하부윈도우필름(22) 및 하부그리드(21)의 그것과 동일할 수 있다. 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.
본 발명에 의한 미세장치에서 하부그리드(21)와 상부그리드(25)는 내면에 각각 하부윈도우필름(22)과 상부윈도우필름(24)을 부착하고 있으면서 상기 관통공(21a, 25a)이 수직으로 일치되어 전자빔이 하부그리드(21)와 상부그리드(25)에 형성된 관통공(21a, 25a)을 통과할 수 있도록 대향 결합되어 있다. 본 발명에 의한 구성요소들은 매우 미세한 크기(하부그리드(21)와 상부그리드(25)가 대략 3㎜ 정도)이므로 하부그리드(21)와 상부그리드(25)를 대향결합 시킬 때 관통공(21a, 25a)을 수직으로 일치시키는 것이 용이하지 않을 수 있다. 이러한 불편함을 해소하기 위해, 하부그리드(21), 스페이서(23), 상부그리드(25)와 상기 수용공간(11)의 접하는 곳에 소정의 위치(방향)결정수단(도시 생략)을 형성해 두는 것도 좋다. 예를 들면 하부그리드(21), 스페이서(23), 상부그리드(25)의 외주연 일부를 직선이 되도록 하거나, 외주연에 홈을 두며, 그에 대응되는 수용공간(11)의 일부를 직선이 되도록 하거나 돌출홈을 두어 wet-cell(20) 조립장착시 하부그리드(21), 스페이서(23), 상부그리드(25)의 위치(방향)결정을 용이하게 할 수 있을 것이다.In the micro apparatus according to the present invention, 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. In agreement with each other, 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). In order to solve this inconvenience, it is also possible to form 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). good. For example, 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. Or it may be easy to determine the position (direction) of the lower grid 21, the spacer 23, the upper grid 25 when mounting the wet-cell (20) assembly.
본 발명에서 상기 고정캡(26)은, 순서대로 안착된 상기 하부그리드(21)-스페이서(23)-상부그리드(25)를 압박하여 고정하여 밀폐시키는 기능을 하는 것으로서, 직경이 상기 수용공간(11)에 대응되고, 상기 상부그리드(25)의 관통공(25a)이 노출되도록 중공부가 형성되어 있는 링 형상이다. 안전한 고정과 밀폐를 위해, 고정캡(26)의 외주변과 그에 대응되는 수용공간(11) 부위가 서로 대응되는 나사산 구조(도시 생략)로 되어 있어 나사체결 방식으로 고정될 수 있도록 하는 것이 좋다.In the present invention, 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. For safe fixing and sealing, 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.
한편, 수용공간(11)과 wet-cell(20) 각 구성요소들 사이의 수직 접촉면에서 밀폐력이 떨어지는 경우 그 사이로 wet-cell(20) 내부의 가스 또는 액체가 외부(전자현미경 경통)로 누출될 우려가 있다. 이러한 수직접촉면에서의 누출 가능성을 방지하기 위하여, 도 7~10에 도시된 것처럼, 상기 수용공간(11)의 상기 상부그리드(25)에 대응되는 부위에 제2단턱(12a)이 형성되어 있고, 상기 상부그리드(25)의 측면이 상기 제2단턱(12a)에 대응되는 구조가 되도록 하는 것이 좋다. 이에 의하면 상부그리드(25)가 고정캡(26)에 의하 아래로 눌려지면서 제2단턱(12a)에서 수용공간(11)과 강하게 밀착되므로 내부의 가스나 액체의 누출염려가 없어진다.On the other hand, when the sealing force is reduced at the vertical contact surface between the receiving space 11 and each of the components of the wet-cell 20, gas or liquid inside the wet-cell 20 may leak to the outside (electron microscope tube). There is concern. In order to prevent the possibility of such a leak in the vertical contact surface, as shown in Figs. 7 to 10, 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). As a result, 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.
이상과 같은 구성요소로 이루어진 본 발명에 의한 전자현미경용 wet-cell(20) 홀더는, 예를 들면, 다음과 같은 과정을 거쳐 시료가 안착된 상태로 조립될 수 있다.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.
먼저 (A) 증류수 등의 액체 위에 상기 하부윈도우필름(22) 또는 상부윈도우필름(24)을을 띄운 상태에서, (B) 포셉 등으로 하부그리드(21) 또는 상부그리드(25)를 홀딩한 상태로 아래에서 위로 상기 하부윈도우필름(22) 또는 상부윈도우필름(24)을 건져 올려 하부그리드(21) 또는 상부그리드(25) 위에 하부윈도우필름(22) 또는 상부윈도우필름(24)을, 관통공(21a, 25a)이 모두 덮혀지도록 안착시키고 건조한다. 이어서 (C) 하부윈도우필름(22)이 상면에 안착된 하부그리드(21)를 상기 홀더팁(10)의 수용공간(11)에 삽입하여 단턱(12)에 안착시킨 다음 (D) 상기 스페이서(23)를 수용공간(11)에 삽입하여 관통로(23a)를 상기 홀더팁(10)의 유입로 및 유출로에 대응되도록 위치시키면서 하부그리드(21)에 안착시킨다. 이어서 (E) 상기 상부그리드(25)를, 상부윈도우필름(24)이 아래를 향하도록 수용공간(11)에 삽입하여 스페이서(23) 위에, 하부그리드(21)와 상부그리드(25)의 관통공(21a, 25a)이 수직으로 일치되도록 안착시킨 다음, (F) 상기 고정캡(26)을 수용공간(11)에 삽입장착하여 상기 하부그리드(21)-스페이서(23)-상부그리드(25)를 압박하여 고정한다. 이렇게 조립된 상태의 부분단면사시도가 도 8, 9에 예시되어 있다[시료 도시 생략].(A) 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. Subsequently, (C) 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. 23 is inserted into the receiving space 11 to be seated in the lower grid 21 while positioning the through passage (23a) to correspond to the inlet and outlet of the holder tip (10). Subsequently, (E) the upper grid 25 is inserted into the receiving space 11 so that the upper window film 24 faces downward, and penetrates the lower grid 21 and the upper grid 25 on the spacer 23. The seats 21a and 25a are seated vertically, and then (F) the fixing cap 26 is inserted into the receiving space 11 so that the lower grid 21-spacer 23-upper grid 25 ) Press to fix it. A partial cross-sectional perspective view of the assembled state is illustrated in FIGS. 8 and 9 (sample not shown).
한편, 상기 단계(C) 전 또는 후에 상기 하부윈도우필름(22) 표면에 시료를 로딩하는 단계;를 추가로 둘 수도 있다. On the other hand, loading the sample on the surface of the lower window film 22 before or after the step (C); may be further added.
이렇게 조립된 본 발명에 의한 전자현미경용 wet-cell(20) 홀더는, 전자현미경의 경통에 삽입된 다음 소정의 가스 또는 액체를 가하면서 시료의 경시적 변화를 관찰하는데 이용되는 것이다.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.

Claims (5)

  1. (A) 팁 부위에 하기 cell이 한 방향으로 삽입 장착되도록 단턱이 형성되어 있는 원통형상의 수용공간; 상기 수용공간을 향하여 형성된 유입로 및 유출로;를 포함하는 전자현미경용 홀더팁: (A) a cylindrical accommodating space in which a step is formed so that the following cell is inserted and mounted in one direction at a tip portion; Electron microscope holder tip including; inlet and outlet formed toward the receiving space:
    (B) ① 직경이 상기 수용공간에 대응되어 상기 단턱에 안착되며, 중앙부에 소정 개수의 빔 통과용 관통공이 형성되어 있는 하부그리드; (B) a lower grid having a diameter corresponding to the receiving space and seated on the stepped portion, and having a predetermined number of through holes for beam passing therethrough;
    ② 상기 하부그리드의 상면에, 관통공을 모두 덮도록 안착되는 하부윈도우필름; A lower window film seated on the upper surface of the lower grid to cover all of the through holes;
    ③ 외경이 상기 수용공간에 대응되고, 상기 하부그리드의 관통공이 노출되도록 중공부가 형성되어 있고, 측면에 상기 유입로 및 유출로에 대응되는 관통로가 형성되어 있으며, 상기 하부그리드의 외주변에 안착되는 스페이서; 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 하기 상부그리드의 하면에, 관통공을 모두 덮도록 안착되는 상부윈도우필름; ④ an upper window film seated on the lower surface of the upper grid to cover all of the through holes;
    ⑤ 직경이 상기 수용공간에 대응되며, 중앙부에 상기 하부그리드의 관통공에 대응되는 관통공이 형성되어 있는 상부그리드; 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;
    ⑥ 직경이 상기 수용공간에 대응되고, 상기 상부그리드의 관통공이 노출되도록 중공부가 형성되어 있으며, 안착된 상기 하부그리드-스페이서-상부그리드를 압박하여 고정하는 고정캡;을 포함하는 wet-cell:⑥ a diameter corresponding to the receiving space, the hollow portion is formed so that the through hole of the upper grid is exposed, a fixed cap for pressing and fixing the seated lower grid-spacer-upper grid; wet-cell comprising:
    을 가지는 전자현미경용 wet-cell 홀더.Wet-cell holder for electron microscopes.
  2. 제 1 항에 있어서,The method of claim 1,
    상기 수용공간의 상기 상부그리드에 대응되는 부위에 제2단턱이 형성되어 있고, 상기 상부그리드의 측면이 상기 제2단턱에 대응되는 구조인 것을 특징으로 하는 전자현미경용 wet-cell 홀더.The second stepped portion is formed in a portion corresponding to the upper grid of the receiving space, the side of the upper grid wet-cell holder for the electron microscope, characterized in that the structure corresponding to the second step.
  3. 제 1 항 또는 제 2 항에 있어서,The method according to claim 1 or 2,
    상기 하부윈도우필름(22)은 카본필름인 것을 특징으로 하는 전자현미경용 wet-cell 홀더.The lower window film 22 is a wet-cell holder for an electron microscope, characterized in that the carbon film.
  4. (A) 증류수에 상기 하부윈도우필름 또는 상부윈도우필름을 띄우는 단계;(A) floating the lower window film or the upper window film in distilled water;
    (B) 상기 하부그리드 또는 상부그리드 위에 상기 하부윈도우필름 및 상부윈도우필름을 안착시키고 건조하는 단계;(B) mounting and drying the lower window film and the upper window film on the lower grid or the upper grid;
    (C) 하부윈도우필름이 상면에 안착된 하부그리드를 상기 홀더팁의 수용공간에 삽입하여 단턱에 안착시키는 단계;(C) inserting the lower grid seated on the upper surface of the lower window film in the receiving space of the holder tip and seated on the step;
    (D) 상기 스페이서를 수용공간에 삽입하여 관통로를 홀더팁의 유입로 및 유출로에 대응되도록 하여 하부그리드에 안착시키는 단계;(D) inserting the spacer into the receiving space to be fitted to the lower grid to correspond to the inlet and outlet of the holder tip;
    (E) 상기 상부그리드를, 상부윈도우필름이 아래를 향하도록 수용공간에 삽입하여 스페이서에 안착시키는 단계;(E) inserting the upper grid into the receiving space so that the upper window film faces downward;
    (F) 상기 고정캡으로 상기 하부그리드-스페이서-상부그리드를 압박하여 고정하는 단계;(F) pressing and fixing the lower grid-spacer-upper grid with the fixing cap;
    를 포함하는 것을 특징으로 하는 제 1 항 내지 제 3 항 중 어느 한 항에 의한 미세장치의 조립방법.Method for assembling the micro device according to any one of claims 1 to 3, characterized in that it comprises a.
  5. 제 4 항에 있어서,The method of claim 4, wherein
    상기 단계(C) 전 또는 후에 상기 하부윈도우필름(22) 표면에 시료를 로딩하는 단계;를 추가로 포함하는 것을 특징으로 하는 제1항 내지 제3항 중 어느 한 항에 의한 미세장치의 조립방법.The method of assembling the micro device according to any one of claims 1 to 3, further comprising the step of loading a sample on the surface of the lower window film 22 before or after the step (C). .
PCT/KR2014/009012 2014-09-26 2014-09-26 Electron microscope holder for sample observation in gas or liquid phase WO2016047829A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/KR2014/009012 WO2016047829A1 (en) 2014-09-26 2014-09-26 Electron microscope holder for sample observation in gas or liquid phase

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2014/009012 WO2016047829A1 (en) 2014-09-26 2014-09-26 Electron microscope holder for sample observation in gas or liquid phase

Publications (1)

Publication Number Publication Date
WO2016047829A1 true WO2016047829A1 (en) 2016-03-31

Family

ID=55581343

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2014/009012 WO2016047829A1 (en) 2014-09-26 2014-09-26 Electron microscope holder for sample observation in gas or liquid phase

Country Status (1)

Country Link
WO (1) WO2016047829A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876234A (en) * 2017-04-17 2017-06-20 南京大学 A kind of sample stage for the analysis of mineral facies automatic identification
WO2019010390A1 (en) * 2017-07-06 2019-01-10 Protochips, Inc. Electron microscope sample holder fluid handling with independent pressure and flow control

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 (en) * 2012-03-09 2013-09-12 株式会社 日立製作所 Liquid sample holder for electron microscope and method for manufacturing same
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 (en) * 2012-03-09 2013-09-12 株式会社 日立製作所 Liquid sample holder for electron microscope and method for manufacturing same

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876234A (en) * 2017-04-17 2017-06-20 南京大学 A kind of sample stage for the analysis of mineral facies automatic identification
CN106876234B (en) * 2017-04-17 2018-06-26 南京大学 A kind of sample stage for the analysis of mineral facies automatic identification
WO2019010390A1 (en) * 2017-07-06 2019-01-10 Protochips, Inc. Electron microscope sample holder fluid handling with independent pressure and flow control
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

Similar Documents

Publication Publication Date Title
JP6666313B2 (en) Connectors for pneumatic devices in microfluidic systems
US5494641A (en) Connectorized capillaries for use with separation instrumentation components
US7807979B2 (en) Specimen kit and fabricating method thereof
PT788600E (en) MEMBRANE FIXING DEVICE AND HIGH PERFORMANCE TECHNIQUE DEMANDING REDUCED FLUID VOLUME
US9797837B2 (en) Detector and detection method
JP2017523412A (en) Microfluidic cartridge with pipette operation guide
EP2681550B1 (en) Handheld device for electrophysiological analysis
CN210108849U (en) Transmission electron microscope in-situ liquid environment mechanical test platform
CN109425573B (en) Solution detection device and detection method
WO2016108401A1 (en) Particle separation and concentration apparatus, and method for separating, concentrating and discharging particle using same
WO2016047829A1 (en) Electron microscope holder for sample observation in gas or liquid phase
US10273523B2 (en) Imaging cartridge, pipette, and method of use for direct sputum smear microscopy
JP2019179040A (en) Replaceable ground electrodes for electrophysiology, electrode rejuvenating apparatus, and related methods and systems
EP2587257A1 (en) Slide holder assembly for comet assay
US8529740B2 (en) Electrochemical apparatus comprising modified disposable rectangular cuvette
WO2017099357A1 (en) Sample extraction container assembly including pipette
CN112899124A (en) Anaerobic microorganism culture and real-time observation device
US7245368B2 (en) Sample chamber for microscopy
WO2015072586A1 (en) Micro device provided to tem holder so as to enable observation of moisture-containing sample through tem
CN111774111A (en) Micro-fluidic chip for detecting glycosylated hemoglobin and detection method thereof
US20180230416A1 (en) Cell chip and dynamic dialysis staining for cells
US9862919B2 (en) Device and method for identification of microorganisms
CN210994383U (en) Clamp and device and system thereof
WO2020222417A1 (en) Pressing-type specimen sampling apparatus
TW201406953A (en) Cell-assembly array chip and manufacturing method thereof

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14902369

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 14902369

Country of ref document: EP

Kind code of ref document: A1