TW201137930A - Method for making transmission electron microscope grid - Google Patents

Method for making transmission electron microscope grid Download PDF

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Publication number
TW201137930A
TW201137930A TW99112614A TW99112614A TW201137930A TW 201137930 A TW201137930 A TW 201137930A TW 99112614 A TW99112614 A TW 99112614A TW 99112614 A TW99112614 A TW 99112614A TW 201137930 A TW201137930 A TW 201137930A
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Taiwan
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carbon nanotube
sheet
nanotube structure
support ring
carbon
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TW99112614A
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Chinese (zh)
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TWI416587B (en
Inventor
Li Qian
Li Fan
Liang Liu
Chen Feng
yu-quan Wang
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Beijing Funate Innovation Tech
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Abstract

The invention relates to a method for making a transmission electron microscope (TEM) grid. The method for making the TEM grid includes the steps of: providing a supporting ring and a sheet-shaped carbon nanotube structure preform; laying the sheet-shaped carbon nanotube structure on the supporting ring; cutting the sheet-shaped carbon nanotube structure preform into a predetermined sized sheet-shaped carbon nanotube structure; and fixing the sheet-shaped carbon nanotube structure to the supporting ring.

Description

201137930 六、發明說明: 【發明所屬之技術領域】 [0001] 本發明涉及一種透射電鏡微柵的製備方法’尤其涉及一 種基於奈米碳管的透射電鏡微栅的製備方法。 【先前技術】 , [0002] 在透射電子顯微鏡中,多孔碳支持膜(微柵)係用於承 • 載粉末樣品,進行透射電子顯微鏡高分辨像(HRTEM)觀 察的重要工具。隨著奈米材料研究的不斷發展,微柵在 奈米材料的電子顯微學表徵領域的應用曰益廣泛。 Ο [0003] 先前技術中,該應用於选射電夺顯微鏡的微柵通常係在 銅網或鎳網等金屬網格上覆蓋一層多孔有機膜,再蒸鍍 一層非晶碳膜製成的。然’當採用前述微栅對被測樣品 的透射電鏡高分辨像進行成份分析時,被測樣品設置於 非晶碳膜表面,位於被測樣品下方的金屬網格因其經常 含有較多雜質,如金屬氧化物等,對被測樣品成份分析 的干擾較大。 Ο [〇〇〇4] 自九十年代初以來,以奈米碳管(請參見Helical microtubules of graphitic carbon, Nature, Sum-io Iijima, vo 1 354,p56(1991))為代表的奈米材料 以其獨特的結構及性質引起了人們極大的關注。將奈米 碳管應用於微柵的製作,有利於降低金屬網格對被測樣 品成份分析的干擾。 【發明内容】 [0005] 有鑒於此’提供一種基於奈米碳管的透射電鏡微柵的製 備方法實為必要,所製備的透射電鏡微柵對被測樣品成 099112614 表單編號A0101 第3頁/共33頁 0992022308-0 201137930 份分析的干擾較小。 [0006] [0007] [0008] [0009] 2透射電鏡微柵的製備方法,包括以 供,奈米碳管結構預製體,鋪設二 2&官結構預製體於所述切環;按預定尺寸切宝,! 描片狀奈米碳管結構預製體,形成-片狀奈米碳管社 構’·以及固定所述片狀奈米碳管結構於所述支#環。、α 相較於先·術’本發明所提供的透㈣鏡微栅通過提 供-支撐環及-片狀奈米碳管結構預製體,將該片狀奈 米碳管結構預製體鋪設於所述支撐環,及將切割後的片 狀奈米碳管結構預製體固定於支撐環來製備,無需蒸鍍 過程,故,製備方法較為簡單。所製備的透射電鏡微栅 包括一支撐環及一片狀奈米碳管結構’片狀奈米碳管結 構週邊通過所述支撑環固定,無需金屬網格,且片狀奈 米碳管結構為純奈米碳管結構,可有效消除傳統微柵中 的位於被測樣品下方的金属網彳各對被測樣品成份分析時 的干擾,從而有利於提高绛用珠舉售鳞進行成份分析時 的精確度。 【實施方式】 下面將結合附圖對本發明透射電鏡微柵及其製備方法作 進一步的詳細說明。 請參閱圖1,本發明實施例提供一種透射電鏡微栅10。該 透射電鏡微柵10包括一支撐環102及一片狀奈米碳管結構 104。所述片狀奈米碳管結構104可為圓片狀,直徑約為3 毫米。所述片狀奈米碳管#構1()4的週邊通過所述支撑環 099112614 102固定。 表單編號Α0101 第4頁/共 33育 0992022308-0 9 9 201137930 [0010] ο 所述支,展1〇2用於固定所述片狀奈采碳管結構叫。所 述支樓環1〇2為圓形的環狀結構。所述支揮環102的直徑 與所述片^米碳營結構104的直徑基本相同,約為3毫 米。所述^環102圍成一通孔(圖未標),位於該通孔 處的片狀不'来碳管結構104懸空設置。所述支擇環102的 讨料V為金屬或㈣等。所述金属包括銅、翻或錄等。 所述支撑衣1〇2的截面(垂直於所述支撐環102所在的平 0截®),為方形、圓形、半圓形或梯形等形狀。優 選地’::切環1〇2具有一平整表面,該平整表面用於 與片兔管結構104賭合’此時,所述片狀奈米碳管 結構、切環1()2的平整表面為面接觸,從而可更好 地,不米夂管結構104於所述支撐環102。所述片 狀==結構1〇4可通過黏結劑、凡德瓦爾力、機械方 ▲,ΙΓ如意結㈣定於料祕環⑽。當採用 黏结社,固定時,所述支撐環102的表面可預先塗覆一 層黏然錢敦片狀奈米碳管結構1㈣ 設置有黏結劑的矣 ^ 〇 4固定時,路、實定。當採用凡德瓦爾力方 " . 述片狀奈米碳管結構1〇4可通過自 =有:::處理直接鋪設於所述支_。:。 :發性有機:Γ理方式固定時’所述有機溶劑優選為 設有片狀太+=,此時,可將揮發性有機溶劑滴落在鋪 不未碳音結構104的支撐環 有機溶劑㈣環1G2表面,在揮發性 .φ 不:炭&結構1 〇 4通過凡德瓦爾 力更緊,地貼合固定 =德3 。可以理解,_、μ 川2的表面,實現固定 102之間的固定| &奈米碳管結構1G4與所述支撐環 M疋並不限於上述方式。 099112614 表單編號A0101 0992022308-0 第5頁/共33頁 201137930 [0011] 固 本實施例中,所 月狀奈米碳管結構104通過機械方式 定於所述支撐環〗 。所述支撐環102為直徑3毫米的銅壞 。所述支撐環1〇2 J包括一圓環狀支撐環本體l〇2a和四個 延伸部102b。所什u 处片狀奈米碳管結構104固定於所述圓環 狀支撐環本體1〇2 和四個延伸部l〇2b之間。所述圓環狀 支撐環本體1 〇2ait 四個延伸部102b可為一體結構。所述 申P 〇2b的材料與所述圓環狀支撐環本體102a的材料 可相同或不同。優 贫選地,所述延伸部l〇2b的材料為具有 較好的彎折性能的 J付科’以可實現所述延伸部l〇2b朝支201137930 VI. Description of the Invention: [Technical Field of the Invention] [0001] The present invention relates to a method for preparing a transmission electron micro-gate, and particularly relates to a method for preparing a transmission electron micro-gate based on a carbon nanotube. [Prior Art], [0002] In a transmission electron microscope, a porous carbon support membrane (microgrid) is an important tool for carrying a powder sample and performing high-resolution image observation (HRTEM) observation of a transmission electron microscope. With the continuous development of nanomaterial research, microgrids have a wide range of applications in the field of electron microscopy characterization of nanomaterials. [0003] In the prior art, the micro-gate applied to the selective electro-acoustic microscope is usually formed by covering a metal mesh such as a copper mesh or a nickel mesh with a porous organic film and then vapor-depositing an amorphous carbon film. However, when the TEM is used to analyze the composition of the sample to be measured by the micro-gate, the sample to be tested is placed on the surface of the amorphous carbon film, and the metal mesh below the sample to be tested often contains more impurities. Such as metal oxides, etc., the interference of the analysis of the components of the sample to be tested is large. Ο [〇〇〇4] Nanomaterials represented by carbon nanotubes (see Helical microtubules of graphitic carbon, Nature, Sum-io Iijima, vo 1 354, p56 (1991)) since the early 1990s With its unique structure and nature, it has attracted great attention. The application of nano carbon tubes to the fabrication of microgrids is beneficial to reduce the interference of metal grids on the analysis of the components of the sample being tested. SUMMARY OF THE INVENTION [0005] In view of this, it is necessary to provide a method for preparing a TEM micro-gate based on a carbon nanotube. The prepared TEM micro-gate is used to measure the sample to 099112614. Form No. A0101 Page 3 / A total of 33 pages 0992022308-0 201137930 analysis of the interference is small. [0007] [0009] [0009] 2 TEM micromirror preparation method, comprising: a carbon nanotube structure preform, laying a 2 2 & official structure preform in the ring; according to a predetermined size Cut Bao,! Describe the sheet-shaped carbon nanotube structure preform, form a sheet-like carbon nanotube structure', and fix the sheet-like carbon nanotube structure to the branch # ring. The α-mirror micro-grid provided by the present invention is provided by the present invention by providing a support ring and a sheet-like carbon nanotube structure preform, and the sheet-shaped carbon nanotube structure preform is laid in the same manner. The support ring is prepared by fixing the cut sheet-shaped carbon nanotube structure preform to the support ring, and the evaporation method is not required, so the preparation method is relatively simple. The prepared TEM microgrid comprises a support ring and a sheet of carbon nanotube structure. The periphery of the sheet-like carbon nanotube structure is fixed by the support ring, no metal mesh is required, and the sheet-shaped carbon nanotube structure is The pure carbon nanotube structure can effectively eliminate the interference of the metal mesh in the traditional micro-grid under the sample to be tested, which is beneficial to improve the composition analysis of the bead. Accuracy. [Embodiment] Hereinafter, a TEM microgate of the present invention and a preparation method thereof will be further described in detail with reference to the accompanying drawings. Referring to FIG. 1, an embodiment of the present invention provides a TEM micro-gate 10. The TEM microgrid 10 includes a support ring 102 and a sheet of carbon nanotube structure 104. The sheet-like carbon nanotube structure 104 may be in the form of a disk having a diameter of about 3 mm. The periphery of the sheet-like carbon nanotube #1)4 is fixed by the support ring 099112614 102. Form No. 1010101 Page 4 / Total 33 Yu 0992022308-0 9 9 201137930 [0010] ο The support, the exhibition 1 〇 2 is used to fix the sheet-shaped carbon nanotube structure. The branch ring 1〇2 is a circular ring structure. The diameter of the fulcrum ring 102 is substantially the same as the diameter of the sheet carbon dam structure 104, which is about 3 mm. The ring 102 is surrounded by a through hole (not shown), and the sheet-shaped carbon tube structure 104 located at the through hole is suspended. The V of the selection ring 102 is metal or (four) or the like. The metal includes copper, turn or record, and the like. The cross section of the support garment 1 (perpendicular to the flat 0 of the support ring 102) is square, circular, semi-circular or trapezoidal. Preferably, the :::Cut ring 1〇2 has a flat surface for betting with the sheet rabbit tube structure 104. At this time, the sheet-like carbon nanotube structure and the tangent ring 1 () 2 are flattened. The surface is in surface contact so that the tube structure 104 is better than the support ring 102. The sheet shape == structure 1〇4 can be set in the material secret ring (10) by a binder, a van der Waals force, a mechanical side ▲, and a ruthenium knot (4). When the bonding mechanism is used, the surface of the support ring 102 may be pre-coated with a layer of sticky Qiandeng sheet-shaped carbon nanotube structure 1 (4) When the 矣 ^ 〇 4 provided with the bonding agent is fixed, the road is fixed. When the van der Waals side is used, the sheet-like carbon nanotube structure 1〇4 can be directly laid on the branch _ by the =:::: treatment. :. : Hairy organic: when the cleavage method is fixed, the organic solvent is preferably provided with a sheet shape too +=, and at this time, the volatile organic solvent may be dropped on the support ring organic solvent of the unbuffered carbon sound structure 104 (4) Ring 1G2 surface, in the volatile. φ No: charcoal & structure 1 〇 4 through the van der Waals force tighter, the ground fit fixed = de 3 . It is to be understood that the surface of the _, μ, 2, and the fixing between the fixings 102 and the support ring MG are not limited to the above. 099112614 Form No. A0101 0992022308-0 Page 5 of 33 201137930 [0011] In the present embodiment, the moon-shaped carbon nanotube structure 104 is mechanically defined by the support ring. The support ring 102 is a copper defect of 3 mm in diameter. The support ring 1〇2 J includes an annular support ring body 102a and four extensions 102b. The sheet-like carbon nanotube structure 104 is fixed between the annular support ring body 1〇2 and the four extensions 102a. The annular support ring body 1 〇 2ait four extensions 102b may be a unitary structure. The material of the P 2 b 2b may be the same as or different from the material of the annular support ring body 102a. Preferably, the material of the extension portion 〇2b is a J keke having a better bending property to enable the extension portion 〇2b to support

撐環102圓心(岁押 牙壤1 0,2所在圓'環的圓心)的方向的彎 折’進而固定片狀奈米碳管結構1G4於所述支擇環本體 102a與延伸部i〇2b之間。本實施例中的延伸部1〇2匕的材 料與支撐環本體l〇2a的材料相同,均為銅。可以理解, 所述延伸部l〇2b的數量並不限於四個,以可實現片狀奈 米碳管結構104較好地固定於所述支撐環本體1〇2&的表面 為準’根據所述延伸部l〇2b的面積,所述延伸部1〇21^的 數量可為一個或複數個。The center of the support ring 102 (bending in the direction of the center of the round ring of the 0'2), and then fixing the sheet-like carbon nanotube structure 1G4 to the support ring body 102a and the extension portion i〇2b between. The material of the extension portion 1〇2匕 in this embodiment is the same as the material of the support ring body 102a, and is copper. It can be understood that the number of the extensions 102b is not limited to four, so as to realize that the sheet-like carbon nanotube structure 104 is better fixed to the surface of the support ring body 1〇2& The area of the extension portion 102b, the number of the extension portions 1〇21^ may be one or plural.

[0012] 請一併參見圖2及圖3 ’所述延伸部1 〇2b從支撐學本體 102a向外延伸,其延伸方向為沿延伸處與支待5裏本體 102a所在圓環的圓心的連線方向即半徑方向。所述支^ 環本體102a可具有一平整表面l〇2c,所述延伸部1〇2]〇從 支撐環本體l〇2a的平整表面l〇2c沿半徑方向向外延伸。 優選地,所述延伸部l〇2b與所述支撐環本體1〇2&位於同 一平面内(參見圖2) ’或所述延伸部i〇2b所在的平面低 於所述支撐環本體l〇2a所在的平面(圖未示、 V。所述延 099112614 表單編號A0101 第6頁/共33頁 0992022308-0 201137930 Ο [0013] 伸部102b的厚度可小於或等於所述支撐環本體1〇2&的厚 度。優選地,所述延伸部1〇2b的厚度小於所述支撐環本 體102a的厚度。採用延伸部1021:)固定片狀奈米碳管結構 104時,可先將一片狀奈米碳管結構預製體直接舖設於所 述支撐環本體102a的平整表面l〇2c,然後按支撐環的形 狀即支樓環本體10 2 a外週沿切割所述片狀奈米碳管結構 預製體,形成片狀奈米碳管結構104,最後朝支樓環1〇2 圓心的方向彎折所述延伸部l〇2b,使其覆蓋位於支撐環 本體102a平整表面l〇2c的片狀奈米碳管結構1〇4,從而 實現片狀奈米碳管結構104固定於所學支撐環本體丨02a與 延伸部102b之間。 ❹ 所述片狀奈米碳官結構10 4用於支搶被測樣品用於透射電 鏡觀測。所述片狀奈米碳管結構104為一多孔結構,其具 有複數微孔106。所述微孔106可為通獨,即其可從片狀 奈米碳管結構1 〇 4的一個表面延伸至與該表面相對的另一 表面所述微孔106的形狀不限,可為圓形、方形、橢圓 形等。所述微孔106的尺寸不限,可根據實際應用需求調 整。所述微孔106的排列方式不限。所述微孔106之間的 距離玎相等或不等。優選地,所述微孔1 均勻分佈在所 述片狀奈米破管結構104表面或所述複數微孔106以陣列 形式分佈在所述片狀奈米碳管結構104表面’且相鄰的微 孔106之間的距離相等。相鄰的微孔106之間的距離可大 於1微米。所述微孔106的尺寸約為1微米〜200微来。所 述片狀奈來破管結構104為自支禮結構’且具有一定的支 樓性能。所述自支撐為片狀奈米碳管結構104不需要大面 0992022308-0 第7頁/共33頁 099112614 201137930 積的載體支撐,而只要相對兩邊提供支撐力即能一體上 懸空而保持自身片狀結構。所述片狀奈米碳管結構104為 純奈米碳管結構。所述片狀奈米碳管結構104可由至少一 奈米碳管線狀結構編織而成或由至少一奈米碳管膜組成 〇 [0014] 當所述片狀奈米碳管結構104包括複數奈米碳管線狀結構 時,所述複數奈米碳管線狀結構可平行、並排、交叉或 纏繞設置。具體地,所述複數奈米碳管線狀結構可採用 先前技術中的編織方法,如平紋編織或斜紋編織法來製 備所述片狀奈米碳管結構104。所述奈米碳管線狀結構可 由至少一奈米碳管線組成。所述奈米碳管線狀結構為複 數奈米碳管線平行設置組成的一束狀結構或複數奈米碳 管線相互扭轉組成的一絞線結構。所述奈米碳管線由複 數奈米碳管組成,所述奈米碳管線中多數奈米碳管係通 過凡德瓦爾力首尾相連。所述奈米碳管線可為一扭轉的 奈米破管線或一非扭轉的奈米碳管線。 [0015] 所述非扭轉的奈米碳管線包括複數沿該非扭轉的奈米碳 管線長度方向擇優取向排列的奈米碳管,其掃描電鏡照 片請參見圖4。非扭轉的奈米碳管線可通過將奈米碳管拉 膜通過有機溶劑處理得到。具體地,該奈米碳管拉膜包 括複數奈米碳管片段,該複數奈米碳管片段通過凡德瓦 爾力首尾相連,每一奈米碳管片段包括複數基本相互平 行並通過凡德瓦爾力緊密結合的奈米碳管。該奈米碳管 片段具有任意的長度、厚度、均勻性及形狀。該非扭轉 的奈米碳管線長度不限,直徑為〇. 5奈米-1毫米。具體地 099112614 表單編號A0101 第8頁/共33頁 0992022308-0 201137930 ❹ ,可將有機溶劑浸潤所述奈米碳管拉膜的整個表面,在 揮發性有機溶劑揮發時產生的表面張力的作用下,奈米 碳管拉膜中的相互平行的複數奈米碳管通過凡德瓦爾力 緊密結合,從而使奈米碳管拉膜收縮為一非扭轉的奈米 碳管線。該有機溶劑為揮發性有機溶劑,如乙醇、甲醇 、丙酮、二氣乙烷或氣仿,本實施例中採用乙醇。通過 有機溶劑處理的非扭轉奈米碳管線與未經有機溶劑處理 的奈米碳管膜相比,比表面積減小,黏性降低。所述奈 米碳管線及其製備方法請參見范守善等人於2002年11月5 日申請的,於2008年11月21日公告的第1303239號台灣 公告專利,及於2005年12月16日申請,於2009年7月21 日公告的第1312337號台灣公告專利。 [0016] 所述扭轉的奈米碳管線為採用一機械力將所述奈米碳管 拉膜兩端沿相反方向扭轉獲得。該扭轉的奈米碳管線包 括複數繞該扭轉的奈米碳管線軸向螺旋排列的奈米碳管 ,其掃描電鏡照片請參見圖5。進一步地,可採用一揮發 〇 性有機溶劑處理該扭轉的奈米碳管線。在揮發性有機溶 劑揮發時產生的表面張力的作用下,處理後的扭轉的奈 米碳管線中相鄰的奈米碳管通過凡德瓦爾力緊密結合, 使扭轉的奈米碳管線的比表面積減小,密度及強度增大 〇 [0017] 所述奈米碳管膜可為奈米碳管絮化膜、奈米碳管碾壓膜 或奈米碳管拉膜。 所述奈米碳管絮化膜包括複數相互纏繞且均勻分佈的奈 米碳管。所述奈米碳管之間通過凡德瓦爾力相互吸引、 099112614 表單編號Α0101 第9頁/共33頁 0992022308-0 [0018] 201137930 纏繞,形成網路狀結構,以形成一自支撐的奈米碳管絮 化膜,其掃描電鏡照片可參閱圖6。所述奈米碳管絮化膜 各向同性。所述奈米碳管絮化膜可通過對一奈米碳管陣 列絮化處理而獲得,具體可參見范守善等人於2007年5月 11日申請,並於2008年11月16日公開的第200844041號 台灣公開專利申請。為節省篇幅,僅引用於此,但所述 申請中的所有技術揭露亦應視為本發明申請技術揭露的 一部分。所述奈米碳管絮化膜並不限於上述製備方法。 所述奈米碳管絮化膜的厚度為1微米至2毫米。所述片狀 奈米碳管結構104可僅包括一層奈米碳管絮化膜,通過調 節其厚度來確保其具有較好的支撐性能。 [0019] 所述奈米碳管碾壓膜包括複數奈米碳管無序排列、沿一 個方向擇優取向排列或沿複數方向擇優取向排列,相鄰 的奈米碳管通過凡德瓦爾力結合。該奈米碳管碾壓膜可 通過採用一平面壓頭沿垂直於上述奈米碳管陣列生長的 基底的方向擠壓上述奈米碳管陣列而獲得,此時所述奈 米碳管碾壓膜t的奈米碳管無序排列,該奈米碳管碾壓 膜各向同性;所述奈米碳管碾壓膜亦可採用一滚軸狀壓 頭沿某一固定方向碾壓上述奈米碳管陣列而獲得,此時 所述奈米碳管碾壓膜中的奈米碳管在所述固定方向擇優 取向排列;所述奈米碳管碾壓膜還可採用滚軸狀壓頭沿 不同方向碾壓上述奈米碳管陣列而獲得,此時所述奈米 碳管碾壓膜中的奈米碳管沿不同方向擇優取向排列此時 ,所述奈米碳管碾壓膜可包括複數部分,每個部分中的 奈米碳管沿一個方向擇優取向排列,且相鄰兩個部分中 099112614 表單編號A0101 第10頁/共33頁 0992022308-0 201137930 Ο [0020] 〇 7奈米碳管的排列方向可不同。所述奈米碳管碾壓膜的 Ζ描電鏡照片請參閲圖7。所述奈米碳管碾壓膜的結構及 製備方法請參見范守善等人於2007年5月 〇Ππο . Μ 丫明,ji於 <年11月16曰公開的第·844〇41號台灣公開專利申 凊。為節省篇幅’僅引用於此’但所述申請中的所有技 術揭露亦應視為本發明申請技術揭露的一部分。所述的 奈米碳管碾廢膜的厚度為1微米至1毫米。所述片狀太米 =結構104可僅包括-層奈米碳管⑽膜,通過調"V其 厚X來實現其具有較好的支撐性能。 。月參見圖8 ’所述奈米碳管拉膜係由複數奈米碳管組成的 自支撑結構。所述複數奈米唉管沿同一方向擇優取向排 列。所述擇優取向仙在奈米碳錄财大多數奈米碳 管的一體延伸方向基本朝同一方向。而且,所述大多數 奈米碳管的—體延伸方向基本平行於奈米碳管拉膜的表 面。進-步地,所述奈求碳管拉膜中多數奈米碳管係通 過凡德瓦爾力首尾相連。具體地,所述奈米碳管拉膜中 基本朝同-方向延伸媒大多數奈米碳管中每—奈米碳管 與在L伸方向上相鄰的奈米碳管通過凡德瓦爾力首尾相 連H所述奈米碳㈣財存在少數隨卿列的奈 米碳管,該等奈米碳管^會對奈米碳錄财大多數奈 米碳管的-體取向排列構成明顯影響。所述自支樓為奈 米碳管拉膜不需要大面積的載體支#,而只要相對兩邊 提供支樓力即能-體上懸空而保持自身膜狀狀態,即將 該奈米碳管拉膜置於(或g^於)間隔—定距離設置的 兩個支樓體上時’位於兩個切體之間的奈米碳管拉膜 099112614 表單編號A0101 第11頁/共33頁 0992022308-0 201137930 能夠懸空保持自身膜狀狀態。所述自支撐主要通過奈米 碳管拉膜中存在連續的通過凡德瓦爾力首尾相連延伸排 列的奈米碳管而實現。 [0021] 具體地,所述奈米碳管拉膜中基本朝同一方向延伸的多 數奈米碳管並非絕對的直線狀,可適當的彎曲;或者並 非完全按照延伸方向上排列,可適當的偏離延伸方向。 故,不能排除奈米碳管拉膜的基本朝同一方向延伸的多 數奈米碳管中並列的奈米碳管之間可能存在部分接觸。 具體地,每一奈米碳管拉膜包括複數連續且擇優取向排 列的奈米碳管片段。該複數奈米碳管片段通過凡德瓦爾 力首尾相連。每一奈米碳管片段包括複數基本相互平行 的奈米碳管,該複數基本相互平行的奈米碳管通過凡德 瓦爾力緊密結合。該奈米碳管片段具有任意的長度、厚 度、均勻性及形狀。該奈米碳管拉膜中的奈米碳管沿同 一方向擇優取向排列。所述奈米碳管拉膜為從一奈米碳 管陣列中拉取獲得。根據奈米碳管陣列中奈米碳管的高 度與密度的不同,所述奈米碳管拉膜的厚度為0.5奈米 〜100微米。所述奈米碳管拉膜的寬度與拉取該奈米碳管 拉膜的奈米碳管陣列的尺寸有關,長度不限。 [0022] 當片狀奈米碳管結構1 04包括複數奈米碳管膜且每個奈米 碳管膜中的奈米碳管沿同一方向擇優取向排列時,相鄰 兩層奈米碳管膜中的奈米碳管的排列方向可相同或不同 。具體地,相鄰的奈米碳管膜中的奈米碳管之間具有一 交叉角度α,且該α大於等於0度且小於等於90度。當片 狀奈米碳管結構中的複數奈米碳管膜中的奈米碳管之間 099112614 表單編號Α0101 第12頁/共33頁 0992022308-0 201137930 具有-交叉角度ah不等於〇度時,即複數奈米碳管膜 交又設置時’所述奈^管相互交織職—網狀結構, 使所述片狀奈米碳管結構的機械性能增強。優選地,所 述複數奈米碳管膜交又設置。 [0023][0012] Please refer to FIG. 2 and FIG. 3 together. The extension portion 1 〇 2b extends outward from the support body 102a, and extends in the direction of the extension to the center of the circle of the body 102a in the support 5 The line direction is the radial direction. The support ring body 102a may have a flat surface 10c, and the extension portion 〇2] 向外 extends radially outward from the flat surface l2c of the support ring body 102a. Preferably, the extension portion 102b is located in the same plane as the support ring body 1〇2& (see FIG. 2) or the plane of the extension portion i2b is lower than the support ring body The plane in which 2a is located (not shown, V. The delay 099112614 Form No. A0101 Page 6 / Total 33 page 0992022308-0 201137930 Ο [0013] The thickness of the extension 102b may be less than or equal to the support ring body 1〇2&amp Preferably, the thickness of the extension portion 1 2b is smaller than the thickness of the support ring body 102a. When the extension portion 1021 :) is used to fix the sheet-shaped carbon nanotube structure 104, a piece of Nai Nai may be first The carbon nanotube structure preform is directly laid on the flat surface l〇2c of the support ring body 102a, and then prefabricated by cutting the sheet-shaped carbon nanotube structure according to the shape of the support ring, that is, the outer ring body 10 2 a Forming a sheet-like carbon nanotube structure 104, and finally bending the extension portion l2b in the direction of the center of the branch ring 1〇2 so as to cover the sheet-shaped navel located on the flat surface l〇2c of the support ring body 102a The carbon nanotube structure is 1〇4, so that the sheet-like carbon nanotube structure 104 is fixed to Studies support the body between the ring and the extending portion 02a Shu 102b. ❹ The sheet-like nano-carbon structure 10 4 is used to capture the sample to be used for transmission electron microscopy. The sheet-like carbon nanotube structure 104 is a porous structure having a plurality of micropores 106. The micropores 106 may be unobstructed, that is, they may extend from one surface of the sheet-shaped carbon nanotube structure 1 〇4 to the other surface opposite to the surface. The shape of the micropores 106 is not limited, and may be a circle Shape, square, oval, etc. The size of the micro-holes 106 is not limited and can be adjusted according to actual application requirements. The arrangement of the micropores 106 is not limited. The distances between the microholes 106 are equal or unequal. Preferably, the micropores 1 are evenly distributed on the surface of the sheet-like nanotube structure 104 or the plurality of micropores 106 are distributed in an array on the surface of the sheet-like carbon nanotube structure 104 and adjacent The distance between the microholes 106 is equal. The distance between adjacent microholes 106 can be greater than 1 micron. The size of the micropores 106 is about 1 micrometer to 200 micrometers. The sheet-like Nylon tube structure 104 is a self-supporting structure' and has certain branch performance. The self-supporting sheet-shaped carbon nanotube structure 104 does not require a large surface 0992022308-0 page 7 / a total of 33 pages 099112614 201137930 product carrier support, and as long as the support force is provided on both sides, it can be suspended in one piece to maintain its own piece Structure. The sheet-like carbon nanotube structure 104 is a pure carbon nanotube structure. The sheet-like carbon nanotube structure 104 may be woven from at least one nanocarbon line-like structure or composed of at least one carbon nanotube film. [0014] When the sheet-like carbon nanotube structure 104 includes a plurality of In the case of a rice carbon line-like structure, the plurality of carbon-carbon line-like structures may be arranged in parallel, side by side, crosswise or wound. Specifically, the plurality of nanocarbon line-like structures may be prepared by a prior art weaving method such as plain weave or twill weave to form the sheet-like carbon nanotube structure 104. The nanocarbon line-like structure may be composed of at least one nanocarbon line. The nanocarbon line-like structure is a stranded structure in which a plurality of carbon nanotubes are arranged in parallel, or a twisted line structure in which a plurality of nanocarbon pipelines are twisted to each other. The nanocarbon pipeline is composed of a plurality of carbon nanotubes, and most of the carbon nanotubes in the nanocarbon pipeline are connected end to end by van der Waals force. The nanocarbon line can be a twisted nano-crushed line or a non-twisted nanocarbon line. [0015] The non-twisted nanocarbon pipeline includes a plurality of carbon nanotubes arranged in a preferred orientation along the length direction of the non-twisted nanocarbon pipeline, and the scanning electron microscope photograph is shown in FIG. 4. The non-twisted nanocarbon line can be obtained by treating the carbon nanotube membrane with an organic solvent. Specifically, the carbon nanotube film comprises a plurality of carbon nanotube segments, and the plurality of carbon nanotube segments are connected end to end by Van der Waals force, and each of the carbon nanotube segments comprises a plurality of substantially parallel to each other and pass through Van der Waals A tightly coupled carbon nanotube. The carbon nanotube segments have any length, thickness, uniformity, and shape. The length of the non-twisted nanocarbon line is not limited, and the diameter is 奈. 5 nm - 1 mm. Specifically, 099112614 Form No. A0101 Page 8 of 33 0992022308-0 201137930 ❹ The organic solvent can be immersed in the entire surface of the carbon nanotube film, under the surface tension generated by the volatilization of volatile organic solvents. The mutually parallel plurality of carbon nanotubes in the carbon nanotube film are tightly bonded by the van der Waals force, thereby shrinking the carbon nanotube film into a non-twisted nano carbon line. The organic solvent is a volatile organic solvent such as ethanol, methanol, acetone, di-ethane or gas, and ethanol is used in this embodiment. The non-twisted nanocarbon line treated with the organic solvent has a smaller specific surface area and a lower viscosity than the carbon nanotube film which is not treated with the organic solvent. The nano carbon pipeline and its preparation method can be found in the patent application filed on November 5, 2002 by Fan Shoushan et al., published on November 21, 2008, and published on December 16, 2005. , Taiwan No. 1312337 announced on July 21, 2009 announced the patent. [0016] The twisted nanocarbon pipeline is obtained by twisting both ends of the carbon nanotube film in a reverse direction by a mechanical force. The twisted nanocarbon line comprises a plurality of carbon nanotubes arranged axially around the twisted nanocarbon line, and a scanning electron micrograph is shown in Fig. 5. Further, the twisted nanocarbon line can be treated with a volatile organic solvent. Under the action of the surface tension generated by the volatilization of volatile organic solvents, the adjacent carbon nanotubes in the treated twisted nanocarbon pipeline are tightly bonded by van der Waals force, so that the specific surface area of the twisted nanocarbon pipeline Decrease, increase density and strength 〇 [0017] The carbon nanotube film may be a carbon nanotube film, a carbon nanotube film or a carbon nanotube film. The carbon nanotube flocculation membrane comprises a plurality of carbon nanotubes intertwined and uniformly distributed. The carbon nanotubes are attracted to each other by van der Waals force, 099112614 Form No. Α0101 Page 9 / Total 33 Page 0992022308-0 [0018] 201137930 Winding, forming a network structure to form a self-supporting nano Carbon tube flocculation membrane, the scanning electron micrograph of which can be seen in Figure 6. The carbon nanotube flocculation membrane is isotropic. The carbon nanotube flocculation membrane can be obtained by flocculation treatment on a carbon nanotube array. For details, see Fan Shoushan et al., filed on May 11, 2007, and published on November 16, 2008. Taiwan Patent Application No. 200844041. To save space, reference is made only to this, but all technical disclosures in the application are also considered to be part of the disclosure of the present application. The carbon nanotube flocculation film is not limited to the above production method. The carbon nanotube film has a thickness of from 1 micrometer to 2 millimeters. The sheet-like carbon nanotube structure 104 may include only one layer of carbon nanotube flocculation film, and its thickness is ensured to ensure better support performance. [0019] The carbon nanotube rolled film comprises a plurality of carbon nanotubes arranged in disorder, arranged in a preferred orientation in one direction or in a preferred orientation in a complex direction, and adjacent carbon nanotubes are bonded by van der Waals force. The carbon nanotube rolled film can be obtained by extruding the carbon nanotube array in a direction perpendicular to the substrate grown by the array of carbon nanotubes by using a planar indenter, wherein the carbon nanotube is rolled. The carbon nanotubes of the membrane t are disorderly arranged, and the carbon nanotube membrane is isotropic; the carbon nanotube membrane can also be rolled by a roller-shaped indenter in a certain fixed direction. Obtained by the carbon nanotube array, wherein the carbon nanotubes in the carbon nanotube rolled film are arranged in a preferred orientation in the fixed direction; the carbon nanotube rolled film may also adopt a roller-shaped indenter Obtaining the above-mentioned carbon nanotube arrays in different directions, wherein the carbon nanotubes in the carbon nanotube rolled film are arranged in different directions in a preferred orientation. At this time, the carbon nanotube rolled film can be Including a plurality of parts, the carbon nanotubes in each part are arranged in a preferred orientation in one direction, and the adjacent two parts are 099112614 Form No. A0101 Page 10 / Total 33 Page 0992022308-0 201137930 Ο [0020] 〇 7 nm The arrangement of the carbon tubes can be different. See Figure 7 for a scanning electron micrograph of the carbon nanotube rolled film. For the structure and preparation method of the carbon nanotube rolled film, please refer to Fan Shoushan et al. in May 2007 〇Ππο. 丫 丫明, ji in the year of November 16th, the open 844〇41 Taiwan public Patent application. All of the technical disclosures in the application are also considered to be part of the disclosure of the present application. The carbon nanotube waste film has a thickness of from 1 micrometer to 1 millimeter. The sheet-like rice = structure 104 may include only a layer of carbon nanotube (10) film, which has better support properties by adjusting its thickness X. . Referring to Fig. 8 ', the carbon nanotube film is a self-supporting structure composed of a plurality of carbon nanotubes. The plurality of nanotubes are arranged in a preferred orientation along the same direction. The preferred orientation is substantially in the same direction as the integral extension direction of most of the carbon nanotubes in the nanocarbon recording. Moreover, the bulk extension direction of the majority of the carbon nanotubes is substantially parallel to the surface of the carbon nanotube film. Further, most of the carbon nanotubes in the carbon nanotube film are connected end to end by van der Waals force. Specifically, the carbon nanotube film is substantially oriented in the same-direction direction. Most of the carbon nanotubes in each of the carbon nanotubes and the carbon nanotubes adjacent in the direction of the L extend through the van der Waals force. There is a small number of carbon nanotubes in the N-carbon (four) of the end-to-end H. The carbon nanotubes have a significant influence on the body-orientation arrangement of most carbon nanotubes. The self-supporting building is a nano-carbon tube pulling film that does not require a large-area carrier branch #, and as long as the supporting force is provided on opposite sides, the body can be suspended and maintained in a self-membranous state, that is, the carbon nanotube film is pulled. Placed on (or g^) intervals - two distances set on the two branch body 'nano carbon tube film between two cut bodies 099112614 Form No. A0101 Page 11 / Total 33 Page 0992022308-0 201137930 Can be suspended to maintain its own membranous state. The self-supporting is mainly achieved by the presence of continuous carbon nanotubes extending through the ends of the van der Waals force through the carbon nanotube film. [0021] Specifically, most of the carbon nanotubes extending substantially in the same direction in the carbon nanotube film are not absolutely linear, and may be appropriately bent; or may not be arranged completely in the extending direction, and may be appropriately deviated. Extend the direction. Therefore, it is not possible to exclude partial contact between the carbon nanotubes juxtaposed in the majority of the carbon nanotubes extending substantially in the same direction. Specifically, each of the carbon nanotube drawn films includes a plurality of carbon nanotube fragments in a continuous and preferentially oriented arrangement. The plurality of carbon nanotube segments are connected end to end by Van der Waals force. Each of the carbon nanotube segments includes a plurality of substantially parallel carbon nanotubes, and the plurality of substantially parallel carbon nanotubes are tightly coupled by van der Waals force. The carbon nanotube segments have any length, thickness, uniformity, and shape. The carbon nanotubes in the carbon nanotube film are arranged in a preferred orientation along the same direction. The carbon nanotube film is obtained by drawing from a carbon nanotube array. The carbon nanotube film has a thickness of from 0.5 nm to 100 μm depending on the height and density of the carbon nanotubes in the carbon nanotube array. The width of the carbon nanotube film is related to the size of the carbon nanotube array for drawing the carbon nanotube film, and the length is not limited. [0022] When the sheet-like carbon nanotube structure 104 includes a plurality of carbon nanotube membranes and the carbon nanotubes in each of the carbon nanotube membranes are aligned in the same direction, the adjacent two layers of carbon nanotubes The arrangement of the carbon nanotubes in the film may be the same or different. Specifically, the carbon nanotubes in the adjacent carbon nanotube film have an intersection angle α between the α and the α is greater than or equal to 0 degrees and less than or equal to 90 degrees. When the carbon nanotubes in the sheet of carbon nanotubes are in the form of a number of carbon nanotubes between 099112614 Form No. Α0101 Page 12 of 33 0992022308-0 201137930 With a cross angle ah is not equal to 〇, That is to say, when the plurality of carbon nanotube membranes are disposed, the mechanical and electrical properties of the sheet-like carbon nanotube structure are enhanced. Preferably, the plurality of carbon nanotube membranes are disposed again. [0023]

[0024][0024]

[0025] # 099112614 可以理解’複數奈米碳管膜交又設置並不要求任意兩層 相鄰的奈米碳管膜均交以置,即允許存在相鄰㈣ς 来碳管膜中的多數奈米峻管的排列方向相同的情形但 優選片狀奈米碳管結構中存在至少兩層奈米碳管膜中的 多數奈米碳管的排列方向之間的交又角度大於0度且小於 等於90度。 本實施例中,所述透射電鏡微柵1〇由所述支撐環1〇2及片 狀奈米碳管結構104組成。該支撐環1〇2為銅環。所述片 狀奈米碳管結構104由複數奈米碳管線狀結構採用平紋編 織法製備。所述片狀奈米碳管結構1〇4的直徑為3毫米。 所述片狀奈米碳管結構104的週邊通過所述支撐環1〇2中 的支推環本體1 0 2 a及延伸部i'〇 2b固定。 本發明實施例提供的透射電鏡微柵丨〇由所述支撐環102及 片狀奈米碳管結構104組成,所述片狀奈米碳管結構104 僅週邊通過所述支撐環102支揮,無需金屬網格’且片狀 奈米碳管結構104為純奈米碳管結構,較為純淨’可有效 消除傳統微棚中位於被測樣品下方的金属網格對被測樣 品成份分析時的干擾,從而有利於提高採用透射電鏡微 柵10進行成份分析時的精確度。另,由於本實施例中的 透射電鏡微柵10中的片狀奈米碳管結構104被所述支撐環 102中的支撐環本體102a及延伸部丨〇21)固定’故’在使 表單編號A0101 第13頁/共33頁 0992022308-0 201137930 [0026] [0027] [0028] [0029] [0030] 099112614 用一鐵子等移動該透射電鏡微柵10時,鑷子可直接挾持 所述延伸部l〇2b ’避免鑷子與所述片狀奈米碳管結構1〇4 直接接觸’從而可避免由於片狀奈米碳管結構1〇4的質量 較輕而引起該片狀奈米碳管結構1〇4的飄移,同時亦減少 了鑷子對片狀奈米碳管結構104的污染,進而有利於提高 採用透射電鏡對樣品進行成份分析時的精確度及解析度 〇 本實施例透射電鏡微栅1〇在應用時,待觀察的材料樣品 承放在所述片狀奈米碳管結構104表面。當所述材料樣品 的尺寸大於所述片狀奈米碳管結構104的微孔106時所 C微孔10 6可支援该材料樣品。可通過微孔1 〇 6觀測該材 料樣品。而當所述材料樣品的尺寸小於所述微孔106時, ^##樣^可通過片狀奈米碳管結構1〇4中的奈米碳管 的吸附作用被穩定地吸附在奈米碳管管壁表面,此時, 亦可通過所述微孔106觀測該材料樣品。 . ;: ,: 明參閱圖9 ’本發明還提供一種上述透射電鏡微桃1〇的製 備方法,該方法可包括以下步驟· 步驟一:提供一支撐環1〇2。 102為圓%狀’其直徑約為3毫米。所述支撐 環102的截面可為方形 '圓形、半圓形或梯形等形狀。所 述支撐環1(32的材料可為金屬或陶-充等 。所述金屬包括銅 、鉬或鎳等。 本實施例中’所述支樓環1〇2為銅環,請參見圖2,所述 支撐環102包括-支撐環本體1()2&和四個延伸部。 頁 0992022308-0 表單編號A0101 第14頁/共33 201137930[0025] # 099112614 It can be understood that the 'multiple carbon nanotube film intersection and setting does not require any two adjacent layers of carbon nanotube film to be placed, that is, the existence of adjacent (four) ς to the carbon nanotube film Where the arrangement direction of the rice tube is the same, but it is preferable that the intersection angle between the arrangement directions of the plurality of carbon nanotubes in the at least two layers of the carbon nanotube film in the sheet-shaped carbon nanotube structure is greater than 0 degrees and less than or equal to 90 degrees. In this embodiment, the TEM micro-gate 1 is composed of the support ring 1〇2 and the sheet-shaped carbon nanotube structure 104. The support ring 1〇2 is a copper ring. The sheet-like carbon nanotube structure 104 is prepared by a plain weave method from a plurality of nanocarbon line-like structures. The sheet-like carbon nanotube structure 1〇4 has a diameter of 3 mm. The periphery of the sheet-like carbon nanotube structure 104 is fixed by the push ring body 1 0 2 a and the extension portion i' 2b in the support ring 1〇2. The TEM microgrid provided by the embodiment of the present invention is composed of the support ring 102 and the sheet-shaped carbon nanotube structure 104, and the sheet-shaped carbon nanotube structure 104 is only peripherally supported by the support ring 102. There is no need for a metal mesh 'and the sheet-shaped carbon nanotube structure 104 is a pure carbon nanotube structure, which is relatively pure', which can effectively eliminate the interference of the metal mesh under the sample under test in the traditional micro-shed to analyze the composition of the sample to be tested. Therefore, it is advantageous to improve the accuracy of component analysis using the TEM microgrid 10. In addition, since the sheet-shaped carbon nanotube structure 104 in the TEM microgrid 10 in the present embodiment is fixed by the support ring body 102a and the extension portion )21 in the support ring 102, the form number is made. A0101 Page 13 of 33 0992022308-0 201137930 [0028] [0030] [0030] When the TEM 10 is moved by a ferrite or the like, the raft can directly hold the extension L〇2b 'avoid the direct contact of the raft with the sheet-like carbon nanotube structure 1〇4' to avoid the sheet-like carbon nanotube structure caused by the light weight of the sheet-like carbon nanotube structure 1〇4 The drift of 1〇4 also reduces the contamination of the sheet-like carbon nanotube structure 104 by the scorpion, which is beneficial to improve the accuracy and resolution of the composition analysis of the sample by transmission electron microscopy. When applied, the sample of material to be observed is placed on the surface of the sheet-like carbon nanotube structure 104. When the size of the material sample is larger than the micropores 106 of the sheet-like carbon nanotube structure 104, the C micropores 106 can support the material sample. The material sample can be observed through the microwell 1 〇 6 . When the size of the material sample is smaller than the micropores 106, the ^## sample can be stably adsorbed on the nanocarbon through the adsorption of the carbon nanotubes in the sheet-like carbon nanotube structure 1〇4. The surface of the tube wall, at which point, the material sample can also be observed through the microholes 106. The invention also provides a method for preparing the above-mentioned TEM micro-peach, which may include the following steps: Step 1: Provide a support ring 1〇2. 102 is a round % shape having a diameter of about 3 mm. The cross section of the support ring 102 may be in the shape of a square 'circular, semi-circular or trapezoidal shape. The material of the support ring 1 (32 may be metal or ceramic-charged, etc. The metal includes copper, molybdenum or nickel, etc. In the embodiment, the branch ring 1〇2 is a copper ring, see Fig. 2 The support ring 102 includes a support ring body 1 () 2 & and four extensions. Page 0992022308-0 Form No. A0101 Page 14 of 33 201137930

所述支標環本體102a和四個延伸部l〇2b可為—體結構。 所述支撐環本體l〇2a可具有一平整表面102c。所述延伸 部102b從支撐環本體102a的平整表面102c向外延伸,其 延伸方向為沿延伸處與支撐環本體1 〇 2 a所在圓環的圓心 的連線方向即半徑方向。優選地,所述延伸邹1〇2b與支 撐環本體102a位於同一平面内。所述延伸部1〇2b的材料 優選為具有較好的彎折性能的材料,以可實現所述延伸 部102b朝支撐環本體102a圓心(支撐環本體l〇2a所在圓 環的圓心)的方向的彎折,進而固定片狀奈米碳管結構 104於所述支撐環本體102a與延伸部102b之間。本實施 例中的延伸部l〇2b的材料與支撐環本體i〇2a的材料相同 ,均為銅。 [0031]步驟二:提供一片狀奈米碳管結構預製體,鋪設所述片 狀奈来碳管結構預製體於所述支撐環1〇2。 [0032] Ο [0033] 所述片狀奈米碳管結構預製體可由至少一奈米碳管線狀 - ;; ·-. ./ ί ' i; 結構編織而成或由至少一奈米碳管膜組成、 所述不米&管膜可為至少_奈米碳管拉膜、—奈米碳管 礙壓膜或-奈来碳管絮化膜。當所述片狀奈米碳管結構 ;π*碳管拉賴成時,所述#狀奈米碳管 結構預製體可通過對魏奈米碳管㈣層疊且交叉設置 而屯成。該奈米碳管拉膜為您— _ 、…從—不、米碳管陣列中直接乾 抽取獲得至少-且# ” <切奈純管陣列中 有—疋寬度和長度的奈米碳管膜。 099112614 表單編號Α0]ίΗ 第】5頁/共33頁 0992022308-0 201137930 [0034] 所述層疊且交叉設置複數奈轉管拉Μ㈣可具體包 括以下步驟.贫先,提供―基體。該基底具有-平整表 面,其材料不限。本實施例中 該基底可為一陶瓷片》 其次’將上述奈米碳管㈣依次層#且交錢設在所述 基體表面。由於奈米礙管㈣純淨且具有較大的比表面 [0035] 積’故從奈米碳管陣職接拉取獲得的奈米碳管拉膜具 有較好的純。所述奈米碳管_可直制設在基體表 面或另-奈米碳管拉臈表面。所謂層疊且交叉設置即在 層疊設置的奈米碳管拉財,賴奈切管拉膜中的夺 米碳管之間具有一交又角度…不等於〇度。相鄰兩層 奈未碳管拉膜之間通過凡德瓦爾力緊密結合。 所述奈米碳管線狀結構可由至少_奈米碳管線組成。當 所达奈米碳管線狀結構由複數奈料管線組成時,所述 奈米礙管驗結構為複數奈㈣管線平行設置組成的一 束狀結構或複數奈米碳管線相互扭轉組成的—絞線結構 。所述奈米碳管線由複數餐被管崎,所述奈米碳管 線中多數Μ碳管料軌德瓦_力首助連。所述奈 未碳官線可為—扭轉的奈米碳管線或-非扭轉的奈米碳 管線。所述片狀奈米碳管結構預製體可由複數奈来碳管 線狀結構採用平紋編織法編織而形。 [0036] L 丁、米碳管結構預製體由複數奈米 碳管線狀結構採用平紋編織法編織而成。所述奈米碳管 線狀結構包括複數奈米碳管線平行設置組成的一束狀結 構。所述奈Μ管線及其製備方法請參見訪善等人於 2002年11月5日巾請的,㈣叫U州日公告的第 099112614 表單編號Α0101 第16頁/共33頁 0992022308-0 201137930 1303239銳台灣公告專利,及於2005年12月16日申請, 於2009年7月21日公告的第1312337號台灣公告專利。 [0037] 所述片狀奈米碳管結構預製體可直接鋪設在所述支撐環 1〇2表面。當所述支撐環102具有一平整表面時,所述片 、米碳s結構預製體可直接鋪設在所述支撑環1〇2的平 本實施例中,所述片狀奈米碳管結構預製體可 述支撐環本體102a的平絲面l〇2c。 [0038] G [0039] 乂驟一.按預定尺寸切割所述片狀奈米碳管結構預製體 ’形成所迷片狀奈米碳管結構104。 ❹ 所述按預定尺寸切割所述片狀奈米碳管結構預製體的步 驟具體包括以下步驟:提供_聚焦雷射光束;將該聚焦 雷射光束照射至所述片狀奈米碳管結構預製體表面;以 及按照支撑環的形狀即支撐環本體102a外週沿進行切割 ,切割後的片狀奈米碳管結構104的週邊通過所述支撐環 102支擇’片狀奈米碳管結構的中心部分懸空設置。具體 地’所述片狀奈米碳管結構104的週邊固定於所述支撐環 本體102a與至少一延伸部1021)之間。本實施例中,雷射 光束可通過傳統的氬離子雷射器或二氧化碳雷射器產生 ’其功率為5〜30瓦(W),優選為18W。具體地,該雷射光 束可通過一透鏡聚焦後從正面直接照射在上述片狀奈米 碳管結構預製體表面,可以理解,該雷射光束可採用垂 直照射或傾斜照射聚焦於所述片狀奈米碳管結構預製體 表面。所述片狀奈米碳管結構預製體可吸收雷射光束的 能量從而與空氣中的氧發生反應並分解,從而使具有預 定尺寸的片狀奈米碳管結構預製體與其他部分斷開❶本 099112614 表單編衆A0101 第17頁/共33頁 0992022308-0 201137930 實施例中,切刻後所形成的片狀奈米碳管結構1 〇 4為圓片 狀,其週邊固定於所述支撐環本體l〇2a與至少一延伸部 1〇2b之間,所形成的片狀奈米碳管結構104的直徑約為3 毫米。 [0040] 上迷切割步驟"5Γ採用固定所述片狀奈米碳管結構預製體 ’移動雷射光束;或固定雷射光束,移動所述片狀奈米 碳營結構預製體的方式來實現。本實施例並不限於上逑 雷射處理方法,先前技術中的其他方法,如物理或化學 蝕刻法,同樣玎用於切割所述片狀奈米碳管結構預製體 [0041] [0042] [0043] [0044] 099112614 步驟四:固定所述片狀奈米碳管結構1〇4於所述支柃 1〇2 〇 牙 ^迷片狀奈米碳管結構1〇4可通過黏結劑、凡德瓦爾力 於用機械方式,或上述任意兩種或多種方式的結 於所述支撐環1〇2。 弋 2 —結劑方式_時’進_步包括在铺設所述 結構預製•所収撐環表蚊前,塗覆1 碳管結構預製體,形成二::在切割所述片狀奈米 化所述黏結劑,進而固定㈣結構1〇4之後, 述支細2。結構叫 =用凡紅爾力方•定時,料Μ奈米 1〇4可通過自身的純或通過有機溶劑處理直接鋪設於 述支撲環1G2的表面1採时機溶财理方式固定時 第18 表單編號A0101 頁/共33頁 環 201137930 [0045] Ο [0046]The support ring body 102a and the four extensions 102b may be in a body structure. The support ring body 102a may have a flat surface 102c. The extending portion 102b extends outward from the flat surface 102c of the support ring body 102a in a radial direction along a line connecting the center of the circle where the support ring body 1 〇 2 a is located. Preferably, the extension is in the same plane as the support ring body 102a. The material of the extending portion 1〇2b is preferably a material having a good bending property, so that the extending portion 102b can be oriented toward the center of the support ring body 102a (the center of the ring in which the ring body l〇2a is supported). The bending is performed to fix the sheet-like carbon nanotube structure 104 between the support ring body 102a and the extending portion 102b. The material of the extension portion 〇2b in this embodiment is the same as that of the support ring body i 〇 2a, and is copper. [0031] Step 2: Providing a sheet-shaped carbon nanotube structure preform, and laying the sheet-shaped carbon nanotube structure preform on the support ring 1〇2. [0033] The sheet-like carbon nanotube structure preform may be woven from at least one nanocarbon line-like structure; or by at least one carbon nanotube The film composition, the non-meter & tube film may be at least a carbon nanotube film, a carbon nanotube film or a carbon nanotube film. When the sheet-like carbon nanotube structure; the π* carbon tube is laminated, the #-shaped carbon nanotube structure preform can be formed by laminating and cross-setting the Weinermi carbon tubes (four). The carbon nanotube film is obtained from - _, ... from - no, directly extracted from the carbon nanotube array to obtain at least - and # ” < Chennai pure tube array with - 疋 width and length of carbon nanotubes 099112614 Form No. Α0] Η 】 】 】 】 】 】 】 】 】 】 】 920 920 920 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠 层叠Having a flat surface, the material of which is not limited. In this embodiment, the substrate can be a ceramic sheet. Secondly, the above-mentioned carbon nanotubes (four) are sequentially layered and disposed on the surface of the substrate. Pure and has a large specific surface [0035] product, so the carbon nanotube film obtained from the carbon nanotube array is better. The carbon nanotubes can be directly fabricated. The surface of the substrate or the surface of the other carbon nanotubes is pulled. The so-called stacking and cross-setting means that the carbon nanotubes are stacked in a stack, and the carbon nanotubes in the Lai Nai tube are in an angle and angle... It is equal to the twist. The adjacent two layers of Naibi carbon tube are tightly bonded by van der Waals force. The nanocarbon pipeline-like structure may be composed of at least a nanocarbon pipeline. When the nanocarbon carbon pipeline-like structure is composed of a plurality of nanocomb pipelines, the nano-barrier inspection structure is composed of a plurality of parallel (four) pipelines. a bundle structure or a plurality of nano carbon pipelines twisted to each other to form a twisted wire structure. The nano carbon pipeline is composed of a plurality of meals, and most of the carbon nanotubes in the nano carbon pipeline are dewa The first carbon support line may be a twisted nano carbon line or a non-twisted nano carbon line. The sheet carbon nanotube structure preform may be made of a plain natrile carbon line structure using plain weave. The weaving method is woven and shaped. [0036] The L-butyl and carbon-carbon tube structure preforms are woven by a plurality of carbon-carbon pipeline structures by plain weave. The nano-carbon line-like structure includes a plurality of carbon carbon pipelines arranged in parallel. A bundle of structures consisting of the naphtha pipeline and its preparation method can be found in the visit of the person who visited the company on November 5, 2002, (4) the number 099112614 of the U state announcement. Form No. 1010101 Page 16 / Total 33 pages 0992022308-0 201137930 1303239 Rui Taiwan Announces Patent, and applied for on December 16, 2005, Taiwan Patent No. 1312337 announced on July 21, 2009. [0037] The sheet-shaped carbon nanotube structure preform can be directly laid in the office. The surface of the support ring 1 〇 2. When the support ring 102 has a flat surface, the sheet, the carbon s structure preform can be directly laid in the flat embodiment of the support ring 1 〇 2, The sheet-shaped carbon nanotube structure preform may be described as a flat surface of the support ring body 102a. [0038] [0039] Step 1. Cutting the sheet-shaped carbon nanotube structure preform by a predetermined size The sheet-like carbon nanotube structure 104 is formed. The step of cutting the sheet-shaped carbon nanotube structure preform according to a predetermined size specifically includes the steps of: providing a focused laser beam; and irradiating the focused laser beam to the sheet-shaped carbon nanotube structure prefabrication a body surface; and cutting according to the shape of the support ring, that is, the outer circumference of the support ring body 102a, and the periphery of the cut sheet-shaped carbon nanotube structure 104 is controlled by the support ring 102 to form a sheet-like carbon nanotube structure. The center part is suspended. Specifically, the periphery of the sheet-like carbon nanotube structure 104 is fixed between the support ring body 102a and the at least one extension portion 1021). In this embodiment, the laser beam can be generated by a conventional argon ion laser or carbon dioxide laser having a power of 5 to 30 watts (W), preferably 18 watts. Specifically, the laser beam can be directly focused on the surface of the sheet-like carbon nanotube structure preform by focusing on a lens, and it can be understood that the laser beam can be focused on the sheet by vertical illumination or oblique illumination. Nano carbon tube structure preform surface. The sheet-shaped carbon nanotube structure preform can absorb the energy of the laser beam to react with and decompose the oxygen in the air, thereby breaking the sheet-shaped carbon nanotube structure preform having a predetermined size from the other portions. Ben 099112614 Form Editor A0101 Page 17 / Total 33 Page 0992022308-0 201137930 In the embodiment, the sheet-like carbon nanotube structure 1 〇4 formed after dicing is in the form of a disk, and the periphery thereof is fixed to the support ring Between the body 10a and the at least one extension 1 2b, the sheet-like carbon nanotube structure 104 is formed to have a diameter of about 3 mm. [0040] The above-described cutting step "5Γ is to fix the sheet-shaped carbon nanotube structure preform to 'move the laser beam; or to fix the laser beam, and move the sheet-shaped nanocarbon camp structure preform to achieve. This embodiment is not limited to the upper laser processing method, and other methods in the prior art, such as physical or chemical etching, are also used to cut the sheet-like carbon nanotube structure preform [0041] [0042] 0043] [0044] 099112614 Step 4: Fixing the sheet-like carbon nanotube structure 1〇4 in the support 〇1〇2 〇牙^迷片状碳碳管结构1〇4 can pass the bonding agent, where Deval force is attached to the support ring 1〇2 by mechanical means, or any two or more of the above.弋2—The method of _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ After the bonding agent is further fixed to the (four) structure 1〇4, the thin portion 2 is described. The structure is called = use the red lyrics. • Timing, the material ΜNan 1〇4 can be directly laid on the surface of the 1G2 by the pure or through the organic solvent treatment. 1 When the time is dissolved, the financial method is fixed. 18 Form No. A0101 Page / Total 33 Pages Ring 201137930 [0045] Ο [0046]

合在奈米破·管線狀結構表面 104包括複數奈米碳管拉膜, 099112614 第19頁/共33 表單編號A0101 0992022308-0 所述有機溶劑優選為揮發性有機溶劑,此時, 性有機溶劑祕在鋪設有片狀奈米碳管結㈣4的支^ 叱表面,在揮發性有機溶劑的作用下,#狀奈米碳/ 構m通過凡德瓦爾力更緊密地貼合固定在所述切二結 102的表面’實現固^。可以理解,所述片狀奈“二 構104與所述支撐環102之間的固定並不限於上述方式:。 本實施例中,可通過將所述四個延伸部1G2b朝支撑幻〇 圓心的方向彎折,使其覆蓋位於支樓環本體1Q2a的平整 表面102c的片狀奈米碳管結構1()4,來實現片狀奈米碳缺 結構104固定於所述支播環本體丨…與四個延伸則官 之間。 進-步地,可採用有機溶劑處理所述片狀奈米碳管結構 預製體或>1狀奈米碳管結構1〇4的步驟丨該有機溶創為常 溫下易揮發的有機溶劑,可選用乙醇、曱醇、兩鲷、‘二* 氯乙烧和氣仿中-種或者幾種的混合,♦實施例中的: 機溶劑採用乙醇。該有機溶劑應與該奈米碳管具有較好 的潤濕性。該使用有機溶劑處理的步驟具體為:通過嗲 管將有機溶劑贿在片狀奈米碳管結構預製體或片狀: 米碳管結構1G4表面,或將固^後的片狀奈米碳管^ 104與支撐壞1〇2浸入盛有有機溶劑的容器中浸潤。有機 溶劑處理後’片狀奈米碳管結構預製體或片狀奈米碳管 結構104中部分相鄰的奈来碳管會聚集形成奈米碳管束, 片狀奈米碳管線狀結構表面財自由端的奈米碳管會貼 當所述片狀奈米碳管結構 且相鄰兩層奈米碳管拉膜中 頁 201137930 的奈米碳管具有一交叉角度α,且0<α $90。時,有機溶 劑處理後的奈米碳管拉膜中的奈米碳管束相互交 而形成複數微孔106。該微孔106的尺寸小於1〇微米可 以理解,進一步地,通過有機溶劑處理還可使該片狀夬 米碳管結構預製體或片狀奈米碳管結構1〇4與支撐環 結合緊密’從而使該片狀奈米碳管結構預製體或片狀齐 米碳管結構104更牢固地固定在該支撐環1〇2上。 [0047] 可以理解,上述步驟可通過鋪設一較大尺寸的片狀夬米 碳管結構預製體於複數支撐環102表面,並按支撑環1〇2 的形狀即支撐環本體的外週沿切割所述片狀奈米碳 管結構預製體,來實現快速批量生產透射電鏡微柵1〇。 [0048] 本發明實施例提供的透射電鏡微柵及其製備方法具有以 下優點:其一,所述透射電鏡微柵由一支撐環及—片狀 奈米碳管結構組成’片狀奈米碳管結構僅週邊通過所述 支撐環固定,無需金屬網格,且片狀奈米碳管結構為純 奈米碳管結構,可有效诮除傳統微柵中的位於被測樣品 下方的金屬網格對被測樣品成份分時的干擾,從而有 利於提高採用透射電鏡進行成份分析時的精確度。其二 ’由於本發明實施例透射電鏡微柵中的片狀奈米碳管結 構被所述支撐環中的支撐環本體及延伸部固定,故,在 使用鑷子等移動該透射電鏡微栅時,鑷子可直接挾持所 述延伸部’避免鑷子與所述片狀奈米碳管結構直接接觸 ’從而可避免由於片狀奈米碳管結構的質量較輕而引起 該片狀奈米石炭官結構的飄移,同時亦減少了録子對片狀 奈米碳管結構的污染,進而有利於提高採用透射電鏡對 099112614 表單編號A0101 第20頁/共33頁 0992022308-0 201137930 樣品進行成份分析時的精確度及解析度β其三,本發明 實施例提供的透射電鏡微柵通過提供一支摟環及一片狀 奈米礙管結構預製體’將該片狀奈米碳管結構預製體鋪 設於支撐環,及將切割後的片狀奈米碳管結構預製體固 定於支撐環來製備,無需蒸鍍過程,故,製備方法較為 簡單。 [0049] Ο [0050] [0051] [0052] ❾ [0053] [0054] [0055] 099112614 綜上所述,本發明確已符合發明專利之要件,遂依法提 出專利申請。惟,以上所述者僅為本發明之較佳實施例 ,自不能以此限制本案之申請專利範圍。舉凡習知本案 技藝之人士援依本發明之精神所作之等效修飾或變化, 皆應涵蓋於以下申請專利範圍内。 【圖式簡單說明】 圖1為本發明實施例透射電鏡微柵的立體結構示意圖。 圖2為本發明實施例透射電鏡板栅中的支撐環的立體結構 示意圖。 圖3為本發明實施例逸射電鏡微栅中的支撐環的剖視結構 示意圖。 圖4為本發明實施例透射電鏡微柵中的非扭轉的奈米碳管 線的掃描電鏡照片。 圖5為本發明實施例透射電鏡微栅中的扭轉的奈米碳管線 的掃描電鏡照片。 圖6為本發明實施例透射電鏡微柵中的奈米碳管絮化膜的 掃描電鏡照片。 0992022308-0The organic solvent is preferably a volatile organic solvent. In this case, the organic solvent is a volatile organic solvent. The organic solvent is preferably a volatile organic solvent. The organic solvent is preferably a volatile organic solvent. The secret surface is covered with a sheet of carbon nanotubes (4) 4, and under the action of a volatile organic solvent, the #nano-carbon/structure m is more closely attached to the cut by the van der Waals force. The surface of the second junction 102 is 'implemented'. It can be understood that the fixing between the two-dimensional structure 104 and the support ring 102 is not limited to the above manner: In this embodiment, the four extensions 1G2b can be moved toward the center of the support illusion The direction is bent so as to cover the sheet-shaped carbon nanotube structure 1 () 4 located on the flat surface 102c of the branch ring body 1Q2a, so as to realize that the sheet-like nano-carbon-deficient structure 104 is fixed to the support ring body... Further, between the four extensions, the step of treating the sheet-shaped carbon nanotube structure preform or the >-type carbon nanotube structure 1〇4 with an organic solvent may be further carried out. For the organic solvent which is volatile at normal temperature, ethanol, decyl alcohol, hydrazine, 'di*chloro chloroethene and gas imitation type or a mixture of several kinds may be used. ♦ In the embodiment: the organic solvent is ethanol. It should have good wettability with the carbon nanotubes. The step of treating with an organic solvent is specifically: bribing the organic solvent through the fistula tube in a sheet-like carbon nanotube structure preform or sheet: carbon nanotube structure 1G4 surface, or immersed in the sheet of carbon nanotubes ^ 104 and support bad 1 〇 2 The organic solvent is infiltrated in the container. After the organic solvent treatment, the partially adjacent carbon nanotubes in the sheet-like carbon nanotube structure preform or the sheet-shaped carbon nanotube structure 104 will aggregate to form a carbon nanotube bundle, and the sheet-shaped nai The carbon nanotubes on the surface of the carbon-carbon line-like structure will be attached to the carbon nanotube structure of the sheet and the carbon nanotubes of the adjacent two layers of carbon nanotubes have a cross angle α of 201137930. And 0 < α $90. The carbon nanotube bundles in the organic carbon nanotube-treated carbon nanotube film cross each other to form a plurality of micropores 106. The size of the micropores 106 is less than 1 μm. Further, The sheet-like carbon nanotube structure preform or the sheet-shaped carbon nanotube structure 1〇4 can be tightly combined with the support ring by the organic solvent treatment, so that the sheet-shaped carbon nanotube structure is prefabricated or sheet-shaped. The carbon nanotube structure 104 is more firmly fixed to the support ring 1〇2. [0047] It can be understood that the above steps can be prefabricated on the surface of the plurality of support rings 102 by laying a larger-sized sheet-shaped carbon nanotube structure. And according to the shape of the support ring 1〇2, that is, the support ring The outer peripheral edge of the body is cut along the sheet-shaped carbon nanotube structure preform to realize rapid mass production of the transmission electron microstrip micro-gate. The TEM micro-gate provided by the embodiment of the invention and the preparation method thereof have the following advantages In the first embodiment, the TEM microgrid is composed of a support ring and a sheet-like carbon nanotube structure. The sheet-like carbon nanotube structure is only fixed by the support ring, and no metal mesh is needed, and the sheet-shaped nai The carbon nanotube structure is a pure carbon nanotube structure, which can effectively eliminate the interference of the metal grid under the sample under the sample in the traditional micro-grid on the time-division of the sample to be tested, thereby facilitating the component analysis by TEM. The accuracy of the time. Second, because the sheet-like carbon nanotube structure in the TEM microgrid is fixed by the support ring body and the extension in the support ring, the transmission is transmitted by using a tweezers or the like. When the micromirror is micromirror, the tweezers can directly hold the extension portion to avoid direct contact between the tweezers and the sheet-like carbon nanotube structure, thereby avoiding the light weight of the sheet-like carbon nanotube structure. The drift of the sheet-like nano-charcoal official structure also reduces the pollution of the sheet-like carbon nanotube structure, which is beneficial to the improvement of the transmission electron microscope pair 099112614 Form No. A0101 Page 20 / Total 33 Page 0992022308-0 201137930 Accuracy and resolution of the sample in the composition analysis β Third, the TEM microgrid provided by the embodiment of the present invention provides a 搂 ring and a piece of nano-barrier structure pre-formed 'the flaky nano The carbon tube structure prefabricated body is laid on the support ring, and the cut sheet-shaped carbon nanotube structure preform is fixed on the support ring to prepare, and the evaporation process is not required, so the preparation method is simple. In summary, the present invention has indeed met the requirements of the invention patent and has filed a patent application in accordance with the law. [0055] [0055] However, the above description is only a preferred embodiment of the present invention, and it is not possible to limit the scope of the patent application of the present invention. Equivalent modifications or variations made by those skilled in the art in light of the spirit of the invention are intended to be included within the scope of the following claims. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic perspective view showing the structure of a transmission electron microscope micro-gate according to an embodiment of the present invention. 2 is a perspective view showing the structure of a support ring in a TEM grid according to an embodiment of the present invention. 3 is a cross-sectional view showing the structure of a support ring in an electron microscope microgrid according to an embodiment of the present invention. 4 is a scanning electron micrograph of a non-twisted carbon nanotube wire in a TEM microgrid according to an embodiment of the present invention. Figure 5 is a scanning electron micrograph of a twisted nanocarbon line in a TEM microgrid according to an embodiment of the present invention. Fig. 6 is a scanning electron micrograph of a carbon nanotube flocculation film in a TEM microgrid according to an embodiment of the present invention. 0992022308-0

表單編號 AGIDI % 21 33 S 201137930 [0056] 圖7為本發明實施例透射電鏡微栅中的奈米碳管碾壓膜的 掃描電鏡照片。 [0057] 圖8為本發明實施例透射電鏡微柵中的奈米碳管拉膜的掃 描電鏡照片。 [0058] 圖9為本發明實施例透射電鏡微柵的製備方法的流程示意 圖。 【主要元件符號說明】 [0059] 透射電鏡微栅:10 [00601 支撐環:102 [0061] 支撐環本體:102a [0062] 延伸部:102b [0063] 片狀奈米碳管結構:104 [0064] 微孔:106 099112614 表單編號A0101 第22頁/共33頁 0992022308-0Form No. AGIDI % 21 33 S 201137930 [0056] FIG. 7 is a scanning electron micrograph of a carbon nanotube rolled film in a transmission electron microstrip micro-gate according to an embodiment of the present invention. 8 is a scanning electron micrograph of a carbon nanotube film drawn in a transmission electron microscope micro-gate according to an embodiment of the present invention. 9 is a schematic flow chart showing a method of fabricating a TEM microgate according to an embodiment of the present invention. [Main component symbol description] [0059] Transmission electron microstrip: 10 [00601 Support ring: 102 [0061] Support ring body: 102a [0062] Extension: 102b [0063] Sheet-shaped carbon nanotube structure: 104 [0064] Micropores: 106 099112614 Form No. A0101 Page 22 of 33 0992022308-0

Claims (1)

201137930 七、申請專利範圍: 1 . 一種透射電鏡微柵的製備方法,包括以下步驟. 提供-支撐環,· ’ 二預:二::::預製體,舖設所奈米碳管 按預定尺寸切割所述片^奈米礙管結構預製體,形成-片 狀奈米碳管結構;以及 ϋ定所述片狀奈米碳管結構於所述支撐環。 〇 2.如申請專利範圍第1項所述的透射電鏡微柵的製備方法’ 其令,所述域環的截面為方形、圓形'半圓形或梯形。 3. 如中凊專利犯圍第1項所述的透射電鏡微柵的製備方法, 其中’所述支撐環包括—圓環狀支揮環本體和至少-延伸 冑’該至少-延伸部從所述支撐環本體向外延伸,延伸方 向為沿支㈣本―㈣半財向,且所述支擇環本 體和至少一延伸部為一體結構。 4. 如申請專利範圍第3項所述的透射電鏡微概的製備方法, 〇 其中,所述支撐環本艘具有一平整表面,所述片狀奈米碳 管結構預製體舖設於所述支樓環本體的平整表面。 5. 如申請專利範圍第4項所述的透射電鏡微拇的製備方法, 其中,所述固定所述片狀奈米碳管結構於所述支樓環的步 ㈣將所述至少一延伸部朝所通支撐環本體所在圓環的圓 "方向伸部覆蓋位於支樓環本體表面的 片狀奈米=、、:構,進而固定片狀奈米碳管結構於所述支 撐環本體與至少一延伸部之間。 如 申請專利範圍第1項所述的透射電鏡微栅的製備方法, 099112614 表單編號A〇l〇l 第23頁/共33頁 0992022308-0 201137930 其中,所述片狀奈米碳管結構預製體由至少一個奈米碳管 線狀結構編織而成或由至少一層奈米碳管膜構成。 7 .如申請專利範圍第1項所述的透射電鏡微栅的製備方法, 其中,所述按預定尺寸切割所述片狀奈米碳管結構預製體 的步驟具體包括以下步驟:提供一聚焦雷射光束;將該聚 焦雷射光束照射至所述片狀奈米碳管結構預製體表面;按 照支撐環的形狀對所述片狀奈米碳管結構預製體進行切割 ,切割後所形成的片狀奈米碳管結構的週邊通過所述支撐 環支撐,片狀奈米碳管結構的中心部分懸空設置。 8 .如申請專利範圍第1項所述的透射電鏡微柵的製備方法, 其中,在鋪設所述片狀奈米碳管結構預製體於所述支撐環 之前,進一步包括塗覆一層黏結劑於所述支撐環的表面, 以及在切割所述片狀奈米碳管結構預製體,形成一片狀奈 米碳管結構之後,固化所述黏結劑,進而固定所述月狀奈 米碳管結構於所述支撐環。 9 .如申請專利範圍第1項所述的透射電鏡微柵的製備方法, 其中,所述片狀奈米碳管結構預製體通過自身的黏性固定 於所述支撐環。 10 .如申請專利範圍第1項所述的透射電鏡微栅的製備方法, 其中,進一步包括一採用有機溶劑處理所述片狀奈米碳管 結構預製體或片狀奈米碳管結構的步驟。 099112614 表單編號A0101 第24頁/共33頁 0992022308-0201137930 VII. Patent application scope: 1. A preparation method of TEM micro-gate, including the following steps. Provide-support ring, · 'Two pre: two:::: Prefabricated body, laying carbon nanotubes according to predetermined size The sheet is obstructed by the structure preform to form a sheet-like carbon nanotube structure; and the sheet-shaped carbon nanotube structure is fixed to the support ring. 〇 2. The method for preparing a TEM microgate according to claim 1, wherein the domain ring has a square, circular 'semicircular or trapezoidal shape. 3. The method of preparing a TEM micro-grid according to the above-mentioned item, wherein the support ring comprises a ring-shaped fulcrum ring body and at least an extension 胄 a at least an extension portion The support ring body extends outwardly, and extends in a direction along the branch (four)-(four) half-finance, and the support ring body and the at least one extension portion are an integral structure. 4. The method of preparing a transmission electron microscopy according to claim 3, wherein the support ring has a flat surface, and the sheet-shaped carbon nanotube structure preform is laid on the branch. The flat surface of the building body. 5. The method according to claim 4, wherein the fixing the sheet-shaped carbon nanotube structure in the step (4) of the branch ring comprises the at least one extension. The circular "direction extension of the ring in which the support ring body is located covers the sheet-like nanometer=,, and structure on the surface of the support ring body, and further fixes the sheet-like carbon nanotube structure on the support ring body and Between at least one extension. The method for preparing a TEM micro-grid as described in claim 1 of the patent application, 099112614, Form No. A〇l〇l, page 23/33, 0992022308-0, 201137930, wherein the sheet-shaped carbon nanotube structure preform It is woven from at least one nanocarbon line-like structure or composed of at least one layer of carbon nanotube film. 7. The method for preparing a TEM micro-gate according to claim 1, wherein the step of cutting the sheet-shaped carbon nanotube structure preform according to a predetermined size comprises the following steps: providing a focused ray Shooting a light beam; irradiating the focused laser beam onto the surface of the sheet-shaped carbon nanotube structure preform; cutting the sheet-shaped carbon nanotube structure preform according to the shape of the support ring, and forming the sheet after cutting The periphery of the carbon nanotube structure is supported by the support ring, and the central portion of the sheet-shaped carbon nanotube structure is suspended. The method for preparing a TEM micro-gate according to claim 1, wherein before the laying of the sheet-shaped carbon nanotube structure preform to the support ring, further comprising coating a layer of a binder a surface of the support ring, and after cutting the sheet-shaped carbon nanotube structure preform to form a sheet of carbon nanotube structure, curing the binder to fix the moon-shaped carbon nanotube structure On the support ring. 9. The method of preparing a TEM micro-grid according to claim 1, wherein the sheet-like carbon nanotube structure preform is fixed to the support ring by its own viscosity. 10. The method for preparing a TEM micro-gate according to claim 1, further comprising the step of treating the sheet-like carbon nanotube structure preform or sheet-like carbon nanotube structure with an organic solvent. . 099112614 Form No. A0101 Page 24 of 33 0992022308-0
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