TW201216316A - TEM phase plate loading system - Google Patents

TEM phase plate loading system Download PDF

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Publication number
TW201216316A
TW201216316A TW099134110A TW99134110A TW201216316A TW 201216316 A TW201216316 A TW 201216316A TW 099134110 A TW099134110 A TW 099134110A TW 99134110 A TW99134110 A TW 99134110A TW 201216316 A TW201216316 A TW 201216316A
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TW
Taiwan
Prior art keywords
phase plate
loading system
electron microscope
phase
sample
Prior art date
Application number
TW099134110A
Other languages
Chinese (zh)
Inventor
Yunn-Shin Shiue
Shao-Kang Hung
Ching-Kai Lin
I-Hui Chen
Chia-Seng Chang
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Academia Sinica
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Priority to TW099134110A priority Critical patent/TW201216316A/en
Publication of TW201216316A publication Critical patent/TW201216316A/en

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26Electron or ion microscopes; Electron or ion diffraction tubes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/02Details
    • H01J2237/024Moving components not otherwise provided for
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26Electron or ion microscopes
    • H01J2237/2614Holography or phase contrast, phase related imaging in general, e.g. phase plates

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

Abstract

The invention discloses a phase plate loading system of a TEM column, which can be installed on any commercial TEM without the need to modify its optical design. This loading system is equipped with an airlock chamber that permits quick loading of a phase plate without the need to re-vent the TEM column. The system also uses a three-axis nano-motor in three translational directions (x, y, and z), for loading the phase plate and fine tuning the phase plate position.

Description

201216316 六、發明說明: 【發明所屬之技術領域】 本發明係關於一種穿透式電子顯微鏡相位板裝載系 統。 【先前技術】 近年來,相位穿透式電子顯微鏡(phase transmissi〇rl electron microscopy,phase TEM)的發展迅速,一般認為若 能成功應用’將能在結構生物學領域帶來突破性的影響。 若有了相位穿透式電子顯微鏡和波形重建的方法,我們可 以利用其得知一些傳統穿透式電子顯微鏡所得不到的生 物結構資訊。一般而言,在發展相位穿透式電子顯微鏡於 生物影像領域的應用時’需克服的技術問題有:(1 )於穿 透式電子顯微鏡安裝相位板時,不能影響穿透式電子顯微 鏡原有的功能;(2)相位板需以奈米級的控制精準度定位 於後聚焦平面;(3 )製作可靠度高的相位板;以及(4 ) 需使用低溫電子顯微鏡和低劑量的成像以避免在成像過 程中破壞到脆弱的生物結構。 目前有許多種類的相位板正在杳展中,包含Zernike 相位板和Hilbert相位板。Zernike相位板可適用於薄膜式、 靜電式或是磁式的相位板。Hilbert相位板則可適用於薄膜 式和磁式的相位板。然而,無論是使用那一種的相位板, 最重要的是,如何把相位板放進穿透式電子顯微鏡腔體和 極片間隙(pole piece gap)的有限空間中以達到使相位對 201216316 比增進目的 用0 但又不能影響穿透式電子顯微鏡的正常使 過去的技術中,欲裝載相位板至穿透式電子 丁顯微鏡 時,需要改變既有電子顯微鏡的光路構造,像1力。^ 雙合轉接透鏡(transfer lens doublet)。如此改變暫 個 主1LJ穿透 式電子顯微鏡的光學路徑的設計並非是個小工# 私,故也盔201216316 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a transmission electron microscope phase plate loading system. [Prior Art] In recent years, phase transmissi〇rl electron microscopy (phase TEM) has developed rapidly, and it is generally believed that successful application will bring about a breakthrough impact in the field of structural biology. With phase-transmission electron microscopy and waveform reconstruction, we can use it to learn about the biological structure that is not available with traditional transmission electron microscopy. In general, when developing the application of phase-transmissive electron microscopy in the field of biological imaging, the technical problems to be overcome are: (1) When the phase plate is installed in a transmission electron microscope, the original of the transmission electron microscope cannot be affected. (2) the phase plate needs to be positioned in the back focus plane with nanometer control accuracy; (3) to produce a highly reliable phase plate; and (4) to use a low temperature electron microscope and low dose imaging to avoid Destruction of fragile biological structures during imaging. There are many types of phase plates currently in development, including Zernike phase plates and Hilbert phase plates. Zernike phase plates are available for thin film, electrostatic or magnetic phase plates. The Hilbert phase plate is suitable for both thin film and magnetic phase plates. However, no matter which phase plate is used, the most important thing is how to put the phase plate into the limited space of the penetrating electron microscope cavity and the pole piece gap to achieve the phase ratio of 201216316. The purpose of using 0 but not affecting the normality of the transmission electron microscope is that in the past technology, when the phase plate is to be loaded to the transmissive electron microscope, it is necessary to change the optical path structure of the existing electron microscope, like a force. ^ Transfer lens doublet. So the design of the optical path of the main 1LJ transmission electron microscope is not a small worker, so it is also a helmet.

法吸引已具有穿透式電子顯微鏡的使用者。另一種將相^ 板放進穿透式電子顯微鏡的方式則是要先將電子顯^位 停機,打開其樣品腔的部分,將相位板放至定位後再、& 體封起,然後重新將整台穿透式電子顯微鏡抽真空 機。此種方錢*實際’因為每次換相位板需钱 間,且經常將穿透式電子顯微鏡停機拆開容易對極為昂眚 之穿透式電子顯微鏡造成毁損,降低其使用壽命。‘ 因此如何提供一種相位板裝載系統,在不改變原有The method attracts users who already have a transmission electron microscope. Another way to put the phase plate into the transmission electron microscope is to stop the electronic display, open the part of the sample cavity, place the phase plate after positioning, & body seal, then re- The entire transmissive electron microscope vacuum pump will be used. This kind of money*actually because every time you change the phase plate, you need to spend money, and often disassemble the penetrating electron microscope to easily damage the extremely expensive penetrating electron microscope and reduce its service life. ‘So how to provide a phase plate loading system without changing the original

=透式電子顯微鏡的光學構造,且*需將顯微鏡停機的 則提下X字相位板裝載至穿透式電子顯微鏡内,並降低裝 載才板所%的時間至實際使用鸾子顯微鏡可接受的時 間範圍,已成為重要課題之一。= optical construction of the transmission electron microscope, and * when the microscope is stopped, the X-shaped phase plate is loaded into the transmission electron microscope, and the time required to load the board is reduced to the actual use of the tweezers microscope. The time horizon has become one of the important topics.

【發明内容】 I /有4a於上述課題.,本發明之目的為提供—種相位板裝 載系統’在錢變原有的穿透式電子顯微鏡的光學構造且 不/頁將電子顯微鏡停機的前提下’裝載相位板至穿透式電 子顯微鏡’並減少整個裝载相位板所需的時間。 5 201216316 為達上述目的,依據本發明之一種相位板装載系統 ”一f透式電子顯微鏡配合,並包含—預抽氣㈣以及〆 傳輸定位單元。預抽氣密腔鄰設於穿透式電子顯微鏡之樣 品區段;傳輸定位單元係經由預抽氣密腔,穿過樣品區段 原有之開口埠,傳輸一相位板至穿透式電子顯微鏡内。 ,本發明—實施财’預抽氣密腔與—幫浦單元連 …°八中’幫浦單元可為-獨立之_單元, 式電子顯微鏡中已有之一預抽氣幫浦單元。…’、 在本發明一實施例中,樣品區段之開口埠,包含一 X 射線他畺放佈光譜儀痒或一物鏡光圈埠。 〜在本發明一實施例中,樣品區段包含一樣品腔,預抽 乳饮腔與樣品腔之間為可連通,但由一間門閥隔開。 =本發m财,傳輸定位單元更包含一導執, 6又置於預抽氣密腔上。 2發I實施财,相位板為—靜電式相 一磁式相位板、或一薄膜式相位板:!。 汊 =發明一實施例中,傳輸定位單元包含一馬達,其 個方± 達為7~壓電馬達,並具有三 個方向自由度。較佳地,傳輪枭 與馬達連結。較佳地,傳卜_ 裝载柃, 件,與馬達連結,相位板裝載件係裝載相位板。載 ^本㈣-實施例中,相位板裝載系統更包含—定位 勺二二旦/監控樣品區段之影像。較佳地,定位監控單元 C s —攝影機、或—感測元件。 201216316 在本發明一實施例中,樣品區段包含一防污染元件, 相位板安裝至防污染元件内。較佳地,樣品區段包含一樣 品裝載件,相位板安裝至樣品裝載件與防污染元件之間。 承上所述,因依據本發明之一種穿透式電子顯微鏡相 位板裝載系統,經由鄰設於穿透式電子顯微鏡樣品區段之 預抽氣密腔,以讓傳輸定位單元將相位板傳輸定位至顯微 鏡内,而不需改變穿透式電子顯微鏡内部的光學系統結 構,即可適用於任何既有的穿透式電子顯微鏡及各式的相 Φ 位板。與習知相較,本發明利用預抽氣密腔的設置,可將 相位板預抽真空後再傳輸進穿透式電子顯微鏡,所以不需 - 要為了裝載相位板而將電子顯微鏡停機後再重新抽真 - 空,進而將裝載相位板至穿透式顯微鏡所需的時間大幅降 低,例如於實施例中,裝載時間可從幾天減低至一小時以 内。最重要的是不需拆開電子顯微鏡即可裝載相位板。本 發明讓實際操作使用相位穿透式電子顯微鏡化為可能。 •【實施方式】 以下將參照相關圖式,說明依據本發明較佳實施例之 一種相位板裝載系統。 請參照圖1所示,其為本發明之一種相位板裝載系統 裝載於穿透式電子顯微鏡的透視圖。相位板裝載系統1與 一穿透式電子顯微鏡2配合,並包含一預抽氣密腔(airlock chamber) 11以及一傳輸定位單元12。 首先,先介紹與本發明之相位板裝載系統1搭配使用 201216316 的穿透式電子顯微鏡2,其係為-習知技術即有的 微鏡,主要由鏡筒(cohimn) 21、真空系統(圖中未顯示^ 和電源控制系統(圖中未顯示)三部分組成。鏡筒^不包 含有電子搶、電子透鏡、樣品裝料、螢光 = 等部件,這些部件通常是自上而下地裝配成―個^機^ 空糸統可由機械真空幫浦、擴散幫浦和真空閥門等構成^ $通過抽氣管道與鏡筒21相聯接1源控㈣統則可包 含局壓發生器、勵磁電流穩流器及各種調節控制單元。 ,預抽氣密腔11是本發明中額外設置於穿透式電子顯 微鏡2外的-個腔室,其係鄰設於穿透式電子顯微鏡以 樣品區段2!卜其中,樣品區段211為樣品聚載谭所處之 區段,具有-樣品腔217 ’樣品設置於極片(p〇lepi⑽) 214之間,複數個開口蜂係設置於樣品區段叫以作為不 同用途使两,其中包含一物鏡光圈埠(〇咖加叩如⑽ P〇rt) 212及—X射線能量散佈光譜儀埠(EDS port) 213。 預抽氣密腔11可設置於樣品區段211的任—的空置開口谭 中/’並能藉由1⑽(娜valve )丨i丨*與?透式電子 顯微鏡2内部的樣品腔217導通。實際運作上,會設置相 位板;13.之穿透式電子顯微鏡2通常不需要X射線能量散 佈光4儀,因此X射線能量散佈光譜儀璋213會空置而可 用來安裝本發明之相位板裝裁系統1。 預抽氣密腔Π可設計成為體積相當小的腔室,以設 置於,。π區段211的開口埠外,而不阻礙其他組件的設置。 明同%•參考圖2及圖4所示,圖2為預抽氣密腔及傳 201216316 早凡設置於f透式電子顯微鏡的示意圖,圖4列為 ==位遠單元的詳細構造示意圖。預柚氣密腔二 獨立單元14為- 在μ ·2之真空线外的幫浦單元U。 ==:依各種類穿透式電子顯微鏡2的不同内部 顯微鏡2内之-J氣;;單Γ為設置於穿透式電子 於前述的真空系統中1早叫且整合 當不需使用相位板13時,預抽氣密腔 一個摘置”供相位板13置放。並且 = π位板觀察生物樣本時,產生的污染可能^ "grgtfect),^^fI^4^11 /、'义W’因此加熱相位板的過程不須在低溫樣本旁進 行可避免跪弱的低溫樣本受到熱傷宝。 傳輸疋位單元12係傳輸定位_相位板13至穿透式電 子_鏡2内’於此’傳輸定位單元12係包含—馬達⑵, 關於傳輸定位單元12之構造細節騎後詳述。 ,將裝載有相錄13的傳料位單幻2的—端放入預 抽氣密腔11後,藉由開啟相位板預抽氣闕(phase細 pre pumping valve) 141 ’讓預抽氣密腔u利用幫浦單元 14進行抽氣。待達到理想的真空狀態後,再開啟預抽氣密 腔11與鏡筒之間的閘門閥111,以利用馬達121傳輸相位 板13至穿透式電子顯微鏡2的鏡筒心如此—來,並不 需要如習知技射,先將穿透式電子顯微鏡2停機拆開沒 201216316 :寺裳载相位板13後才再進行抽氣和復 ::板裝載系統1可節省《相位板η後,重= 到真空條件所需的抽氣i重新達 式電子顯料户9& 更重要的疋’不需拆開穿透 子/超2㈣可避免顯微鏡被 咖L JEM_2l〇〇F機型的穿透式電子 =來5兄 相位板_統1進行相位板u的更換,=SUMMARY OF THE INVENTION I / 4a is in the above-mentioned problem. The object of the present invention is to provide a phase plate loading system 'the optical structure of the transmission electron microscope which is used in the money and does not stop the electron microscope. Next 'Load the phase plate to the transmission electron microscope' and reduce the time required to load the entire phase plate. 5 201216316 In order to achieve the above object, a phase plate loading system according to the present invention cooperates with a f-transmission electron microscope, and includes a pre-extraction (four) and a sputum transmission positioning unit. The pre-extraction airtight chamber is adjacent to the transmission type. The sample section of the electron microscope; the transport positioning unit transmits a phase plate to the transmission electron microscope through the pre-extracting airtight cavity through the original opening of the sample section. The present invention-implements the pre-pumping The dense cavity and the pump unit are connected to each other. In the eighth embodiment, the pump unit can be an independent unit, and one of the pre-exhaust pump units is provided in the electron microscope. The opening of the sample section includes an X-ray spectroscopy spectrometer itch or an objective aperture 埠. In an embodiment of the invention, the sample section comprises a sample chamber between the pre-drinking cavity and the sample chamber It is connectable, but separated by a door valve. = This is a m-fund, the transmission positioning unit further includes a guide, and 6 is placed on the pre-extracting airtight chamber. 2I I implement the money, the phase plate is - electrostatic Phase-magnetic phase plate, or a thin film phase !=Inventive In one embodiment, the transmission positioning unit comprises a motor, each of which has a 7~piezo motor and has three degrees of freedom. Preferably, the transmission rim is coupled to the motor. Good, 传 _ loading 柃, parts, and motor connection, phase plate loading parts are loaded phase plate. Loaded (4) - In the embodiment, the phase plate loading system further includes - positioning spoon 22nd / monitoring sample area Preferably, the positioning monitoring unit C s is a camera, or a sensing component. 201216316 In an embodiment of the invention, the sample section includes an anti-contamination component, and the phase plate is mounted to the anti-contamination component. Preferably, the sample section comprises a sample carrier, the phase plate being mounted between the sample carrier and the anti-contamination component. According to the present invention, a transmissive electron microscope phase plate loading system according to the present invention is provided adjacent to Pre-extracting the airtight cavity in the sample section of the transmission electron microscope, so that the transmission positioning unit can position the phase plate into the microscope without changing the optical system structure inside the transmission electron microscope. Applicable to any existing transmissive electron microscope and various types of phase Φ-position plates. Compared with the prior art, the present invention utilizes the pre-extraction airtight chamber setting to pre-vacuate the phase plate and then transmit it through. Electron microscopy, so there is no need - to stop the electron microscope after loading the phase plate and then re-suck the true-air, which will greatly reduce the time required to load the phase plate to the penetrating microscope, for example in the embodiment, loading The time can be reduced from a few days to less than one hour. The most important thing is to load the phase plate without disassembling the electron microscope. The present invention makes it possible to use phase-transmissive electron microscopy in actual operation. Referring to the related drawings, a phase plate loading system in accordance with a preferred embodiment of the present invention will be described. Referring to Figure 1, there is shown a perspective view of a phase plate loading system of the present invention loaded on a transmission electron microscope. The phase plate loading system 1 cooperates with a transmission electron microscope 2 and includes a pre-extracting airlock chamber 11 and a transmission positioning unit 12. First, a transmissive electron microscope 2 using 201216316 in conjunction with the phase plate loading system 1 of the present invention will be first introduced, which is a conventional micromirror, mainly a lens tube (cohimn) 21, a vacuum system (Fig. The power supply control system (not shown) is not shown in three parts. The lens barrel does not contain components such as electronic grab, electronic lens, sample loading, fluorescent =, etc. These components are usually assembled from top to bottom. ―一^机^ The air system can be composed of mechanical vacuum pump, diffusion pump and vacuum valve. ^Connected to the lens barrel 21 through the suction pipe. 1 Source control (4) System can include local pressure generator, excitation current is stable The flow device and various adjustment control units. The pre-extracting airtight chamber 11 is a chamber additionally provided outside the transmission electron microscope 2 in the present invention, which is disposed adjacent to the transmission electron microscope to sample section 2 In the sample section 211, the sample is located in the section where the sample is collected, and the sample chamber 217' is placed between the pole pieces (p〇lepi(10)) 214, and a plurality of open bee lines are set in the sample section. To make two for different uses, including The objective aperture (埠 叩 ( ( ( ( ) ) 212 212 212 212 212 212 212 212 212 212 212 212 212 212 ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED ED /' can be turned on by the 1(10)(navalve)丨i丨* and the sample chamber 217 inside the transmissive electron microscope 2. In actual operation, a phase plate is provided; 13. The transmission electron microscope 2 usually does not need The X-ray energy disperses the light meter, so the X-ray energy dispersive spectrometer 璋213 is vacant and can be used to install the phase plate mounting system 1 of the present invention. The pre-extracting airtight chamber can be designed to be a relatively small chamber to set The opening of the π section 211 is outside, and does not hinder the setting of other components. The same as %2 refers to FIG. 2 and FIG. 4, and FIG. 2 shows the pre-extracting airtight cavity and the transmission 201216316 Schematic diagram of the electron microscope, Figure 4 shows the detailed structure diagram of the == remote unit. The pre-pome airtight chamber two independent unit 14 is - the pump unit U outside the vacuum line of μ · 2. ==: Type-transmission electron microscope 2 in the different internal microscope 2 - J gas; In the vacuum system described above, the penetrating electrons are first called and integrated. When the phase plate 13 is not needed, the pre-extracting airtight chamber is "applied" for the phase plate 13 to be placed. And when the biological sample is observed by the π-position plate The resulting pollution may be ^ "grgtfect), ^^fI^4^11 /, 'Ye W' so the process of heating the phase plate does not need to be carried out next to the low temperature sample to avoid the weak cold samples being thermally damaged. The bit unit 12 transmits the positioning_phase plate 13 to the transmissive electron mirror 2, and the transmission positioning unit 12 includes a motor (2). Details of the configuration of the transmission positioning unit 12 are detailed after riding. After the end of the transfer position of the record 13 is placed in the pre-exhaust airtight chamber 11, the pre-extraction is performed by opening the phase plate pre-pumping valve 141 ' The cavity u is pumped by the pump unit 14. After the desired vacuum state is reached, the gate valve 111 between the pre-exhaust airtight chamber 11 and the lens barrel is opened to transmit the phase plate 13 to the lens barrel of the transmission electron microscope 2 by the motor 121. It is not necessary to perform the technical shooting. First, the penetrating electron microscope 2 is shut down and not opened. 201216316: After the temple is loaded with the phase plate 13, the pumping and re-up are performed again: The board loading system 1 can save the phase plate η. Heavy = pumping required to vacuum conditions i re-arranged electronic display households 9 & more important 疋 'do not need to open the penetrator / super 2 (four) can avoid the penetration of the microscope by the coffee machine J JEM_2l〇〇F model Type of electronics = to 5 brother phase plate _ system 1 to replace the phase plate u, =

可達到顯微鏡運作所需的真空條件 刀 '里P =常更換相位板U以取得相位影像的使用^ 需特別注意的是,穿透式電子顯 同。Ί幫㈣統’依其幫浦效率其抽氣時間可能不 圖。詳細構造示意 二傳::位早…馬達121,在本實施例中為—㈣ 精準度為奈米級,並具有三個方向自由度(X,y, z〜達121包含複數金屬棒1211、複數 連,、,。’並朝向不同方向(x,.y,z) =再與上述金屬棒咖垂直連接,金屬部⑵3:電 ΓΓΓ/Λ而可沿著與其連料金屬棒1211的方向移 上為馬達121的其中—個方&上的移動機制,宜餘 的=向的移動機制亦同,因而使馬達121達到三個方向 、’丁、米尺度的移動,其精準度可達到1〇奈米以下。 接著’請再同時參考圖2及圖4所示,本實施例中, 傳輸定位單元12更可包含一裝載桿122、一導軌US以及 10 201216316 -相位板裝載件124,裝載桿i22 分別與馬達⑵的兩端連接,123設2= 7 11 ^用以導引裝载桿122進入穿透 : 同時限制使用者施與其旋轉力和橫向力m立 :板裝載㈣在裝載或卸载過程中遭到損害 =:裝及,·以承載並心:板: °月夢考圖5A及圖5B所示,i盔士政 位單元π穿、# 4带 ,、為本么明之一種傳輸定 位早兀政載於穿透式電子顯微鏡中的側視圖及 位板裝載件124係用以裝載相位板Π,相位板13為一靜 電式相位板、或-磁式相位板、或—薄膜式相位板月, 樣品區段211中更包含—防污染元件(_,nt_nati〇n ―⑶仏腳叫215,以及一樣品裂载件(sa 祕相,設置於穿透式電子顯微鏡2的兩個極片:: 〜η τ 叼 >可染元件 以使相位板裝载件124及其上 即可保留且不影響防污染元件 二…1相連的相位板裝载件124 裝載’亚傳輸至防料元件215内,且位於樣品裝載件別 與防染几件215之間。須特別注意的是,因防污 215設置於兩極片214之間,會阻礙相位板η的傳 徑。但防污染元件215係用來避免低溫樣本被污染 能十分重要不能隨意移除,故於本實施例中,= 215的開口處被略為挖大..、·&,. 卞70什 之相位板13可順利通過 215的功能。The vacuum conditions required for the operation of the microscope can be achieved. Knife 'P = often replace the phase plate U to obtain the phase image. ^ It is important to note that the penetrating electrons are identical. The gang (4) system may not be able to pump time according to its pump efficiency. The detailed configuration shows that the second pass: the motor 121, in this embodiment, is - (4) the accuracy is nanometer, and has three degrees of freedom (X, y, z ~ up to 121 includes a plurality of metal rods 1211, The plural is connected, , and . ' and oriented in different directions (x,.y,z) = and then vertically connected to the above metal bar, the metal portion (2) 3: electric ΓΓΓ / Λ can be moved along the direction of the metal rod 1211 The upper part is the movement mechanism of the motor 121, and the movement mechanism of the remaining = direction is the same, so that the motor 121 reaches the three directions, the movement of the 'd, m scale, and the precision can reach 1 In the present embodiment, the transfer positioning unit 12 further includes a loading rod 122, a guide rail US, and 10 201216316 - phase plate loading member 124, which are loaded as shown in FIG. 2 and FIG. The rods i22 are respectively connected to the two ends of the motor (2), and 123 is set to 2 = 7 11 ^ to guide the loading rod 122 into the penetration: at the same time restricting the user from applying the rotational force and the lateral force to the m: the plate loading (four) is loading or Damaged during the uninstall process =: loaded, · to carry the heart: board: ° month dream map 5A and FIG. 5B, the i-mirror political unit π-piercing, #4-belt, and a transmission positioning of the present invention are used in a transmissive electron microscope for side view and position plate loading member 124. In order to load the phase plate Π, the phase plate 13 is an electrostatic phase plate, or a magnetic phase plate, or a film phase plate, and the sample segment 211 further includes an anti-pollution component (_, nt_nati〇n - (3) The squat is called 215, and a sample splitting member (sa secret phase, set in the two pole pieces of the transmission electron microscope 2: ~ η τ 叼 > dyeable components to make the phase plate loading member 124 and its The phase plate loading member 124, which can be retained and does not affect the anti-pollution element, is connected to the anti-fouling element 215 and is located between the sample loading member and the anti-dyeing member 215. Special attention must be paid. Therefore, since the anti-fouling 215 is disposed between the two pole pieces 214, the diameter of the phase plate η is hindered. However, the anti-pollution element 215 is used to prevent the low-temperature sample from being contaminated, so that it cannot be removed at will, so in this embodiment. In the middle, the opening of 215 is slightly digging..,·&,. 卞70 Successfully passed the 215 function.

本毛月之一種相位板 ,更包含一定位監控單元15用執糸,,兄 i5用以監控由預抽氣密腔U 另外,如圖5B所示 * 11 201216316 傳輸至鏡筒21内的相位板13,是否準確到達定位。其中, 疋位監控單元15包含一攝影機、或一感測元件,用以監 控相位板13在樣品區段211内之位置。定位監控單元 设置於樣品區段211外,在實際運作上,定位監控單元15 可裝設於樣品區段211中之物鏡光圈埠212,但為了保持 原本物鏡光圈的功能,光圈可與相位板13的組件整合, 或是將物鏡光圈安裳於穿透式電子顯微鏡2的其他地方。 請同時參照圖5C及圖5D所示,其為本發明之相位板 利用工單元進行疋位對準的示意圖。使用者可透過電腦 螢幕觀看定位監控單元顯示承載有相位板13的相位板 裝載件124移動狀況,不僅可大幅減少脆弱的相位板u 與相位板裝載件124撞擊其他元件而被毀損的機會,更加 快I尋找相位孔131 (phaseplateh〇le)的速度。圖5d中 乂尋找相位孔131為例,說明如何使相位板13定位,讓 相位孔m對準於穿過樣品裝載件216之電子束。若實際 應用之相位孔為-環狀設計,此方法同樣可應用於定位對 準相位環’非用以限制本發明。如圖冗及5d所示,在實 際操作上’傳輸相位板13冑,使用者可依各種不同的相 板13規格,預先於相位板展載件124的側壁標記一標 圯線1241,u顯示相位孔131、的相對位置。當相位板裝載 件124插入於樣品裝載件216之下時,彳藉由定位監控單 凡15從側面觀看,並移動相位板裝載件124,使相位板裝 載件124側壁的標記線1241對準於樣品裝載件…的中 間,俾使相位孔131大致位於電子束穿過的位置。之後, 201216316 使用&者只要於觀察影像時利用穿透式電子顯微鏡2的微調 功Bb即可讓相位孔131精準地位於電子束穿過的位置。 另外,標記線1241可於使用後擦栻去除,再依下次使用 的相位极13所需對準的部位來重新標記,相當方便。再 ^丄本發明使用定位監控單元15的定位對準方式,不論 °又疋為手動控制、或是使用電腦自動控制,均能大幅滅少 使用者於裝載相位板13時的定位對準時間。 所述,依據本發明之一種穿透式電子顯微鏡相位 •板系統’經由鄰設於穿透式電子顯微鏡樣品區段之預 抽氣费胺’以讓傳輸定位單元將相位板傳輸定位至顯微鏡 ' 内命不而改變穿透式電子顯微鏡内部的光學系統結構,也 -不☆將电子顯微鏡停機拆開就可將相位板傳輸至所需位 置1可適用於任何既有的穿透式電子顯微鏡及各式的相位 板與1知相較,本發明利用預抽氣密腔的設置,不需要 為了裂载相位板而將電子顯微鏡停機後再重新抽真空,進 而將裝載相位板至穿透式顯微鏡所需的時間,從幾天大幅 一小時以内。最重要的是不需拆開電子顯微鏡即 =载相位板,可避免電子顯微鏡被毁損的機會。本發明 讓貫際操作使用相位穿透式電子顯微鏡化為可能。 二上:述僅為舉例性,而非為限制性者 離 之精神與㈣,而對其進行之等效修 均 應包含於後附之申請專利範圍中。 文 【圖式簡單說明】 13 201216316 載於穿透式電子顯 圖1為本發明之相位板裝载系統襄 微鏡的外觀透视圖; 、 圖2為本發明之預抽氣密 透式4子顯微鏡上的示意圖. 腔及傳輪定位單元設置於穿 圖3為本發明之馬達的詳細構造示意圖; 圖4為本發明之傳敎位單元的詳細構造示意圖; 圖5A及圖5B為本發明之傳輸定位單元裝载於穿遂 式電子顯微鏡中的側視圖及俯視圖;以及 圖5C及圖5D為本發明之相位板定位對準的示索圖。 【主要元件符號說明】 1 :相位板裝載系統 11 : 預抽氣密腔 111 : 閘門閥 12 : 傳輸定位單元 121 馬達 1211 .金屬棒 1212 :壓電元件 1213 :金屬部 122 裝载桿 123 導執 124 相位板裝载件 1241 •標記線 13 : 相位板 201216316 131 :相位板孔. 14 :幫浦單元 141 :相位板預抽氣閥 15 :定位監控單元 2:穿透式電子顯微鏡 21 :鏡筒 211 :樣品區段 212 :物鏡光圈埠 φ 213 : X射線能量散佈光譜儀埠 214 :極片 - 215 :防污染元件 _ 216:樣品裝載件 217:樣品腔A phase plate of the present month includes a positioning monitoring unit 15 for monitoring, and the brother i5 is used for monitoring the phase transmitted from the pre-extracting airtight chamber U to the inside of the lens barrel 21 as shown in FIG. 5B*11 201216316. The board 13 is accurately positioned. The clamp monitoring unit 15 includes a camera or a sensing component for monitoring the position of the phase plate 13 within the sample section 211. The positioning monitoring unit is disposed outside the sample section 211. In actual operation, the positioning monitoring unit 15 can be mounted on the objective aperture 埠 212 in the sample section 211, but in order to maintain the function of the original objective aperture, the aperture can be combined with the phase plate 13 The components are integrated, or the objective aperture is placed elsewhere in the transmission electron microscope 2. Please refer to FIG. 5C and FIG. 5D simultaneously, which is a schematic diagram of the phase alignment of the phase plate utilization unit of the present invention. The user can view the position monitoring unit through the computer screen to display the movement condition of the phase plate loading member 124 carrying the phase plate 13, which not only greatly reduces the chance that the fragile phase plate u and the phase plate loading member 124 are damaged by hitting other components, and Speed up I to find the speed of the phase hole 131 (phaseplateh〇le). In Fig. 5d, the phase hole 131 is taken as an example to illustrate how to position the phase plate 13 so that the phase hole m is aligned with the electron beam passing through the sample loading member 216. If the phase hole of the actual application is a ring-shaped design, this method can also be applied to the positioning of the alignment phase ring 'not to limit the invention. As shown in Fig. 5d and 5d, in actual operation, 'transmission phase plate 13胄, the user can mark a standard line 1241 in front of the side wall of the phase plate carrier 124 according to various different phase plate 13 specifications, u display The relative position of the phase hole 131. When the phase plate loading member 124 is inserted under the sample loading member 216, the positioning plate 12 is viewed from the side and the phase plate loading member 124 is moved to align the marking line 1241 of the side wall of the phase plate loading member 124 with In the middle of the sample loading member, the phase hole 131 is positioned substantially at a position where the electron beam passes. Then, 201216316 uses & as long as the fine adjustment function Bb of the transmission electron microscope 2 is used when observing the image, the phase hole 131 can be accurately positioned at the position where the electron beam passes. In addition, the marking line 1241 can be removed by rubbing after use, and then re-marked according to the portion of the phase pole 13 to be used next time, which is quite convenient. Further, the positioning alignment method of the positioning monitoring unit 15 of the present invention can greatly reduce the positioning alignment time of the user when loading the phase plate 13 regardless of whether the manual control or the automatic control of the computer is used. According to the present invention, a transmissive electron microscope phase plate system 'via a pre-extraction amine in the sample section of the transmission electron microscope to allow the transmission positioning unit to position the phase plate to the microscope' The internal structure does not change the structure of the optical system inside the transmission electron microscope. Also - no ☆ Disassemble the electron microscope to transfer the phase plate to the desired position. 1 It can be applied to any existing transmission electron microscope and Compared with the prior art, the present invention utilizes the pre-extraction airtight chamber arrangement, does not need to stop the electron microscope after the shutdown of the phase plate, and then re-vacuum, and then load the phase plate to the transmission microscope. The time required is significantly less than an hour from a few days. The most important thing is that you don't need to disassemble the electron microscope, ie the phase plate, to avoid the chance of the electron microscope being damaged. The present invention makes it possible to use a phase penetrating electron microscope for a continuous operation. 2. The above descriptions are for illustrative purposes only and are not intended to limit the spirit of the invention and (4), and equivalent modifications thereto shall be included in the scope of the appended patent application. [Simplified description of the drawing] 13 201216316 is shown in the perspective of the transmissive electronic display 1 is a perspective view of the microplate of the phase plate loading system of the present invention; and FIG. 2 is a pre-extracting and dense 4 submicroscope of the present invention. The schematic diagram of the above is shown in Fig. 3 is a detailed structural diagram of the motor of the present invention; Fig. 4 is a schematic structural diagram of the transmission unit of the present invention; Fig. 5A and Fig. 5B are transmissions of the present invention; A side view and a top view of the positioning unit mounted in the through-hole electron microscope; and FIGS. 5C and 5D are diagrams showing the alignment of the phase plate of the present invention. [Main component symbol description] 1 : Phase plate loading system 11 : Pre-exhaust airtight chamber 111 : Gate valve 12 : Transmission positioning unit 121 Motor 1211 . Metal rod 1212 : Piezoelectric element 1213 : Metal part 122 Loading rod 123 124 Phase plate loading piece 1241 • Marking line 13 : Phase plate 201216316 131 : Phase plate hole. 14 : Pump unit 141 : Phase plate pre-exhaust valve 15 : Positioning monitoring unit 2 : Penetrating electron microscope 21 : Lens barrel 211: sample section 212: objective aperture 埠 φ 213 : X-ray energy dispersive spectrometer 埠 214 : pole piece - 215 : anti-contamination element _ 216: sample holder 217: sample chamber

1515

Claims (1)

201216316 七 、申請專利範圍: 、,,相位板錢系統,與—穿透式電子顯微鏡配合, 亚包含: f抽乳⑥、腔’鄰設於該穿透式電子顯微鏡之樣品區 段;以及 」 單元,係經由該預抽氣密腔傳輸一相位板 至5亥穿透式電子顯微鏡内。 ^申μ專利㈣第1項所述之相位板统,其中 该預抽氣密腔係與一幫浦單元連結。 I!:,範圍第2項所述之相位板裝載系統,其中 獨立之幫浦單元或為該穿透式電子 顯倣鏡之一預抽氣幫浦單元。 4 專利範圍第1項所述之相位板裝載系統,其中 光圈埠。 Χ射線此罝散佈光譜儀埠或一物鏡 專,圍第1項所述之相位板裝齡統,其十 :門包含品腔’該預抽氣密腔與該樣品腔 之間為可連通,由一閘門闊隔開。 5、如申請專利範圍苐1 該傳衿定位星-L 相位板裝載系統,其中 上。則 兀匕含一導執,設置於該預抽氣密腔 申明專㈣目帛丨項所叙相位板裝㈣統, 该相位板為一靜電式相位 ,、τ 薄膜式相储。 m切位板、或- CD 16 201216316 兮傳二,軏圍第1項所述之相位板裝載系統,其中 9、;=位單元包含一馬達,其精準度為奈米級。 =利範圍第8項所述之相位板裝載系統,其中 -i。:申4了電馬達’並具㈣^ • %^:_範圍第8項所述之相位板裝載系統,其中 u、=r單元更包含—裂載桿,與該馬達連結。 第8項所述之相位板裝載系統,其中 =傳輪讀單元更包含—相位板«件,與該馬達連 專利範圍第n項所述之相位板裝載系統,其 中_位板裝載件餘载該相位板。 1申請專利範圍第1項所述之相位板裝載系統,更包 Η、如控Ϊ元’監控該相位板於該樣品區段之位置。 :利乾圍第13項所述之相位板裝載系統,其 中=立監控單元包含—攝影機、或一感測元件。 ^ 第1項所述之相位板裝載系統,其中 包含一防污染元件,該相位板安裝至該防 /可染7G件内。 如申請專利範圍第 — 卜「 項所奴相位板«系統,其 ^樣扣區段包含-樣品裝載件,該相位板安裝至該 樣品裝載件與該防污染元件之。 *装至 !ί; 17201216316 VII. Patent application scope: ,,, phase plate money system, in conjunction with - penetrating electron microscope, sub-including: f pumping 6, cavity 'adjacent to the sample section of the transmission electron microscope; and The unit transmits a phase plate through the pre-extracting airtight chamber to a 5 hr penetrating electron microscope. The phase plate system of the first aspect of the invention, wherein the pre-extracting airtight cavity is connected to a pump unit. I!: The phase plate loading system of item 2, wherein the independent pump unit or the pre-pumping pump unit of the transmissive electronic display mirror. 4 The phase plate loading system of claim 1, wherein the aperture is 埠. Χ 罝 罝 罝 罝 光谱 光谱 光谱 埠 埠 埠 埠 埠 埠 埠 埠 埠 埠 埠 光谱 光谱 光谱 光谱 光谱 光谱 光谱 光谱 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位A gate is widely spaced. 5. If the patent application scope is 苐1, the transmission positioning star-L phase plate loading system, in which. Then, the 兀匕 一 导 , , , , , , , , , , , , τ τ τ τ τ τ τ τ τ τ τ τ τ τ τ τ 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位 相位m cutting board, or - CD 16 201216316 兮传二, the phase plate loading system described in item 1, wherein the == bit unit comprises a motor with a precision of nanometer. The phase plate loading system of item 8 of the benefit range, wherein -i. The application of the fourth embodiment of the phase plate loading system of the eighth item, wherein the u and =r units further comprise a splitting rod coupled to the motor. The phase plate loading system of item 8, wherein the = transmission read unit further comprises a phase plate member, and the phase plate loading system according to the nth patent range of the motor, wherein the _ bit plate loader is loaded The phase plate. 1 The phase plate loading system of claim 1, wherein the phase plate, such as the control unit, monitors the position of the phase plate in the sample section. The phase plate loading system of claim 13, wherein the monitoring unit comprises a camera or a sensing component. ^ The phase plate loading system of item 1, comprising an anti-contamination component, the phase plate being mounted to the anti-stainable 7G piece. For example, the scope of the patent application - "the phase plate of the item" system, the sample button section contains a sample loading member, the phase plate is mounted to the sample loading member and the anti-pollution component. * Mounted to ! 17
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TWI557768B (en) * 2014-12-26 2016-11-11 財團法人工業技術研究院 Sample holding device for studying light-driven reactions and sample analysis method using the same
US9837244B2 (en) 2014-12-26 2017-12-05 Industrial Technology Research Insitute Sample holding device for studying light-driven reactions and sample analysis method using the same
CN107544121A (en) * 2017-09-22 2018-01-05 中国科学院生物物理研究所 A kind of phase panel assembly for transmission electron microscope imaging
CN107622934A (en) * 2017-09-22 2018-01-23 中国科学院生物物理研究所 A kind of phase-plate for transmission electron microscope imaging changes transfer device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI557768B (en) * 2014-12-26 2016-11-11 財團法人工業技術研究院 Sample holding device for studying light-driven reactions and sample analysis method using the same
US9837244B2 (en) 2014-12-26 2017-12-05 Industrial Technology Research Insitute Sample holding device for studying light-driven reactions and sample analysis method using the same
CN107544121A (en) * 2017-09-22 2018-01-05 中国科学院生物物理研究所 A kind of phase panel assembly for transmission electron microscope imaging
CN107622934A (en) * 2017-09-22 2018-01-23 中国科学院生物物理研究所 A kind of phase-plate for transmission electron microscope imaging changes transfer device
CN107622934B (en) * 2017-09-22 2024-04-12 中国科学院生物物理研究所 Phase plate replacement transfer device for transmission electron microscope imaging
CN107544121B (en) * 2017-09-22 2024-05-24 中国科学院生物物理研究所 Phase plate device for transmission electron microscope imaging

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