TW201137921A - Method for making transmission electron microscope grid - Google Patents

Method for making transmission electron microscope grid Download PDF

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TW201137921A
TW201137921A TW99112611A TW99112611A TW201137921A TW 201137921 A TW201137921 A TW 201137921A TW 99112611 A TW99112611 A TW 99112611A TW 99112611 A TW99112611 A TW 99112611A TW 201137921 A TW201137921 A TW 201137921A
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carbon nanotube
carrier
ring
hole
carbon
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TW99112611A
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TWI410998B (en
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Liang Liu
Li Fan
Chen Feng
Li Qian
yu-quan Wang
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Beijing Funate Innovation Tech
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Abstract

The present 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 carrier, a carbon nanotube structure, and a fixture, the carrier having first through holes, and the fixture having second through holes; stacking the carrier and the fixture; and placing the carbon nanotube structure between the carrier and the fixture; and welding the carrier and the fixture together.

Description

201137921 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 種基於奈米碳管結構的透射電鏡微栅的製備方法。 ; [0002] 【先前技術】 在透射電子顯微鏡中,微拇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。先 前技術中,透射電子顯微鏡的微柵通常係在鋼網或鎳網 等金屬網格上覆蓋一層多孔有機膜,再蒸鍍一層非晶碳 〇 膜製成的。然而,在實#應用中,當採甩上述微柵對被 測樣品的透射電鏡高分辨像進行成份分柝時,尤其在觀 察尺寸比較小的奈米顆粒,如小於5奈米的顆粒的透射電 鏡高分辨像時,微柵中的非晶碳膜對奈米顆粒的透射電 鏡高分辨像的干擾比較大。 [0003] 自九十年代初以來’以奈米碳管(請參見Helical mi一 ❹ crotubules of graphitic carbon, Nature, Sum--io I ijima,- YOl 354,p56(1991))為代表的奈米讨料 以其獨特的結構和性質引起了人們極大的關注。將奈米 碳管應用於微栅的製作,有利於降低非晶碳膜對被測樣 品成份分析的干擾。然而’由於奈米碳管的質量比較輕 ,在應用於微柵時容易發生飄移,從而影響了透射電鏡 的解析度以及測量的準確性。 [0004] 【發明内容】 有鑒於此,提供一種能夠防止奈米碳管結構飄移的透射 電鏡微柵的製備方法實為必要。 099112611 表單編號A0101 第3頁/共56頁 〇992〇223〇5 201137921 [〇〇〇5] —種透射電鏡微柵的製備方法,包括以下步驟:提供— 載體、一奈米碳管結構,以及一固定體,所述載體具有 第一通孔,所述固定體具有第二通孔;將所述固定體與 所述載體層疊設置’並將所述奈米碳管結構設置於所述 載體與所述固定體之間;以及將所述載體及固定體焊接 固定。 [0006] —種透射電鏡微栅的製備方法,包括以下步驟:提供複 數個間隔設置的載體’每個載體具有一第一通孔·,提供 一奈米碳管結構,將該奈米碳管結構覆蓋所述複數個載 體的第一通孔;提供複數個固定體,每個固定體具有一 第二通孔’使每個固定體與所述載體--對應層疊設置 ’使得所述奈米碳管結構設置於所述複數個載體與所述 複數個固定體之間;將所述每個固定體與所述載體焊接 固定;以及斷開所述複數個載體之間的奈米碳管結構, 從而形成複數個透射電鏡微柵。 Λ .. .1:..201137921 VI. Description of the Invention: [Technical Field] [0001] The present invention relates to a method for preparing a transmission electron micro-gate, and more particularly to a method for preparing a transmission electron micro-gate based on a carbon nanotube structure. [0002] [Prior Art] In the transmission electron microscope, the micro-flip system is used to carry a powder sample and is an important tool for observation by high-resolution image (HRTEM) of transmission electron microscopy. In the prior art, the microgrid of the transmission electron microscope is usually formed by covering a metal mesh such as a steel mesh or a nickel mesh with a porous organic film and vapor-depositing an amorphous carbon film. However, in the application of the real application, when the micro-gate is used to perform the component enthalpy of the TEM high-resolution image of the sample to be tested, especially in the observation of the transmission of relatively small-sized nanoparticles, such as particles smaller than 5 nm. When the electron microscope is high-resolution image, the amorphous carbon film in the micro-gate has a large interference to the high-resolution image of the TEM of the TEM. [0003] Since the early 1990s, 'nano carbon nanotubes (see Helical mi cro crotubules of graphitic carbon, Nature, Sum--io I ijima, - YOl 354, p56 (1991)) The material has attracted great attention due to its unique structure and nature. The application of nano carbon tubes to the fabrication of micro-gates is beneficial to reduce the interference of amorphous carbon films on the analysis of the components of the sample to be tested. However, due to the relatively light mass of the carbon nanotubes, drifting is likely to occur when applied to the microgrid, which affects the resolution of the TEM and the accuracy of the measurement. SUMMARY OF THE INVENTION In view of the above, it is necessary to provide a method of preparing a TEM micro-grid capable of preventing the structure of a carbon nanotube from drifting. 099112611 Form No. A0101 Page 3 of 56 〇992〇223〇5 201137921 [〇〇〇5] A method for preparing a TEM microgrid, comprising the steps of: providing a carrier, a carbon nanotube structure, and a fixing body, the carrier has a first through hole, the fixing body has a second through hole; the fixing body is stacked with the carrier and the carbon nanotube structure is disposed on the carrier Between the fixed bodies; and fixing the carrier and the fixed body. [0006] A method for preparing a TEM microgrid, comprising the steps of: providing a plurality of spaced apart carriers, each carrier having a first through hole, providing a carbon nanotube structure, the carbon nanotube a structure covering a plurality of first through holes of the plurality of carriers; providing a plurality of fixing bodies, each of the fixing bodies having a second through hole 'such that each of the fixing bodies and the carrier are disposed in a stacking manner to make the nano a carbon tube structure disposed between the plurality of carriers and the plurality of fixing bodies; soldering and fixing each of the fixing bodies to the carrier; and disconnecting a carbon nanotube structure between the plurality of carriers , thereby forming a plurality of TEM micro-gates. Λ .. .1:..

[οοοη 相較於先前技術,由本發明提供的製備方法製備的透射 電鏡微柵通過將所述奈米破管结構聲i於所述載體及固 定體之間,可以防止在使用所述透射電鏡微柵過程中, 挾持該透射電鏡微栅的器具與所述奈米碳管結構直接接 觸,而由於奈米碳管結構的質量較輕引起該奈来碳管結 構的飄移,以消除微柵在使用過程中奈米碳管結構容易 飄移的現象,從而提高透射電鏡的解析度及準確性。 【實施方式】 [0008] 下面將結合附圖及具體實施例’對本發明提供的透射電 鏡微柵及其製備方法作進一步的詳細說明。 099112611 表單編號A0101 第4頁/共56頁 0992022305-0 咬來朗&圖2,本發明第-實施例提供-種透射電鏡试 [0009]請參閱圖1及圖々求破 微栅10。所述透射電鏡微柵10包括一載體110、了 12〇 管支樓體120及〆固定體130。所述奈米破管支務,该 設置於所述載體11〇及所述固定體130之間。優遂地微米 透射電鏡微柵1〇的外控為3笔米,厚度為3微米 的圓片狀、结構° ,、〆個第 [0010] ο 所述戟體11〇包括至少一個第一通孔116 ;該炱V邊形 一通孔πθ的形狀可以為圓形、四邊形、六邊形八士構 、橢圓开ί笼。具體地’所填栽體11.0為.一圓片狀多 ,該圓片狀多孔結構包括—第"'圓片狀本體11 ’ " 圓片狀本體111包括一第一圓環112以及一第〆網狀、 114,該第〆圓環112具有一_通孔,該第一網狀結構 。戶斤述 114彀置於該通孔處,並形成複數個第一通孔1丨6 ° 、 ,.^ 10 第一_狀结構114的第一通孔116的尺寸不限,4P ' 微米〜200微米。其中,所述“尺寸,,係指第〆通? ’ 大寬度《可以理解,所述複數個第一通孔11 6的形狀 Ο 列方式不限,可根據實際應用屬求調整。所述複數摘 一通孔11 6之間的距離可相等或不等。優選地’所述複數 個第〜通孔116均勻分佈在所述載體110的表面,相鄰的 第一通孔116之間的距離大於1微米。所述載體11〇的村料 可以係銅、鎳、鉬或陶瓷等材料。所述載體110的第一網 狀結磷η4可以通過蝕刻的方法形成。所述第一圓環112 上设薏兩個狭縫118,該兩個狹縫118對稱設置,以便與 所述固定體130固定。 [0011] [0011] 本實施例中,所述載體110的外徑為3毫米。所述複數個 099112611 表單塢號Α0101 第5頁/共56頁 0992022305-0 201137921 第一通孔11 6的形狀為方形。該複數個方形第一通孔11 6 均勻分佈在所述載體110的表面。相鄰的方形第一通孔 116之間的距離相等。該方形第一通孔116的尺寸在40微 米〜120微米之間。該第一網狀結構114與所述第一圓環 112位於同一平面内。所述載體110的材料為銅。 [0012] 所述奈米碳管支撐體120設置於所述載體110的表面。具 體地,所述奈米碳管支撐體120至少覆蓋部分所述複數個 第一通孔116。優選地,所述奈米碳管支撐體120覆蓋第 一網狀結構114的全部第一通孔116。所述奈米碳管支撐 體120為一片狀結構,優選地,該奈米碳管支撐體120為 圓片狀,直徑小於等於3毫米,進一步優選地,所述奈米 碳管支撐體120的直徑小於等於2.8毫米。 [0013] 所述奈米碳管支撐體120包括至少一個奈米碳管膜。所述 奈米碳管膜係由複數個奈米碳管組成的自支撐結構。所 述複數個奈米碳管沿同一方向擇優取向排列。所述擇優 取向係指在奈米碳管膜中大多數奈米碳管的整體延伸方 向基本朝同一方向。而且,所述大多數奈米碳管的整體 延伸方向基本平行於奈米碳管膜的表面。進一步地,所 述奈米碳管膜中多數奈米碳管係通過凡德瓦爾力首尾相 連。具體地,所述奈米碳管膜中基本朝同一方向延伸的 大多數奈米碳管中每一奈米碳管與在延伸方向上相鄰的 奈米碳管通過凡德瓦爾力首尾相連。當然,所述奈米碳 管膜中存在少數隨機排列的奈米碳管,這些奈米碳管不 會對奈米碳管膜中大多數奈米碳管的整體取向排列構成 明顯影響。所述自支撐為奈米碳管膜不需要大面積的載 099112611 表單編號A0101 第6頁/共56頁 0992022305-0 201137921 體支撐,而只要相對兩邊提供支撐力即能整體上懸空而 保持自身膜狀狀態,即將該奈米碳管膜置於(或固定於 )間隔一定距離設置的兩個支撐體上時,位於兩個支撐 體之間的奈米碳管膜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。 [0014] Ο 具體地,所述奈米碳管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,可以適當的彎曲;或者並 非完全按照延伸方向上排列,可以適當的偏離延伸方向 。因此,不能排除奈米碳管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,每一奈米碳管膜包括複數個連續且擇優取向 排列的奈米碳管片段。該複數個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個基本相 互平行的奈米碳管,該複數個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。該奈米碳管膜中的奈米碳 管沿同一方向擇優取向排列。所述奈米碳管膜為從一奈 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,所述奈米碳管膜的厚度為0. 5奈米 〜100微米。所述奈米碳管膜的寬度與拉取該奈米碳管膜 的奈米碳管陣列的尺寸有關,長度不限。 所述奈米碳管結構可包括複數層層疊設置的奈米碳管膜 。當所述奈米碳管支撐體120包括兩層或兩層以上層疊設 置的奈米碳管膜時,相鄰兩層奈米碳管膜之間通過凡德 099112611 表單編號A0101 第7頁/共56頁 0992022305-0 [0015] 201137921 瓦爾力緊密結合,且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。所述奈米碳管膜的結構及其製備方 法請參見2008年8月16日公開的,公開號為200833862 的台灣發明專利申請公開說明書。所述兩層以上的奈米 碳管膜優選為層疊且交叉設置。所謂層疊且交叉設置即 所述交又角度α不等於0度。所述交叉角度α優選為90度 〇 [0016] 由於複數層奈米碳管膜層疊且交叉設置,不同層奈米碳 管膜中的奈米碳管之間相互交織形成一網狀結構,使所 述奈米碳管支撐體120的機械性能增強,同時使該所述奈 米碳管支撐體120具有複數個均勻且規則排布的微孔122 ,該微孔122的孔徑與奈米碳管膜的層數有關,層數越多 ,微孔122的孔徑越小。所述微孔122的孔徑可為1奈米 〜1微米。此外,該奈米碳管支撐體120的厚度優選小於 100微米。 [0017] 所述奈米碳管支撐體12 0亦可以係由奈米碳管線組成的至 少一個奈米碳管網狀結構,該奈米碳管網狀結構由至少 一個奈米碳管線組成,且該至少一個奈米碳管線組成的 網狀結構包括複數個微孔,該微孔的尺寸可為1奈米〜1微 米。所述奈米碳管線由奈米碳管組成,該奈米碳管線可 為一非扭轉的奈米碳管線或扭轉的奈米碳管線。 [0018] 所述非扭轉的奈米碳管線包括大多數沿該非扭轉的奈米 碳管線軸向方向排列的奈米碳管。非扭轉的奈米碳管線 099112611 表單編號Α0101 第8頁/共56頁 0992022305-0 201137921 Ο [0019][ οοοη η Compared with the prior art, the TEM microgrid prepared by the preparation method provided by the present invention can prevent the use of the TEM microscopy by oscillating the nanotube structure between the carrier and the fixed body. During the gate process, the device holding the TEM micro-gate is in direct contact with the carbon nanotube structure, and the structure of the carbon nanotube structure is caused by the light weight of the carbon nanotube structure to eliminate the micro-gate in use. In the process, the structure of the carbon nanotubes is easy to drift, thereby improving the resolution and accuracy of the transmission electron microscope. [Embodiment] The TEM microgrid and the preparation method thereof provided by the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. 099112611 Form No. A0101 Page 4 of 56 0992022305-0 Bite Lai & Figure 2, the first embodiment of the present invention provides a TEM test [0009] Please refer to Figure 1 and the pleading of the micro-gate 10. The TEM micro-grid 10 includes a carrier 110, a 12-tube tube body 120, and a crucible holder 130. The nano tube breaking service is disposed between the carrier 11A and the fixed body 130. The external control of the micro-mirror micro-mirror micro-gate 1 为 is 3 strokes, the thickness of the wafer is 3 micrometers, the structure °, the first one [0010] ο The body 11〇 includes at least one first pass The hole 116; the shape of the 炱V-shaped one through hole πθ may be a circular shape, a quadrilateral shape, a hexagonal octagonal structure, or an elliptical open cage. Specifically, the 'filled body 11.0 is a plurality of disc-shaped porous structures, and the disc-shaped porous structure includes a 'thick' body 11 ' " the disc-shaped body 111 includes a first ring 112 and a first The mesh structure 114, the second ring 112 has a through hole, the first mesh structure. The size of the first through hole 116 of the first _-shaped structure 114 is not limited, 4P 'micron~ 200 microns. Wherein, the "size" refers to the first pass? 'large width'. It can be understood that the shape of the plurality of first through holes 11 6 is not limited, and can be adjusted according to the actual application. The distance between the through holes 11 6 may be equal or unequal. Preferably, the plurality of first through holes 116 are evenly distributed on the surface of the carrier 110, and the distance between adjacent first through holes 116 is greater than 1 μm. The carrier of the carrier 11 may be made of copper, nickel, molybdenum or ceramics, etc. The first reticulated phosphatium η4 of the carrier 110 may be formed by etching. Two slits 118 are provided, which are symmetrically arranged to be fixed with the fixing body 130. [0011] In this embodiment, the outer diameter of the carrier 110 is 3 mm. A plurality of 099112611 forms dock number Α 0101 page 5 / 56 pages 0992022305-0 201137921 The first through hole 11 6 has a square shape. The plurality of square first through holes 11 6 are evenly distributed on the surface of the carrier 110. The distance between the adjacent square first through holes 116 is equal. The square first through hole 116 The size is between 40 micrometers and 120 micrometers. The first mesh structure 114 is in the same plane as the first ring 112. The material of the carrier 110 is copper. [0012] The carbon nanotube support 120 is disposed on a surface of the carrier 110. Specifically, the carbon nanotube support 120 covers at least a portion of the plurality of first through holes 116. Preferably, the carbon nanotube support 120 covers the first All of the first through holes 116 of the mesh structure 114. The carbon nanotube support 120 is a one-piece structure, and preferably, the carbon nanotube support 120 is in the form of a disk having a diameter of 3 mm or less, further Preferably, the carbon nanotube support body 120 has a diameter of 2.8 mm or less. [0013] The carbon nanotube support body 120 includes at least one carbon nanotube film. The carbon nanotube film system is composed of plural a self-supporting structure composed of carbon nanotubes. The plurality of carbon nanotubes are arranged in a preferred orientation along the same direction. The preferred orientation refers to the overall extension direction of most of the carbon nanotubes in the carbon nanotube film. In the same direction. Moreover, most of the carbon nanotubes The direction of body extension 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 Each of the carbon nanotubes in most of the carbon nanotubes extending substantially in the same direction is connected end to end with a vanadium tube in the extending direction. Of course, the carbon nanotube film is present. A small number of randomly arranged carbon nanotubes, these carbon nanotubes do not significantly affect the overall orientation of most of the carbon nanotubes in the carbon nanotube membrane. The self-supporting carbon nanotube membrane does not need to be large. The area of the load 099112611 Form No. A0101 Page 6 / 56 pages 0992022305-0 201137921 body support, and as long as the support is provided on both sides, it can be suspended in the whole to maintain its own film state, that is, the carbon nanotube film is placed ( When it is fixed on two supports arranged at a certain distance, the carbon nanotube film located between the two supports can be suspended to maintain its own film state. The self-supporting is mainly achieved by the presence of continuous carbon nanotubes extending through the end-to-end extension of the van der Waals force in the carbon nanotube film. [0014] Specifically, most of the carbon nanotube membranes extending substantially in the same direction in the same direction are not absolutely linear, and may be appropriately bent; or may not be completely aligned 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 membranes comprises a plurality of carbon nanotube fragments arranged in a continuous and preferential orientation. The plurality of carbon nanotube segments are connected end to end by Van der Valli. 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 in the same direction. The carbon nanotube film is obtained by drawing from a carbon nanotube array. The thickness of the carbon nanotube film is 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 in which the carbon nanotube film is drawn, and the length is not limited. The carbon nanotube structure may include a plurality of layers of carbon nanotube membranes stacked. When the carbon nanotube support 120 comprises two or more layers of carbon nanotube film stacked, the adjacent two layers of carbon nanotube film pass between the van der 099112611 form number A0101 page 7 / total 56 pages 0992022305-0 [0015] 201137921 Valli is tightly coupled, and the arrangement of the carbon nanotubes in the adjacent two layers of carbon nanotube 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. The structure of the carbon nanotube film and the preparation method thereof are described in the Taiwan Patent Application Publication No. 200833862, which is published on Aug. 16, 2008. The two or more layers of the carbon nanotube film are preferably laminated and arranged in a cross. The so-called cascading and cross setting means that the angle α is not equal to 0 degrees. The intersection angle α is preferably 90 degrees 〇 [0016] Since the plurality of layers of carbon nanotube films are stacked and disposed at the same time, the carbon nanotubes in the different layers of the carbon nanotube film are interwoven to form a network structure, so that The mechanical properties of the carbon nanotube support 120 are enhanced while the carbon nanotube support 120 has a plurality of uniform and regularly arranged micropores 122 having a pore size and a carbon nanotube The number of layers of the film is related, and the more the number of layers, the smaller the pore diameter of the micropores 122. The pores 122 may have a pore diameter of from 1 nm to 1 μm. Further, the thickness of the carbon nanotube support 120 is preferably less than 100 μm. [0017] The carbon nanotube support 120 may also be at least one carbon nanotube network composed of a nano carbon line, the nano carbon tube network is composed of at least one nano carbon line, and The network structure composed of the at least one nanocarbon line includes a plurality of micropores, and the pores may have a size of 1 nm to 1 μm. The nanocarbon line is composed of a carbon nanotube, which may be a non-twisted nano carbon line or a twisted nano carbon line. [0018] The non-twisted nanocarbon pipeline includes a majority of carbon nanotubes aligned along the axial direction of the non-twisted nanocarbon pipeline. Non-twisted nanocarbon pipeline 099112611 Form No. 1010101 Page 8 of 56 0992022305-0 201137921 Ο [0019]

[0020] 099112611 可通過將奈米碳管膜通過有機溶劑處理得到。所述奈米 碳管膜包括複數個奈米碳管片段,該複數個奈米碳管片 段通過凡德瓦爾力首尾相連,每一奈米碳管片段包括複 數個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0. 5奈米〜1 毫米。具體地,可將揮發性有機溶劑浸潤所述奈米碳管 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,奈米碳管膜中的相互平行的複數個奈米碳 管通過凡德瓦爾力緊密結合,從而使奈米碳管膜收縮為 一非扭轉的奈米碳管線。該揮發性有機溶劑為乙醇、曱 醇、丙酮、二氯乙烷或氣仿,本實施例中採用乙醇。通 過揮發性有機溶劑處理的非扭轉奈米碳管線與未經揮發 性有機溶劑處理的奈米碳管膜相比,比表面積減小,黏 性降低。 所述扭轉的奈米碳管線包括大多數繞該扭轉的奈米碳管 線軸向螺旋排列的奈米碳管。該奈米碳管線可採用一機 械力將所述奈米碳管膜兩端沿相反方向扭轉獲得。進一 步地,可採用一揮發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。 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,2008年11月21日公告的,公告號為I 表單編號Α0101 第9頁/共56頁 0992022305-0 201137921 303239的台灣專利;以及於2005年12月16日中請的, 20 0 9年7月21日公告的,公告號為1 31 2337的台灣專利。 [0021] 本實施例中,所述奈米碳管支撐體120覆蓋所述透射電鏡 微柵10中的載體110,且完全覆蓋所述複數個第一通孔 116。所述奈米碳管支撐體120的直徑為2. 6毫米。所述 奈米碳管支撐體120為兩層層疊設置的奈米碳管膜,且該 兩層奈米碳管膜中的奈米碳管垂直交叉設置。 [0022] 所述固定體130設置於所述奈米碳管支撐體120的表面, 使得所述奈米碳管支撐體120固定於該固定體130與所述 載體110之間。所述固定體130包括至少一個第二通孔 136,該至少一個第二通孔136的形狀可以為圓形、四邊 形、六邊形、八邊形、橢圓形等。具體地,所述固定體 130為一圓片狀多孔結構,該圓片狀多孔結構包括一第二 圓片狀本體131,該第二圓片狀本體131包括一第二圓環 132以及一第二網狀結構134,該第二圓環132具有一個 通孔,該第二網狀結構134設置於該通孔處,並形成複數 個第二通孔136 ;該第二網狀結構134的複數個第二通孔 136的尺寸不限,可以為10微米〜200微米。可以理解, 所述複數個第二通孔136的形狀及排列方式不限,可根據 實際應用需求調整。所述複數個第二通孔136之間的距離 可相等或不等。優選地,所述複數個第二通孔136均勻分 佈在所述固定體130的表面,相鄰的第二通孔136之間的 距離大於1微米。所述固定體130的第二網狀結構134可以 通過蝕刻的方法形成。所述固定體130的材料可以係銅、 鎳、鉬或陶瓷等材料。所述第二圓環132設置有兩個卡扣 099112611 表單編號A0101 第10頁/共56頁 0992022305-0 201137921 [0023] ❹ ❹ [0024] 138,該兩個卡扣138與所述狹縫118匹配設置。所述載 體110與所述固定體130通過將所述卡扣138插入所述狹 缝118中卡合而固定在一起,從而使得所述奈米碳管支撐 體120固定於所述载體110與固定體130之間。 本實施例中,所述固定體130的結構及尺寸與所述載體 110的結構及尺寸相同,即所述固定體130的外徑亦為3毫 米,第二通孔136的尺寸與所述第一通孔116的尺寸亦相 同,所述第二通孔136的形狀亦為方形,且該第二網狀結 構134與所述第二圓環132位於同一平面内。所述複數個 第一通孔116與所述複數個第二通孔136錯位相對設置, 從而配合形成複數個第三通孔丨5〇,該第三通孔150為第 一通孔11&與第二通孔136重疊的部分,該複數個第三通 孔150的尺寸小於所述第一通孔116或第二通孔136的尺 寸,該第三通孔15〇的尺寸為20微米〜6〇微米之間,所述 第三通孔150對應一個電子透射部,該奈米碳管支樓體 120在該第三通孔150處懸空設置。 可以理解,所述狭缝118與所述卡扣138的數量不限,如 ,可以為三個’只要其能夠將所述載體11〇即固定體13〇 固定即可。另外’能夠實現將所述載體110及固定體13〇 固定在一起的方式不限於本實施例所述,還可以通過其 他機械方式將兩者固定在一起;如,通過焊接將兩者固 定在一起。 [0025] 本實施例透射電鏡微栅10在應用時,將待觀察樣&承放 在所述奈米碳管支撐體120表面。當所述樣品的尺寸大於 099112611 所述奈米碳管支撐體120的微孔122時, 表單編號A0101 第11頁/共56頁 所述微孔122可 0992022305-0 201137921 以支援該材料樣品。可通過對應於第三通孔⑽的電 射部觀測該樣品。而當所述樣品的尺寸小於所述微孔⑵ 時,尤其當所述樣品為粒徑小於5奈米的奈米顆粒時所 述樣品可通過奈米碳管切體12G中的奈米碳管的吸附作 用被穩定地吸时奈米•管壁表面,此時,亦可通過 對應於第三通孔150的電子透射部觀測該樣品。從7每 現可以觀測粒徑小於5奈米的奈米顆粒樣品,提高透^ 鏡高解析度像的解析度及清晰度。 [0026] [0027] [0028] 099112611 ㈣射―米噥管 120被所述載體11〇及固定體13〇固定,因此,在使 子等移動該透射電鏡微柵時,鑷子直接挾持所述= 及固定體⑽,而補直接麵料奈米碳管切體12〇 ;這樣可以避免鎖子與所述奈米碳管支撐體⑵直⑼ ,避免由於奈米碳管支撑體12()的質量較輕而^接觸 碳管支撐體120的飄移’同時亦減少了録子對該太2米 支撐體120的污染’從而有利於提高_透射電於^灭s 進行成分分析時的準確性及解析度」 兄對樣品 此外,由於所述奈米碳管支撐體12〇由複數個首尾才 奈米碳管束組成,而奈米碳管為㈣導t=連的 緣,所以該奈米碳管支撐體12〇的導電性較好,可^絶 將積累在奈米碳管支撐體12〇表面的電子導击° 乂即時 樣品的觀察。 更’有利於對 另外,由於奈米碳管支撐體12〇由複數個首尾相連的太” 碳管束組成,即該奈米碳管膜中的奈米管之間相的奈米 固定在-起,所以該奈米碳管膜具有較好的穩=作用 表單編號A0101 第12頁/共56頁 在 〇992〇223〇5-〇 201137921 [0029] Ο ο [0030] 對樣品進行觀察時奈米碳管膜中的奈米碳管不會晃動, 使得觀察的樣品所成的圖像更清晰。進一步地,由於所 述奈米碳管支撐體120由複數個首尾相連的奈米碳管束組 成’奈米碳管支撐體120中的奈米碳管規則排列,所以在 對樣品進行觀察時便於定位尋找樣品。 6月參閱圖3及圖4,本發明第二實施例提供一種透射電鏡 微柵20。該透射電鏡微柵2〇的外徑為3毫米,厚度為3微 米〜20微米的圓片狀結構。所述透射電鏡微栅2〇包括一 載體210、一奈米碳管支撐體220以及一固定體230。所 述載體21 0為一圓片狀多礼給構’其包括一第一圓片狀本 體211,s亥第一圓片狀本體211包括一第一-圓_環212以及 複數個第一條狀結構214,該第一圓環212具有一個通孔 ,該複數個第一條狀結構214設置於第一圓環212的通孔 處,並相互間隔設置形成複數個第一通孔216 ;所述第一 圓環212上設置兩個狹縫218。所述固定體23〇為一圓片 狀多孔結構,其包括一第;圓片狀本體231,該第二圓片 狀本體231包括一第二圓環232以及複數個第二條狀結構 234,該第一圓環232具有一個通孔,該複數個第二條狀 結構234設置於該通孔處,並間隔設置形成複數個第二通 孔2 36 ;所述第二圓環232上設置兩個卡扣238。所述齐 米碳管支撐體220設置於所述載體21〇及所述固定體23〇 之間。所述載體210與固定體230通過所述卡扣238與狹 缝218的配合固定在一起。因此,所述奈米碳管支撐體 220被固定於所述載體210及所述固定體23〇之間。 所述奈米碳管支撐體220與第一實施例透射電鏡微柵的 099112611 表單編珑Α0101 0992022305-0 201137921 奈米碳管支撐體I20相同’所述第一圓環212及第二圓環 232的結構分別與第—實施例中的第一圓環11 2及第二圓 環132的結構相同。所述透射電鏡微柵20與所述透射電鏡 微栅10的不同之處在於:所述複數個第一條狀結構214相 互平行且等間隔設置’形成複數個相互平行的第一通孔 216,相鄰的第一條狀結構214之間的間隔在30微米〜 150微米之間,所述第一條狀結構214的直徑大於1微米。 所述複數個第二條狀結構234相互平行且等間隔設置,形 成複數個相互平行的第二通孔236 ’且相鄰的第二條狀結 構2 3 4之間間隔3 〇微米〜15〇微來。所述複數個第一條狀 結構214通過所述奈米碳管支撐體220與所述複數個第二 條狀結構234交又相對設置’且第一條狀結構214與第二 條狀結構234之間呈90度夾角,因此,所述複數個第一通 孔216與複數個第二通孔236交叉相對設置’從而形成複 數個第三通孔250 ’該複數個第三通孔250的尺寸在30微 米〜150微米之間’相鄰的第王通乳250之間的距離大於1 微米。所述奈米碳管支撐體220在每個第三通孔250處懸 空設置,且對應一個電子透射部。該電子透射部用於承 載被測樣品。 [0031] 可以理解,所述第一條狀結構214與第二條狀結構234之 間形成的夾角亦町以大於等於0度小於90度。所述複數個 第一條狀結構21 4及第二條狀結構234的排列方式不限於 本實施例。如,所述第一條狀結構214之間的距離可以不 等,所述第一條狀結構214之間可以交叉排列;相鄰的第 一條狀結構214之間的距離亦可以為10微米~2〇〇微米, 099112611 表單煸號A0101 第14頁/共56頁 0992022305-0 201137921 所述第-條狀結構214的寬度可大於】微米。所述第二條 狀結構234之間的距離可以不等,所述第二條狀結構234 之間可以交又排列;相鄰的第二條狀結構234之間的距離 亦可以為1〇微米〜200微米,所述第二條狀結構234的寬 度可大於1微米。所述第二條狀結構234的排列方式亦可 以與所述第一條狀結構214的排列方式不同。 [0032] 〇 可以理解,所述載體21〇的第一條狀結構214及固定體 230的第二條狀結構234可以通過蝕刻的方法形成。所述 第一條狀結構214及第二條狀結構234亦可以係通過拉絲 法形成的絲狀結構《 [0033]請參閱圖5及圖6,本發明第三實施例提供一種透射電鏡 微柵30。該透射電鏡微柵30的外徑為3毫米,厚度為3微 米〜20微米的圓片狀結構。所述透射愈鏡微柵3 〇包括一 載體310、一奈米碳管支撐體320以及一固定體330 ^所 述载體310為一圓片狀多孔結構,其包括一第一圓片狀本 體311 ’該第一圓片狀本體311包括一第一圓環312以及 Q 一第一網狀結構314,該第一圓環312具有一個通孔,該 第一網狀結構314設置於該通孔處,並形成複數個第一通 孔316 ;所述第一圓環312上設置兩個狹縫318。所述固 定體330為一第二圓環332,且該固定體330只包括—個 第二通孔336 ;所述第二圓環332上設置兩個卡扣338。 所述奈米碳管支樓體320設置於所述載體310及所述固定 體330之間。所述載體310與固定體330通過所述卡扣338 與狹縫318配合固定在一起。因此,所述奈米碳管支撐體 320被固定於所述載體31〇及所述固定體330之間。 099112611 表單編號A0101 第15頁/共56頁 0992022305-0 201137921 [0034] 所述透射電鏡微栅3 0的結構與第一實施例的透射電鏡微 柵10的結構相似,具體地,所述載體31〇及奈米碳管支撐 體320的材料及結構分別與透射電鏡微柵1〇的載體11〇及 奈米碳管支撐體120的材料及結構相同。不同之處在於: 所述固定體330為一第二圓環332,且該固定體330包括 一個第二通孔33δ。該固定體330的直徑與載體310的直 桎相同,優選地,第二圓環332的内徑與第一圓環312的 内相同。所述奈米碳管支撐體32〇固定於第一圓環312 與第二圓環332之間,且該奈米碳管支撐體32〇的直徑略 大於第—圓環332的内:徑。所述第一通孔316對應一個電 子透射部。所述奈米碳管支撐體320在第一通孔316處懸 空設置。 [0035] 請參閱圖7及圖8,本發明第四實施例提供一種透射電鏡 微柵40。所述透射電鏡微栅40包括一載體41〇、一奈米碳 管支撐體420以及一固定體430。優選地,該透射電鏡微 拇40的外徑為3毫米,厚度為3微米〜2〇微米的圓片狀結 構。 [0036] 所述栽體41〇為一第一圓環412,且該載體410包括一個 第—通孔416 ;所述第一圓環412上設置兩個狹縫418。 所述固定體430為一第二圓環432,且該固定體430包括 —個第二通孔436 ;所述第二圓環432上設置兩個卡扣 438。所述載體410與固定體430通過所述卡扣438與狹縫 418匹配固定在一起。 所述奈米碳管支撐體420設置於所述載體410及所述固定 體430之間,且在所述第一通孔416及第二通孔436處懸 099112611 表單編號A0101 第16頁/共56頁 〇9 [0037] 201137921 〇 W [0038] 切置該奈米碳管支撐體420的直徑略大於所述第一圓 衣412及第—圓環432的内徑。所述奈米碳管支撐體420 的結構與第—音, 耳苑例提供的透射電鏡微柵1 〇的奈米碳管 支撲體120的結構相似,優選地,所述奈米碳管支樓體 420為複數層層疊且交叉設置的奈米碳管膜。本實施例中 ’所述奈米碳管支撐體420為四層層疊且交叉設置的奈米 碳管膜’且相鄰的奈米碳管膜中的奈米碳管垂直設置; 該奈米碳管支撐體420具有複數個均勻且規則排布的微孔 ,該微孔的孔徑為1奈米~ 0. 5微米。 請參閱圖9及圖1〇,本發明第五實施例提供一種透射電鏡 微栅50。所述透射電鏡微柵5〇包括一載體510、一奈米碳 管支撐體520以及一固定體530。所述奈米碳管支撐體 520設置於所述載體510及所述固定體530之間。優選地 ’該透射電鏡微柵50的外徑為3毫米,厚度為3微米〜20 微米的片狀結構。 [0039] 所述載體510與所述固定體530之間具有一連接處’在該 G 連接處形成有一折譽#550,且該載體與固定體530 通過該折疊部550活動連接,可以使得該載體510與固定 體530處於打開狀態或閉合狀態。所述折疊部550可以係 由所述載體510與所述固定體530 —體成型而形成的’亦 可以係一樞轴。所述載體510為一片狀多孔結構,其包括 一第一圓片狀本體511,該第一圓片狀本體511包括一第 一圓環512以及一第一網狀結構514,該第一圓環512具 有一個通孔,且該第一網狀結構514設置於該通孔處,並 形成複數個第一通孔516 ;所述第一圓環512上設置一個 099112611 0992022305-0 表單編號A0101 第17頁/共56頁 201137921 狹缝518。所述固定體530為一片狀多孔結構,其包括一 第二圓片狀本體531,該第二圓片狀本體531包括一第二 圓環532以及一第二網狀結構534,該第二圓環532具有 一個通孔,且該第二網狀结構534設置於該通孔處,並形 成複數個第二通孔536 ;所述第二圓環532上設置一個卡 扣538,該卡扣538與所述狹縫518匹配設置。 [0040] 具體地’所述折疊部550形成於所述第一圓環512與所述 第二圓環532之間’使得該第一圓環512與第二圓環532 相交且連接設置’其形狀類似;因此’所述第一 圓片狀本體511與第二圓片狀本體531的形狀,以及第一 圓環512及第二圓環532的形狀均為類圓形,該第一圓片 狀本體511與第二圓片狀本體531的相交處為所述折疊部 550。所述載體510與所述固定體530通過該折疊部550折 叠之後,可以使得所述第一圓5衣512的内沿與第二圓環 532的内沿正對設置。優還地’所述載體510與固定體 530折疊之後完全重合。所述狹縫518與卡扣538分別設 置於與所述折疊部550相對的I1置’當所述載體510與固 定體530通過該折疊部折疊之後,所述卡扣538穿過 該狹縫518,卡在所述第〆圓環512上,從而使得所述載 體與所述固定體53〇固定在一起,進而使得所述奈米 碳管支撐體520固定於該載體510與固定體530之間。 [0041] 本實施例中,所述載體51〇與固定體530係—體成型結構 。所述載體51〇與囡定體530相對於所述折疊部550對稱 設置,即所述載體51〇的具體結構與所述固定體530的具 體結構相同◊所述第〆通孔516及第二通孔536的具體結 099112611 表單碥號A0101 第18真/共56頁 0992022305-0 201137921 構與第一實施例提供的透射電鏡微柵1〇中的第一通孔Π6 及第二通孔136相同,所述第一通孔5丨6的形狀及尺寸與 第—通孔536的形狀與尺寸相同,當所述载體510與固疋 體530折疊之後,所述第一通孔516與第二通孔536-- 對應且重合,並對應一個電子透射部。所述奈米碳管支 撐體520在第二通孔536及第一通孔516處懸空設置。 [0042] Ο 所述奈米碳管支撐體520與第一實施例中的奈米碳管支撐 體120相同’包括至少一個奈米碳管嫉,或由至少一個奈 求碳管線組成的奈米碳管網狀結構。具體地,本實施例 .;: 中’所述奈米碳管支撐體520包括兩層層疊且交叉設置的 奈米碳管膜’且該兩層奈米碳管膜中的奈米碳管垂直設 置,形成複數個均勻且規則排布的微孔,該微孔的孔徑 為1奈米〜1微米。 [0043] Ο 可以理解,所述狹縫518與卡扣538的數量及具體結構不 限’只要能夠實現固定載體510與固定體530即可。所述 載體510與固定體530上亦可以不設置所述狹縫518與卡 扣538 ’只要將載體510與固定體530沿所述折疊部55〇 對折開合即可《在使用該透射電鏡微柵5〇時,利用挾持 物挾持所述載體510與固定體530,這樣可以避免因挾持 物直接接觸所述奈米碳管支撐體520而引起奈米碳管結構 522較大的飄移,以及污染該奈米碳管支撐體“^ ;有利 於提高該透射電鏡微柵5〇的解析度及準確度。當然,序 所述栽體510與所述固定體530通過設置卡扣或焊接等^ 械方式連接固定在一起的時候,可以進一步地固定奈米 碳管支撐體520,進而可以更加防止奈米碳管支撐體 099112611 表單編號Α0101 第19頁/共56頁 0992022305-0 201137921 在使用透射電鏡微柵50的時候飄移。 [0044] 可以理解,本發明第一實施例、第二實施例、第三實施 例以及第四實施例中的載體與固定體亦可以係一體結構 [0045] 本發明還提供一種製備透射電鏡微柵的方法,該方法包 括以下步驟:提供一載體,該載體具有第一通孔;提供 一奈米碳管結構,將該奈米碳管結構覆蓋所述載體的第 一通孔;以及提供一固定體,該固定體具有第二通孔, 將所述固定體與所述載體層疊設置,使所述奈米碳管結 構固定於所述載體和所述固定體之間。 [0046] 其中,所述載體與所述固定體可以係兩個獨立的、分離 結構體,亦可以係一體結構。可以理解,當所述載體與 固定體係一體結構時,所述奈米碳管結構可以同時覆蓋 所述載體的第一通孔及所述固定體的第二通孔。 [0047] 所述奈米碳管結構為至少一個奈米碳管膜、至少一個奈 米碳管線或至少一個奈米碳管網狀結構。所述至少一個 奈米碳管膜或至少一個奈米碳管線係從一奈米碳管陣列 中直接抽取出來的。所述奈米碳管網狀結構係由所述至 少一個奈米碳管線按照一定順序編織或組合交叉設置而 組成的。 [0048] 所述將該奈米碳管結構覆蓋所述載體的第一通孔的步驟 進一步包括採用有機溶劑處理覆蓋所述載體的第一通孔 的奈米碳管結構的步驟。 [0049] 所述將所述載體與固定體層疊設置的步驟可以為:通過 099112611 表單編號A0101 第20頁/共56頁 0992022305-0 201137921 [0050] G [0051] 〇 [0052] 機械方式層疊所述载體與固定體,使得所述固定體的第 二通孔與所述載體的第一通孔至少部分重疊。具體地, 可以採用焊接或卡扣的方式將所述固定體及載體層疊設 置,從而使得所述奈米碳管切體挾持於所述載體與固 定體之間。 可以理解,上述f備透射電鏡微栅的方法中,提供所述 載體、固定體以及奈米碳管結構的順序可以根據實際情 況確定。如,可以同時提供所述載體與固定體;亦可以 同時提供所述載體、固定體以及奈米碳管結構;還可以 同時提供所述載體及奈米碳管;結:構..β . 請參閱圖9至圖11,本實施例具體提供一種製備上述透射 電鏡微柵50的方法。該製備方法包括以下步驟:(si〇) 提供所述載體510以及所述固定體53〇,所述載體5i〇具 有複數個帛-通孔516,所述固定體53()具有複數個第二 通孔536; (S2G)提供-奈米碳管結構如,將該奈米碳 管結構522覆蓋所述載體510的第一通孔516 ; (s3㈧將 所述固定鎖G麻述_51G層疊設置,使所述奈米碳 管結構522固定於所述載體510和所述固定體53〇之間。 步驟(sio) t所述載體510及固定體53〇為一體成型結 構’所述載體51G與固^體53G的連接處具有—折叠部 550,該載體51G與固^體53G通過該折疊部咖可以完全[0020] 099112611 can be obtained by treating a carbon nanotube membrane with an organic solvent. The carbon nanotube film comprises a plurality of carbon nanotube segments, the plurality of carbon nanotube segments are connected end to end by Van der Waals force, and each carbon nanotube segment comprises a plurality of parallel and through Van der Waals force Tightly bonded carbon nanotubes. The carbon nanotube segments have any length, thickness, uniformity and shape. 5纳米〜1毫米。 The non-twisted nano carbon line length is not limited, the diameter is 0. 5 nanometers ~ 1 mm. Specifically, the volatile organic solvent may be immersed in the entire surface of the carbon nanotube film, and the plurality of nanoparticles parallel to each other in the carbon nanotube film under the action of surface tension generated when the volatile organic solvent is volatilized The carbon tubes are tightly coupled by van der Waals forces, thereby shrinking the carbon nanotube membrane into a non-twisted nanocarbon pipeline. The volatile organic solvent is ethanol, decyl alcohol, acetone, dichloroethane or gas, and ethanol is used in this embodiment. The non-twisted nanocarbon line treated with a volatile organic solvent has a smaller specific surface area and a lower viscosity than a carbon nanotube film treated with a non-volatile organic solvent. The twisted nanocarbon line includes a majority of carbon nanotubes arranged axially helically about the twisted carbon nanotube line. The nanocarbon line can be obtained by mechanically twisting both ends of the carbon nanotube film in opposite directions. Further, the twisted carbon nanotube wire can be treated with a volatile organic solvent. Under the action of the surface tension generated by the volatilization of the volatile organic solvent, the adjacent carbon nanotubes in the treated twisted nanocarbon pipeline are tightly bonded by the van der Waals force, so that the specific surface area of the twisted nanocarbon pipeline Decrease, increase in density and strength. The nano carbon pipeline and its preparation method can be found in Fan Shoushan et al., which was filed on November 5, 2002, and announced on November 21, 2008. The announcement number is I Form No. 1010101 Page 9/56 Page 0992022305- 0 201137921 303239 Taiwan patent; and on December 16, 2005, the Taiwan Patent No. 1 31 2337 announced on July 21, 2009. [0021] In the embodiment, the carbon nanotube support body 120 covers the carrier 110 in the TEM micro-gate 10 and completely covers the plurality of first through holes 116. 6毫米。 The diameter of the carbon nanotube support body is 2. 6 mm. The carbon nanotube support body 120 is a two-layer laminated carbon nanotube film, and the carbon nanotubes in the two-layer carbon nanotube film are vertically disposed. [0022] The fixing body 130 is disposed on a surface of the carbon nanotube support 120 such that the carbon nanotube support 120 is fixed between the fixed body 130 and the carrier 110. The fixing body 130 includes at least one second through hole 136, and the shape of the at least one second through hole 136 may be a circle, a quadrangle, a hexagon, an octagon, an ellipse or the like. Specifically, the fixed body 130 is a disk-shaped porous structure, and the disk-shaped porous structure includes a second disk-shaped body 131. The second disk-shaped body 131 includes a second ring 132 and a second a mesh structure 134, the second ring 132 has a through hole, the second mesh structure 134 is disposed at the through hole, and forms a plurality of second through holes 136; the plurality of second mesh structures 134 The size of the second through holes 136 is not limited and may be from 10 micrometers to 200 micrometers. It can be understood that the shape and arrangement of the plurality of second through holes 136 are not limited and can be adjusted according to actual application requirements. The distance between the plurality of second through holes 136 may be equal or unequal. Preferably, the plurality of second through holes 136 are evenly distributed on the surface of the fixed body 130, and the distance between the adjacent second through holes 136 is greater than 1 micrometer. The second mesh structure 134 of the fixed body 130 may be formed by etching. The material of the fixing body 130 may be a material such as copper, nickel, molybdenum or ceramic. The second ring 132 is provided with two buckles 099112611 Form No. A0101 Page 10 / Total 56 Page 0992022305-0 201137921 [0023] 00 ❹ [0024] 138, the two buckles 138 and the slit 118 Match settings. The carrier 110 and the fixing body 130 are fixed together by inserting the buckle 138 into the slit 118, so that the carbon nanotube support 120 is fixed to the carrier 110 and Between the fixed bodies 130. In this embodiment, the structure and size of the fixing body 130 are the same as the structure and size of the carrier 110, that is, the outer diameter of the fixing body 130 is also 3 mm, and the size of the second through hole 136 is the same as the above. The size of the through hole 116 is also the same, the shape of the second through hole 136 is also square, and the second mesh structure 134 is in the same plane as the second ring 132. The plurality of first through holes 116 and the plurality of second through holes 136 are oppositely disposed opposite to each other to form a plurality of third through holes 丨5〇, wherein the third through holes 150 are first through holes 11& a portion of the second through hole 136 that is smaller than the size of the first through hole 116 or the second through hole 136. The size of the third through hole 15 is 20 micrometers to 6 Between the micrometers, the third through hole 150 corresponds to an electron transmissive portion, and the carbon nanotube branch body 120 is suspended at the third through hole 150. It is to be understood that the number of the slits 118 and the buckle 138 is not limited, and may be, for example, three as long as it can fix the carrier 11 or the fixed body 13A. In addition, the manner in which the carrier 110 and the fixing body 13 can be fixed together is not limited to that described in the embodiment, and the two can be fixed together by other mechanical means; for example, the two are fixed together by welding. . [0025] In the present embodiment, the TEM microgrid 10 is placed on the surface of the carbon nanotube support 120 when it is applied. When the size of the sample is larger than the micropores 122 of the carbon nanotube support 120 of 099112611, the form number A0101 can be 0992022305-0 201137921 to support the sample of the material. The sample can be observed through an electric portion corresponding to the third through hole (10). And when the size of the sample is smaller than the micropores (2), especially when the sample is a nanoparticle having a particle diameter of less than 5 nm, the sample can pass through a carbon nanotube in the carbon nanotube cut 12G. The adsorption is stably absorbed by the surface of the nano tube wall, and at this time, the sample can also be observed through the electron transmissive portion corresponding to the third through hole 150. From 7 to 7 nanometer particle samples with a particle size of less than 5 nm can be observed to improve the resolution and sharpness of the high resolution image of the lens. [0028] [0028] [0028] 099112611 (d) The shot-meter tube 120 is fixed by the carrier 11〇 and the fixed body 13〇, therefore, when the sub-etc. is moved by the transmission electron micro-gate, the dice directly hold the above= And the fixed body (10), and the direct fabric nano carbon tube body 12 〇; this can avoid the lock and the carbon nanotube support (2) straight (9), to avoid the quality of the carbon nanotube support 12 () Lightly and in contact with the drift of the carbon tube support 120 'also reduces the contamination of the 2 m support body 120 by the recording', thereby facilitating the improvement of the accuracy and resolution of the component analysis of the transmission electrons In addition, since the carbon nanotube support 12 is composed of a plurality of first and last carbon nanotube bundles, and the carbon nanotubes are (four) conducting t=connected edges, the carbon nanotube support is The conductivity of 12 较好 is good, and the observation of the electron sample that will accumulate on the surface of the carbon nanotube support 12 ° can be observed. More favorable for the other, since the carbon nanotube support 12 is composed of a plurality of carbon nanotube bundles connected end to end, that is, the nanophase between the nanotubes in the carbon nanotube membrane is fixed at Therefore, the carbon nanotube film has a good stability = effect form No. A0101 Page 12 of 56 at 〇992〇223〇5-〇201137921 [0029] Ο ο [0030] When the sample is observed, the nanometer The carbon nanotubes in the carbon nanotube film do not sway, making the image formed by the observed sample clearer. Further, since the carbon nanotube support 120 is composed of a plurality of end-to-end carbon nanotube bundles The carbon nanotubes in the carbon nanotube support body 120 are regularly arranged, so that it is easy to locate and look for a sample when the sample is observed. Referring to FIG. 3 and FIG. 4 in June, the second embodiment of the present invention provides a transmission electron microscope microgrid 20 The TEM micro-gate 2 has an outer diameter of 3 mm and a thickness of 3 micrometers to 20 micrometers. The TEM micro-gate 2 includes a carrier 210, a carbon nanotube support 220, and a fixed body 230. The carrier 21 0 is a wafer-shaped gift The first wafer-shaped body 211 includes a first-circle-ring 212 and a plurality of first strip-shaped structures 214. The first ring 212 has a through hole. A plurality of first strip structures 214 are disposed at the through holes of the first ring 212 and are spaced apart from each other to form a plurality of first through holes 216; the first ring 212 is provided with two slits 218. The fixed body 23 is a disk-shaped porous structure, and includes a first disk-shaped body 231. The second disk-shaped body 231 includes a second ring 232 and a plurality of second strip-shaped structures 234. The ring 232 has a through hole, and the plurality of second strip structures 234 are disposed at the through hole, and are spaced apart to form a plurality of second through holes 2 36; and the second ring 232 is provided with two buckles 238. The zircon carbon nanotube support body 220 is disposed between the carrier 21〇 and the fixed body 23〇. The carrier 210 and the fixed body 230 are fixed by the cooperation of the buckle 238 and the slit 218. Therefore, the carbon nanotube support 220 is fixed between the carrier 210 and the fixed body 23〇. The carbon nanotube support body 220 is the same as the first embodiment of the TEM microelectrode of the first embodiment of the first embodiment of the present invention. The first ring 212 and the second ring 232 are the same as the first embodiment of the TEM 1210112611. The structure is the same as that of the first ring 11 2 and the second ring 132 in the first embodiment. The TEM micro-gate 20 is different from the TEM micro-gate 10 in that: The first strip structures 214 are parallel to each other and are equally spaced apart to form a plurality of mutually parallel first through holes 216, and the spacing between adjacent first strip structures 214 is between 30 micrometers and 150 micrometers. The first strip structure 214 has a diameter greater than 1 micron. The plurality of second strip structures 234 are parallel to each other and equally spaced to form a plurality of second through holes 236 ′ that are parallel to each other and the adjacent second strip structures 2 3 4 are spaced apart by 3 μm to 15 〇. Micro. The plurality of first strip structures 214 are disposed opposite to the plurality of second strip structures 234 by the carbon nanotube support 220 and the first strip structure 214 and the second strip structure 234 The angle between the plurality of first through holes 216 and the plurality of second through holes 236 is opposite to each other to form a plurality of third through holes 250 ′. The size of the plurality of third through holes 250 Between 30 microns and 150 microns, the distance between adjacent kings is greater than 1 micron. The carbon nanotube support 220 is suspended at each of the third through holes 250 and corresponds to one electron transmission portion. The electron transmissive portion is for carrying a sample to be tested. [0031] It can be understood that the angle formed between the first strip structure 214 and the second strip structure 234 is greater than or equal to 0 degrees and less than 90 degrees. The arrangement of the plurality of first strip structures 21 4 and the second strip structures 234 is not limited to the embodiment. For example, the distance between the first strip structures 214 may be unequal, and the first strip structures 214 may be arranged in a crosswise manner; the distance between the adjacent first strip structures 214 may also be 10 micrometers. ~2〇〇micron, 099112611 Form nickname A0101 Page 14/56 page 0992022305-0 201137921 The width of the first strip structure 214 may be greater than [micrometers]. The distance between the second strip structures 234 may be unequal, and the second strip structures 234 may be arranged and arranged; the distance between the adjacent second strip structures 234 may also be 1 〇 micron. 〜200 microns, the second strip structure 234 may have a width greater than 1 micron. The arrangement of the second strip structures 234 may also be different from the arrangement of the first strip structures 214. [0032] It can be understood that the first strip structure 214 of the carrier 21〇 and the second strip structure 234 of the holder 230 can be formed by etching. The first strip structure 214 and the second strip structure 234 may also be a filament structure formed by a wire drawing method. [0033] Referring to FIG. 5 and FIG. 6, a third embodiment of the present invention provides a TEM microgrid. 30. The TEM micro-gate 30 has an outer diameter of 3 mm and a disk-like structure having a thickness of 3 to 20 μm. The transmission mirror microgrid 3 includes a carrier 310, a carbon nanotube support 320, and a fixed body 330. The carrier 310 is a disk-shaped porous structure including a first wafer-shaped body 311. The first wafer-shaped body 311 includes a first ring 312 and a first mesh structure 314. The first ring 312 has a through hole, and the first mesh 314 is disposed at the through hole. And forming a plurality of first through holes 316; two slits 318 are disposed on the first ring 312. The fixing body 330 is a second ring 332, and the fixing body 330 includes only one second through hole 336. The second ring 332 is provided with two buckles 338. The carbon nanotube branch body 320 is disposed between the carrier 310 and the fixed body 330. The carrier 310 and the fixing body 330 are fixedly coupled together with the slit 318 by the buckle 338. Therefore, the carbon nanotube support body 320 is fixed between the carrier 31A and the fixed body 330. 099112611 Form No. A0101 Page 15 of 56 0992022305-0 201137921 [0034] The structure of the TEM micro-gate 30 is similar to that of the TEM micro-gate 10 of the first embodiment, specifically, the carrier 31 The material and structure of the tantalum and carbon nanotube support 320 are the same as those of the carrier 11 and the carbon nanotube support 120 of the transmission electron microstrip. The difference is that the fixing body 330 is a second ring 332, and the fixing body 330 includes a second through hole 33δ. The diameter of the fixing body 330 is the same as the diameter of the carrier 310. Preferably, the inner diameter of the second ring 332 is the same as that of the first ring 312. The carbon nanotube support 32 is fixed between the first ring 312 and the second ring 332, and the diameter of the carbon nanotube support 32 is slightly larger than the inner diameter of the first ring 332. The first through hole 316 corresponds to one electron transmitting portion. The carbon nanotube support 320 is suspended at the first through hole 316. Referring to FIG. 7 and FIG. 8, a fourth embodiment of the present invention provides a TEM micro-gate 40. The TEM micro-gate 40 includes a carrier 41, a carbon nanotube support 420, and a fixed body 430. Preferably, the TEM microbuckle 40 has an outer diameter of 3 mm and a disk-like structure having a thickness of 3 μm to 2 μm. [0036] The carrier 41 is a first ring 412, and the carrier 410 includes a first through hole 416; and two slits 418 are disposed on the first ring 412. The fixing body 430 is a second ring 432, and the fixing body 430 includes a second through hole 436. The second ring 432 is provided with two buckles 438. The carrier 410 and the fixed body 430 are fixedly coupled to the slit 418 by the buckle 438. The carbon nanotube support body 420 is disposed between the carrier 410 and the fixed body 430, and is suspended at the first through hole 416 and the second through hole 436. 099112611 Form No. A0101 Page 16 / Total 56 〇 9 [0037] 201137921 〇W [0038] The diameter of the carbon nanotube support 420 is set to be slightly larger than the inner diameters of the first and second circular 412 and 432. The structure of the carbon nanotube support body 420 is similar to that of the first embodiment of the nano-carbon tube support body 120 of the TEM micro-gate 1 提供 provided by the example of the ear, preferably the carbon nanotube branch The building body 420 is a carbon nanotube film which is laminated and arranged in a plurality of layers. In the present embodiment, the carbon nanotube support body 420 is a four-layer laminated and cross-mounted carbon nanotube film and the carbon nanotubes in the adjacent carbon nanotube film are vertically disposed; the nano carbon 5微米。 The tube support 420 has a plurality of uniform and regularly arranged micropores, the pore size of the pores of 1 nm ~ 0. 5 microns. Referring to FIG. 9 and FIG. 1 , a fifth embodiment of the present invention provides a TEM micro-gate 50. The TEM micro-gate 5A includes a carrier 510, a carbon nanotube support 520, and a fixed body 530. The carbon nanotube support 520 is disposed between the carrier 510 and the fixed body 530. Preferably, the TEM micro-gate 50 has a sheet-like structure having an outer diameter of 3 mm and a thickness of 3 μm to 20 μm. [0039] The carrier 510 and the fixing body 530 have a connection between the G-connection forming a reputation #550, and the carrier and the fixing body 530 are movably connected through the folding portion 550, so that the The carrier 510 and the fixed body 530 are in an open state or a closed state. The folded portion 550 may be formed by the body 510 being integrally formed with the fixed body 530 or may be a pivot. The carrier 510 is a one-piece porous structure, and includes a first wafer-shaped body 511. The first wafer-shaped body 511 includes a first ring 512 and a first mesh structure 514. The first circle The ring 512 has a through hole, and the first mesh structure 514 is disposed at the through hole, and forms a plurality of first through holes 516; the first ring 512 is provided with a 099112611 0992022305-0 form number A0101 17 pages / total 56 pages 201137921 slit 518. The fixing body 530 is a one-piece porous structure, and includes a second disk-shaped body 531. The second disk-shaped body 531 includes a second ring 532 and a second mesh structure 534. The ring 532 has a through hole, and the second mesh structure 534 is disposed at the through hole, and forms a plurality of second through holes 536; the second ring 532 is provided with a buckle 538, the buckle 538 is matched to the slit 518. [0040] Specifically, the folding portion 550 is formed between the first ring 512 and the second ring 532 such that the first ring 512 and the second ring 532 intersect and are connected to each other. The shape is similar; therefore, the shape of the first wafer-shaped body 511 and the second wafer-shaped body 531, and the shapes of the first ring 512 and the second ring 532 are all circular, the first wafer The intersection of the body 511 and the second wafer body 531 is the folded portion 550. After the carrier 510 and the fixing body 530 are folded by the folding portion 550, the inner edge of the first circular garment 512 and the inner edge of the second circular ring 532 may be disposed opposite to each other. Preferably, the carrier 510 and the holder 530 are completely overlapped after being folded. The slit 518 and the buckle 538 are respectively disposed on the opposite side of the folding portion 550. After the carrier 510 and the fixing body 530 are folded by the folding portion, the buckle 538 passes through the slit 518. , the card is fixed on the second ring 512, so that the carrier and the fixing body 53 are fixed together, so that the carbon nanotube support 520 is fixed between the carrier 510 and the fixed body 530. . [0041] In this embodiment, the carrier 51〇 and the fixed body 530 are integrally formed. The carrier 51 and the damper 530 are symmetrically disposed with respect to the folded portion 550, that is, the specific structure of the carrier 51 is the same as the specific structure of the fixed body 530, the second through hole 516 and the second The specific junction of the through hole 536 is 099112611. The form number A0101 is 18th true/common 56 page 0992022305-0 201137921 is the same as the first through hole Π6 and the second through hole 136 in the TEM microgrid 1〇 provided by the first embodiment. The shape and size of the first through hole 5丨6 are the same as the shape and size of the first through hole 536. After the carrier 510 and the solid body 530 are folded, the first through hole 516 and the second hole The through holes 536-- correspond and coincide, and correspond to one electron transmitting portion. The carbon nanotube support body 520 is suspended at the second through hole 536 and the first through hole 516. [0042] The carbon nanotube support 520 is the same as the carbon nanotube support 120 in the first embodiment 'comprising at least one carbon nanotube, or a nanometer consisting of at least one carbon nanotube Carbon tube network structure. Specifically, in the present embodiment, the carbon nanotube support 520 includes two layers of carbon nanotube membranes stacked and intersected, and the carbon nanotubes in the two carbon nanotube membranes are vertical. Provided to form a plurality of uniform and regularly arranged micropores having a pore size of from 1 nm to 1 μm. [0043] It can be understood that the number and specific structure of the slit 518 and the buckle 538 are not limited as long as the fixed carrier 510 and the fixed body 530 can be realized. The carrier 510 and the fixing body 530 may not be provided with the slit 518 and the buckle 538 ′ as long as the carrier 510 and the fixing body 530 are folded and folded along the folding portion 55 《. When the grid is 5 ,, the carrier 510 and the fixed body 530 are held by the holding material, so as to avoid the large drift of the carbon nanotube structure 522 due to the direct contact of the holding material with the carbon nanotube support 520, and pollution. The carbon nanotube support "^ is advantageous for improving the resolution and accuracy of the TEM micro-gate 5". Of course, the carrier 510 and the fixed body 530 are provided with a snap or soldering device. When the connection is fixed together, the carbon nanotube support body 520 can be further fixed, thereby further preventing the carbon nanotube support body 099112611 Form No. 1010101 Page 19 / Total 56 Page 0992022305-0 201137921 In the use of transmission electron microscopy It is understood that the carrier and the fixed body in the first embodiment, the second embodiment, the third embodiment and the fourth embodiment of the present invention may also be integrated. [0045] The present invention also A method of preparing a TEM microgrid is provided, the method comprising the steps of: providing a carrier having a first via; providing a carbon nanotube structure, the first carbon nanotube structure covering the carrier a through hole; and a fixing body having a second through hole, the fixing body and the carrier are stacked, and the carbon nanotube structure is fixed between the carrier and the fixed body [0046] wherein the carrier and the fixing body may be two independent structures, or may be a unitary structure. It can be understood that when the carrier and the fixing system are integrated, the nano carbon The tube structure may simultaneously cover the first through hole of the carrier and the second through hole of the fixed body. [0047] The carbon nanotube structure is at least one carbon nanotube film, at least one nano carbon line or At least one carbon nanotube network structure. The at least one carbon nanotube membrane or at least one nanocarbon pipeline is directly extracted from a carbon nanotube array. The carbon nanotube network structure By the at least one The nano carbon line is composed of a certain order of weaving or a combination of crossover arrangements. [0048] The step of covering the first through hole of the carrier with the carbon nanotube structure further comprises covering the carrier with an organic solvent treatment The step of stacking the carbon nanotube structure of the first through hole. [0049] The step of laminating the carrier and the fixed body may be as follows: 099112611 Form No. A0101 Page 20 / Total 56 Page 0992022305-0 201137921 [ [0501] G [0052] The carrier and the fixing body are mechanically laminated such that the second through hole of the fixing body at least partially overlaps with the first through hole of the carrier. Specifically, the fixing body and the carrier may be laminated by welding or snapping so that the carbon nanotube cut body is held between the carrier and the fixing body. It can be understood that in the above method of preparing a TEM microgrid, the order of providing the carrier, the fixed body and the carbon nanotube structure can be determined according to actual conditions. For example, the carrier and the fixing body may be provided at the same time; the carrier, the fixing body and the carbon nanotube structure may be simultaneously provided; and the carrier and the carbon nanotube tube may be simultaneously provided; the structure: β. Referring to FIG. 9 to FIG. 11, the embodiment specifically provides a method for preparing the above-described TEM micro-gate 50. The preparation method comprises the steps of: (si〇) providing the carrier 510 and the fixing body 53〇, the carrier 5i〇 having a plurality of 帛-through holes 516, the fixing body 53() having a plurality of second a through hole 536; (S2G) provides a carbon nanotube structure, for example, the carbon nanotube structure 522 covers the first through hole 516 of the carrier 510; (s3 (eight) the fixed lock G _51G stacked The carbon nanotube structure 522 is fixed between the carrier 510 and the fixing body 53. Step (sio) t The carrier 510 and the fixing body 53 are integrally formed structure 'the carrier 51G and The junction of the solid body 53G has a folded portion 550 through which the carrier 51G and the solid body 53G can be completely

Pd合或打開任意的角度。本實施例中,所述載體51〇與所 述固定體530在所述折疊部55Q處對稱設置。打開所述載 體510與固定體53G,使得該載體51〇與固定體53G通過該 折疊部550的失角為9〇度。 099112611 表單編號A0101 第21頁/共56頁 0992022305-0 201137921 [0053] 步驟(S20)具體包括以下步驟:(S21 )提供一奈米碳 管結構522,並將該奈米碳管結構522覆蓋所述載體510 的第一網狀結構514; (S22)採用有機溶劑處理覆蓋所 述載體510的第一通孔516的奈米碳管結構522 ;以及( S23)去除多餘的奈米碳管結構522,以形成奈米碳管支 撐體520。 [0054] 本實施例中,所述奈米碳管結構522為兩個層疊且交叉設 置的奈米碳管膜,且該兩個奈米碳管膜中的奈米碳管垂 直設置,並覆蓋所述載體510的第一網狀結構514。其中 ,每個奈米碳管膜的製備方法包括以下步驟: [0055] 首先,提供一奈米碳管陣列,優選地,該陣列為超順排 奈米碳管陣列。 [0056] 本實施例中,超順排奈米碳管陣列的製備方法採用化學 氣相沉積法,其具體步驟包括:(a)提供一平整基底, 該基底可選用P型或N型矽基底,或選用形成有氧化層的 矽基底,本實施例優選為採用4英寸的矽基底;(b)在 基底表面均勻形成一催化劑層,該催化劑層材料可選用 鐵(Fe)、鈷(Co) '鎳(Ni)或其任意組合的合金之 一;(c)將上述形成有催化劑層的基底在700〜900°C的 空氣中退火約30分鐘〜90分鐘;(d)將處理過的基底置 於反應爐中,在保護氣體環境下加熱到500〜740°C,然後 通入碳源氣體反應約5~30分鐘,生長得到超順排奈米碳 管陣列,其高度為200〜400微米。該超順排奈米碳管陣列 為複數個彼此平行且垂直於基底生長的奈米碳管形成的 純奈米碳管陣列。通過上述控制生長條件,該超順排奈 099112611 表單編號A0101 第22頁/共56頁 0992022305-0 201137921 米碳管陣列中基本不含有雜 化劑金屬顆粒等。該奈米碳管^型碳或殘留的催 過凡德瓦爾力緊密接觸形成陣列。的奈米碳管彼此通 [0057] [0058] Ο 伞頁施例中碳源氣可選用 化合物,減纽可選錢學性錄活潑的碳氫 飞氣氣或惰性氣體。 其次’採用一拉伸工具從上奸、*, 一定寬度和長度的奈米列中抽取獲得 、具體包括以下步驟:(a )從上述奈米碳管陣列中選定 ^ W —疋寬度的複數個奈米碳 S片奴,本實施例優選為採 定寬度的膠帶接觸 不木妷官陣列以選定一定寬如 度的複數個奈米碳管片段; y)以-魏m本Μ於“碳管_生長方向拉 伸該複數個奈米碳管片段,叫成_奈米碳管膜。 [0059]Pd closes or opens any angle. In this embodiment, the carrier 51 is symmetrically disposed with the fixed body 530 at the folded portion 55Q. The carrier 510 and the fixed body 53G are opened such that the corner angle of the carrier 51A and the fixed body 53G through the folded portion 550 is 9 degrees. 099112611 Form No. A0101 Page 21 of 56 0992022305-0 201137921 [0053] Step (S20) specifically includes the following steps: (S21) providing a carbon nanotube structure 522 and covering the carbon nanotube structure 522 a first mesh structure 514 of the carrier 510; (S22) treating the carbon nanotube structure 522 covering the first through hole 516 of the carrier 510 with an organic solvent; and (S23) removing the excess carbon nanotube structure 522 To form a carbon nanotube support 520. [0054] In this embodiment, the carbon nanotube structure 522 is two stacked and cross-mounted carbon nanotube membranes, and the carbon nanotubes in the two carbon nanotube membranes are vertically disposed and covered. The first mesh structure 514 of the carrier 510. Wherein, the preparation method of each carbon nanotube film comprises the following steps: First, an array of carbon nanotubes is provided, and preferably, the array is a super-sequential carbon nanotube array. [0056] In this embodiment, the method for preparing the super-sequential carbon nanotube array adopts a chemical vapor deposition method, and the specific steps thereof include: (a) providing a flat substrate, and the substrate may be a P-type or N-type germanium substrate. Or, using a germanium substrate formed with an oxide layer, in this embodiment, a 4-inch germanium substrate is preferably used; (b) a catalyst layer is uniformly formed on the surface of the substrate, and the catalyst layer material may be iron (Fe) or cobalt (Co). One of the alloys of nickel (Ni) or any combination thereof; (c) annealing the substrate on which the catalyst layer is formed in air at 700 to 900 ° C for about 30 minutes to 90 minutes; (d) treating the substrate It is placed in a reaction furnace, heated to 500-740 ° C in a protective gas atmosphere, and then reacted with a carbon source gas for about 5 to 30 minutes to grow a super-aligned carbon nanotube array having a height of 200 to 400 μm. . The super-sequential carbon nanotube array is a plurality of pure carbon nanotube arrays formed of carbon nanotubes that are parallel to each other and perpendicular to the substrate. By controlling the growth conditions as described above, the super-shun-nai 099112611 Form No. A0101 Page 22 of 56 0992022305-0 201137921 The carbon nanotube array is substantially free of hybrid metal particles and the like. The carbon nanotubes of the carbon type or the residual urging of the van der Waals force in close contact form an array. The carbon nanotubes are connected to each other [0057] [0058] 碳 The umbrella source can be used as a carbon source gas in the application of the compound, and the carbon can be used to record the active hydrocarbon fly gas or inert gas. Secondly, using a stretching tool, it is extracted from the nanometer column of a certain width and length, and specifically includes the following steps: (a) selecting a plurality of widths of the width of the above-mentioned carbon nanotubes from the above-mentioned carbon nanotube array. Nano carbon S-slice slaves, in this embodiment, it is preferred that the tape of the predetermined width is in contact with the array of not-timbers to select a plurality of carbon nanotube segments of a certain width; y) is a "carbon tube" The plurality of carbon nanotube segments are stretched in the direction of growth, and are called a carbon nanotube film. [0059]

G 在上述拉伸過程中’顧數個奈米碳管)i段在拉力作用 下沿拉伸方向逐漸脫離基底的同時,由於凡德瓦爾力作 用《亥選定的複數個奈米碳管片段分別與其他奈米碳管 片段首尾相連地連續地被拉出,從而形成—奈來碳管膜 。該奈米碳管膜為定向排列的複數個奈米碳管束首尾相 連形成的具有-定寬度的奈米碳管膜。該奈来碳管膜中 奈米碳管的排列方向基本平行於奈米碳管膜的拉伸方向 [0060] 本實施例中’該奈米碳管膜的寬度與奈米碳管陣列所生 長的基底蚊寸有關,該奈#碳管㈣長度不限 ,可根 據實際需求製得。本實施例中採用4英寸的基底生長超順 排奈米衫陣列,該奈米碳管膜的寬度可為^ 〜10cm。 099112611 表單編號A010! 第23頁/共56頁 0992022305-0 201137921 [0061] 其中,所述奈米碳管結構522的製備方法具體包括以下步 驟: [0062] 首先,提供一基體。該基底具有一平整表面,其材料不 限。本實施例中,該基底可為一陶瓷片。 [0063] 其次,將上述兩個奈米碳管膜依次層疊且交叉鋪設在所 述基體表面。 [0064] 由於奈米碳管較為純淨且具有較大的比表面積,故從奈 米碳管陣列直接拉取獲得的奈米碳管膜具有較好的黏性 。所述奈米碳管膜可直接鋪設在基體表面或另一奈米碳 管拉膜表面。該兩層奈米碳管膜之間通過凡德瓦爾力緊 密結合。 [0065] 可以理解的係,所述奈米碳管結構522亦可以係一層所述 奈米碳管膜,還可以係由兩層以上所述奈米碳管膜層疊 且交叉設置而形成的。當然,所述奈米碳管結構522亦可 以係至少一個奈米碳管線或至少一個奈米碳管網狀結構 〇 [0066] 步驟(S22)具體為:通過容器560將有機溶劑562滴落 在所述奈米碳管結構522的表面浸潤整個奈米碳管結構 5 2 2。該有機溶劑5 6 2為揮發性有機溶劑,如乙醇、曱醇 、丙酮、二氣乙烷或氯仿,本實施例中採用乙醇。該奈 米碳管結構522經有機溶劑562浸潤處理後,在揮發性有 機溶劑562的表面張力的作用下,每個奈米碳管膜中的平 行的奈米碳管片段會部分聚集成奈米碳管束。另外,奈 米碳管膜中奈米碳管聚集成束,使得該奈米碳管膜中平 099112611 表單編號A0101 第24頁/共56頁 0992022305-0 201137921 行的奈米碳管束之間基本相互間隔,且該奈來碳管結構 522中的兩層奈米碳管财的奈米碳管束交又排列形成微 孔結構。這些微孔係由順序排列而又互相交疊的奈米碳 管’以及奈米碳管束構成的。 队 [0067] 所述步驟(S23)為:待有機溶劑揮發後,沿載體51〇的 第一圓環512的内環去除多餘的奈米碳管結構⑽,使得 奈米破管結構522的直徑小於該第一圓環512的外徑,以 形成所述奈米碳管支撐體520。其中,可以通過雷射切割 法去除多餘的奈米碳管結構5 22來形成所述奈米碳管支揮 體520。本實施例中,去除多餘的奈米碳管結構522時可 採用傳統的氬離子雷射器或二氧化碳雷射器,其功率為 5〜30瓦(W) ’優選為18W。所述奈米碳管支撐體52〇的直 徑為2. 6毫米,與所述第一圓環512的内徑相等。可以理 解,當步驟(S20)中的奈米碳管結構52$的直徑小於所 述第一圓環512的外徑,尤其係小於等·於該第一圓環512 的内徑時,可以不用實施所述步驟(S23)。 [0068] 可以理解,所述步驟(S21 )、(S22)以及(S23)的 先後順序可以根據需要確定。如’可以將所述步驟(S21 )與步驟(S22)的先後順序互換的,即可以先用有機溶 劑處理所述奈米碳管結構522,然後再將該奈米碳管結構 522設置於所述載體510的表面。 [0069] 步驟(S30)層疊所述固定體530與所述載體510,使所 述第一通孔516與第二通孔536至少部分重疊,且所述奈 米碳管支撐體52〇的表面固定於所述載體510與固定體 530之間。具體地,通過所述折疊部550將所述固定體 099112611 表軍編號A0101 第25頁/共56頁 0992022305-0 201137921 530與載體51〇層叠设置,使付所述奈米碳管結構522固 定於所述載體510與固定體530之間。更具體地’閉合所 述固定體530與載體510,使付該載體5丨〇與固定體mo在 該折疊部550處的夾角逐漸減小至〇度;此時,該載體 51〇與固定體530正對設置,且所述載體51〇的第一通孔 516與所述固定體530的第二通孔536 — —對準設置,且 使得所述奈米碳管支撐體520在第一通孔516及第二通孔 536處懸空s又置。该步驟(S33)通過所述折疊部55〇折 疊所述載體510及固定體530,可以比較容易地實現該載 體510及固定體530的對準,尤其係比較容易實現第一通 孔516與第二通孔536的精確對準。 [0070] [0071] 另外,所述步驟(S3G)進-步包括:採用機械方式固定 所述載體510與固定體530,使得所述奈米碳管支撑體 520挾持於所述載體510及固定體530之間。本實施例中 ,所述步驟(S30)在閉合所述栽體51〇及固定體53〇的 過程中,卡合所述第二圓環532的^^ρ53ϊ與所述第一圓 環512的狹縫518,使之配合設置來固定所述載體51〇及 固定體530,從而使得所述奈米碳管支撐體52()固定於該 載體510與固定體530之間。 此外,所述透射電鏡微柵50的製僑方法不限於上述步驟 ,其中,可以將所述步驟(S30)置於步驟(S21) 和步 驟(S22)之間;此時,所述奈米碳管結構522設置於所 述載體510及固疋體530之間,所以’所述步驟($22) 玎以將所述奈米碳管結構522、栽體51〇及固定體53〇整 個浸入盛有有機溶劑的容器中浸潤來進行有機溶劑處理 099112611 表單編號A0101 第26頁/共56頁 0992022305-0 201137921 邊:驟(S23)沿所述第一圓環512或第二圓環532的外 沿切割多餘的奈米碳管結構522,得到所述夺米碳管支 撐體 ύ20,且該奈米碳管支撐體52〇設置與所述載體51〇 及固定體530之間。 [0072] 虽所述步驟(S20)提供的奈来碳管結構522包括 數個奈米碳管膜或複數個奈米碳管線,或複數個奈米 磁故 不 s _狀結構時,所述透射電鏡微栅5〇的製備方法 以兔 - ❹ 將所述奈米碳管結構5 2 2中的部分奈米碳管結構設 :所述載體510的第一通孔516上,將該奈米碳管結構 中的另一部分奈米碳管結構設置於所述固定體530的 第—通孔536上;再層疊設置具有奈米碳管的固定體53〇 Y及具有奈米碳管結構的載體51〇上,以形成所述奈米碳 g支撐體520,且使得該奈米碳管支撐體52〇設置與所述 第一通孔516與第二通孔536之間》 [0073] Ο 本發明還提供一種製備複數個透射電鏡微柵5〇的方法, 該方法包括以下步驟:(Sli〇)提供複數個載體51〇,該 複數個載體510間隔設置於一基底表面,每個載體51〇具 有一第一通孔516; (S120)提供一奈米碳管結構522, 將該奈米碳管結構522覆蓋所述複數個載體51〇的第一通 孔516; (S130)提供複數個固定體530,每個固定體 530具有一第二通孔536,並將該每個固定體53〇與所述 載體510 對應層疊設置,使得所述奈米碳管結構522 固定於所述複數個栽體51〇和所述複數個固定體530之間 ;以及(S140)斷開所述複數個載體51〇之間的奈米碳管 結構522,從而形成複數個透射電鏡微柵5〇。 099112611 表單編號A0101 第27頁/共56頁 0992022305-0 201137921 [0074] 其中,所述步驟(silO)中的所述恭底的 為平面 ,其材料不限,可以為陶兗、玻璃等。相鄰的兩個載體 51〇之間的距離不能過大或過小,過大心利於提高透射 電鏡微栅5G的生產效率,過小則使後續y驟中對不来碳 管結構522的加工難度增加,不利於降低生產成本*在 彳請步驟中使用雷射光束照射方法處一米碳管結構522 時,該相鄰的兩個载體510之間的雜離應大於雷射光束照 射在奈米碳管結構522表面上所形成光班1直控’該相鄰 的兩個載體51〇之間的距離優選為5〇~2〇〇« 進v ’為提高奈米碳管結構522的利用率旅方便切。1】可以將 該複數個載體51 〇緊密並規則排列於所述基底表面可以 理解,所述載體510及固定體530的姑構^ '為*實施 例至第四實施例中的載體及固定體的結構 [0075] 其中,所述步驟(S120)與所述少鱗(S2G)的實施方式 相同。所述步驟(S1 30)與所述少驟(S3〇)的實施方式 相同。其中,所述固定體53〇的數量與所述載體510的數 量係相同的,且每一傭載體51〇均有/固疋體53〇與之配 合。 [0076] 所述步驟(S140)可以通過雷射束照射相鄰的載體510之 間的奈米碳管結構52 2。具體地可以採用以下三種方法: [0077] 方法一:採用雷射光束照射沿每一個載體510的外邊沿區 域照射所述奈米碳管結構522—週,使得覆蓋於該載體 51〇上的奈米碳管結構522的直徑小於等於該載體51〇的 外根,形成—沿所述載體510的外邊沿環繞該載體51〇的 分離區域,從而使覆蓋於該複數個載體510上的奈米碳管 0992022305-0 099112611 表車編號A0101 第28頁/共56頁 201137921 [0078] 結構522與覆蓋於該複數個載體51〇以外的奈米碳管結構 ^2分離。 方法二:移動雷射光束,照射全部載體510之間的奈米碳 官結構522 ’從而去除全部載體51〇之間的奈米碳管結構 522 〇 [0079] Ο [0080] [0081] [0082]Ο [0083] 方法三:當該複數個載體510為按陣列方式排列於所述基 底表面時,移動雷射光束,沿直線照射覆蓋該複數個載 體510行間及列間空隙的奈米碳管結構522,從而使複數 個載體51 0之間的奈米碳管結構5 2 2斷開。 上述斷開複數個載體510之間的奈米碳管結構522的步驟 中’該雷射光束移動及照射的線路可通過電腦程式控制 〇 /1. %-V . :·;. ;. 可以理解,所述步輝(S130)與(S140)的實施順序係 可以不分先後的,可以實際情況選擇。 請參閱圖12及圖13,本發明第六實施例提供一種透射電 鏡微栅60。所述透射杳鏡微栅60包括一載體610、一奈米 碳管支撐體620以及一固定體630。所述奈米碳管支撐體 620設置於所述載體610及所述固定體630之間。優選地 ’該透射電鏡微柵60的外徑為3毫米,岸度為3微米〜20 微米的圓片狀結構。 所述載體610為一圓片狀多孔結構,其包括—第一圓片狀 本體611,該第一圓片狀本體611包括一第一圓環612以 及一第一網狀結構614,該第一圓環612具有一個通孔, 且該第一網狀結構614設置於該通孔處,並形成複數個第 099112611 表單編號A0101 第29頁/共56頁 0992022305-0 201137921 一通孔616。所述固定體630為一圓片狀多孔結構,其包 括一第二圓片狀本體631,該第二圓片狀本體631包括一 第二圓環632以及一第二網狀結構634,該第二圓環632 具有一個通孔,且該第二網狀結構634設置於該通孔處, 並形成複數個第二通孔636。所述載體610的邊緣及固定 體630的邊緣接觸設置,在該接觸處設置有焊接元件640 〇 [0084] 所述載體610及固定體630的結構與第一實施例的透射電 鏡微柵10中的載體610及固定體630的結構相似,不同之 處在於:所述第一圓片狀本體611的邊緣與所述第二圓片 狀本體631的邊緣形成面與線的接觸。具體地,所述第一 圓環612具有一第一表面618,即該第一圓環612的第一 表面618為一平面結構。該第一圓環612的橫截面為長方 形、半圓形、三角形或梯形等形狀。所述第二圓環632具 有一第二表面638,該第二圓環632的第二表面638的形 狀可以為一弧形面或棱線等形狀。故,所述第一圓環612 的邊沿與第二圓環632的邊沿接觸時,為面與線的接觸。 其中,所述載體610與所述固定體630的具體結構不限, 只要係該固定體630的邊緣與載體610的邊緣能夠實現線 與平面的接觸,以形成線接觸即可,如,當所述載體610 與所述奈米碳管支撐體620接觸的表面為平面時,所述固 定體630還可以由一第二圓環632組成,或由一第二圓環 632及複數個條狀結構組成;且該第二圓環632與所述奈 米碳管支撐體620接觸的表面為一弧形面或棱線。本實施 例中的第一圓環61 2的橫截面為長方形,所述第二圓環 099112611 表單編號A0101 第30頁/共56頁 0992022305-0 201137921 632的橫截面為圓形;所以,所述第一圓環612的第—表 面618與所述第二圓環632的第二表面638可以實現線接 觸。 [0085] 所述奈米碳管支撐體620與第一實施例中的奈米碳管支撐 體120相同,包括至少一個奈米碳管膜,或由至少—個奈 米故管線組成的奈米碳管網狀結構。本實施例中,所述 奈米碳管支撐體620包括兩層層疊設置的奈米碳管膜,且 該兩層奈米碳管膜中的奈米碳管垂直設置,形成複數個 ❹ [0086] 均勻且規則排布的微孔,該褥孔的孔徑可為丨奈米q微米 〇 Ο 所述焊接元件640係通過焊接所述載體61〇及固定體63〇 形成的’並位於所述第一圓環612與第二圓環632的接觸 處’具體地’該焊接元件640設置於所述第一圓環612的 第一表面618與所述第二圓環632的第二表面638的線接 觸處;該第一圓環612與第二圓環632在該線接觸處通過 點焊、釺焊等方式焊接在一起,來固定所述載體61〇與固 定體630 ;從而使得所述奈米碳管支撐體620固定於該載 體610及固定體630之間。本實施例中,所述焊接元件 640為複數個點焊點。 [0087] 本發明還提供一種採用焊接的方式來製備透射電鏡微柵 的方法,該方法包括以下步驟:提供一載體、一奈米碳 管結構’以及一固定體,其中,所述载體具有第一通孔 ,所述固定體具有第二通孔;將所述固定體與所述載體 層疊設置,並將所述奈米碳管結構設置於所述載體與所 述固定體之間;以及將所述載體及固定體焊接固定。 099112611 表單編號Α0101 第31頁/共56頁 0992022305-0 201137921 [0088] 所述載體具有一第一圓環,該第一圓環具有一通孔,且 該至少一第一通孔設置於該第一圓環的通孔處。所述固 定體具有一第二圓環,該第二圓環具有一通孔,且該至 少一第二通孔設置於該第二圓環的通孔處。其中,所述 第一圓環具有一第一表面,所述第二圓環具有一第二表 面,該第二表面與所述第一表面相對設置。 [0089] 所述奈米碳管結構為至少一個奈米碳管膜、至少一個奈 米碳管線或至少一個奈米碳管網狀結構。所述至少一個 奈米碳管膜或至少一個奈米礙管線係從一奈米$炭管陣列 中直接抽取出來的。所述奈米碳管網狀結構係由所述至 少一個奈米碳管線按照一定順序編織或組合交又設置而 組成的。 [0090] 所述層疊設置所述固定體與載體的步驟進一步包括採用 有機溶劑處理所述奈米碳管結構。 [0091] .當所述固定體與所述載體層疊設置時,所述固定體的邊 緣與所述載體的邊緣形成線與面的接觸,有利於實現所 述固定體與載體的對準,尤其係現實所述第一通孔與第 二通孔的--對準。 [0092] 請參閱圖14,本實施例具體提供一種製備上述透射電鏡 微栅60的方法。該製備方法包括以下步驟:(W10)提供 所述載體610、一奈米碳管結構622以及所述固定體630; (W20)將所述固定體630及載體610層疊設置,並將所 述奈米碳管結構622設置於所述載體610與固定體630之 間;以及(W30)將所述載體610及固定體630焊接固定 099112611 表單編號A0101 第32頁/共56頁 0992022305-0 201137921 [0093]步驟(W10)中的奈米碳管結構622及其製備方法與第五 實施例提供的透射電鏡微栅50的製備方法中的奈来碳管 結構522及其製備方法相同。其中,所述第一圓環612且 有一第一表面618,該第一表面618為平面;所述第二圓 環632具有一第二表面638,該第二表面638為弧形面或 棱線等形狀,可以與所述第一圓環612的第一表面618形 成線與面的接觸。 [0094]G In the above-mentioned stretching process, the number of segments of the carbon nanotubes is gradually separated from the substrate by the tensile force, and the multiple carbon nanotube segments selected by the Hai The other carbon nanotube segments are continuously pulled out end to end to form a Naibi carbon tube film. The carbon nanotube film is a carbon nanotube film having a constant width formed by a plurality of aligned carbon nanotube bundles. The arrangement direction of the carbon nanotubes in the carbon nanotube film is substantially parallel to the stretching direction of the carbon nanotube film [0060] In the present embodiment, the width of the carbon nanotube film and the growth of the carbon nanotube array are Related to the base mosquitoes, the Nai # carbon tube (four) is not limited in length and can be made according to actual needs. In this embodiment, a 4-inch substrate-grown super-aligned nano-shirt array is used, and the width of the carbon nanotube film can be from 〜10 cm. 099112611 Form No. A010! Page 23 of 56 0992022305-0 201137921 [0061] wherein the preparation method of the carbon nanotube structure 522 specifically includes the following steps: [0062] First, a substrate is provided. The substrate has a flat surface and its material is not limited. In this embodiment, the substrate can be a ceramic sheet. [0063] Next, the above two carbon nanotube films are sequentially laminated and cross-laid on the surface of the substrate. [0064] Since the carbon nanotubes are relatively pure and have a large specific surface area, the carbon nanotube film obtained by directly drawing from the carbon nanotube array has good viscosity. The carbon nanotube film can be directly laid on the surface of the substrate or on the surface of the other carbon nanotube film. The two layers of carbon nanotube membranes are tightly bonded by van der Waals force. [0065] It can be understood that the carbon nanotube structure 522 may also be a layer of the carbon nanotube film, or may be formed by laminating and intersecting two or more layers of the carbon nanotube film. Of course, the carbon nanotube structure 522 can also be at least one nano carbon line or at least one carbon nanotube network structure. [0066] Step (S22) specifically: the organic solvent 562 is dropped through the container 560 The surface of the carbon nanotube structure 522 wets the entire carbon nanotube structure 52. The organic solvent 652 is a volatile organic solvent such as ethanol, decyl alcohol, acetone, di-ethane or chloroform, and ethanol is used in this embodiment. After the carbon nanotube structure 522 is infiltrated by the organic solvent 562, the parallel carbon nanotube fragments in each of the carbon nanotube membranes partially aggregate into nanometers under the surface tension of the volatile organic solvent 562. Carbon tube bundle. In addition, the carbon nanotubes in the carbon nanotube film aggregated into a bundle, so that the carbon nanotube film in the flat 099112611 form number A0101 page 24 / total 56 page 0992022305-0 201137921 row of carbon nanotube bundles are basically mutual At intervals, and the carbon nanotube bundles of the two layers of carbon nanotubes in the carbon nanotube structure 522 are arranged to form a microporous structure. These micropores are composed of a carbon nanotube' and a carbon nanotube bundle which are arranged in series and overlap each other. [0067] The step (S23) is: after the organic solvent is volatilized, the excess carbon nanotube structure (10) is removed along the inner ring of the first ring 512 of the carrier 51〇, so that the diameter of the nano tube-breaking structure 522 It is smaller than the outer diameter of the first ring 512 to form the carbon nanotube support 520. Among them, the carbon nanotube bulk 520 can be formed by removing the excess carbon nanotube structure 5 22 by laser cutting. In this embodiment, a conventional argon ion laser or carbon dioxide laser can be used to remove the excess carbon nanotube structure 522, and its power is 5 to 30 watts (W)', preferably 18 watts. The diameter of the carbon nanotube support body 52 is 2.6 mm, which is equal to the inner diameter of the first ring 512. It can be understood that when the diameter of the carbon nanotube structure 52$ in the step (S20) is smaller than the outer diameter of the first ring 512, especially less than the inner diameter of the first ring 512, it may be omitted. The step (S23) is carried out. It can be understood that the order of the steps (S21), (S22) and (S23) can be determined as needed. For example, 'the step (S21) and the step (S22) may be interchanged, that is, the carbon nanotube structure 522 may be first treated with an organic solvent, and then the carbon nanotube structure 522 is placed in the The surface of the carrier 510. [0069] Step (S30) laminating the fixing body 530 and the carrier 510 such that the first through hole 516 and the second through hole 536 at least partially overlap, and the surface of the carbon nanotube support body 52 It is fixed between the carrier 510 and the fixed body 530. Specifically, the fixed body 099112611, the military number A0101, the 25th page, the 56th page 0992022305-0 201137921 530, and the carrier 51〇 are stacked by the folding portion 550, so that the carbon nanotube structure 522 is fixed to The carrier 510 is disposed between the carrier 510 and the fixed body 530. More specifically 'close the fixing body 530 and the carrier 510 such that the angle between the carrier 5 丨〇 and the fixing body mo at the folded portion 550 is gradually reduced to a twist; at this time, the carrier 51 〇 and the fixed body The 530 is disposed opposite to each other, and the first through hole 516 of the carrier 51 is aligned with the second through hole 536 of the fixing body 530, and the carbon nanotube support 520 is in the first pass. The hole 516 and the second through hole 536 are suspended and repositioned. In this step (S33), the carrier 510 and the fixing body 530 are folded by the folding portion 55, so that the alignment of the carrier 510 and the fixing body 530 can be relatively easily realized, and in particular, the first through hole 516 and the first through hole 516 are relatively easy to implement. Precise alignment of the two through holes 536. [0071] In addition, the step (S3G) further includes: mechanically fixing the carrier 510 and the fixing body 530, so that the carbon nanotube support 520 is held by the carrier 510 and fixed. Between the bodies 530. In this embodiment, the step (S30) is to engage the first ring 532 and the first ring 512 during the process of closing the carrier 51 and the fixed body 53〇. The slit 518 is configured to fix the carrier 51 and the fixing body 530 such that the carbon nanotube support 52 is fixed between the carrier 510 and the fixed body 530. In addition, the method for manufacturing the TEM micro-gate 50 is not limited to the above steps, wherein the step (S30) may be placed between the step (S21) and the step (S22); at this time, the nanocarbon The tube structure 522 is disposed between the carrier 510 and the solid body 530, so the step ($22) is immersed in the whole of the carbon nanotube structure 522, the carrier 51, and the fixed body 53. Immersing in an organic solvent container for organic solvent treatment 099112611 Form No. A0101 Page 26 of 56 0992022305-0 201137921 Side: Step (S23) is cut along the outer edge of the first ring 512 or the second ring 532 The excess carbon nanotube structure 522 obtains the carbon nanotube support body 20, and the carbon nanotube support 52 is disposed between the carrier 51 and the fixed body 530. [0072] Although the carbon nanotube structure 522 provided in the step (S20) includes a plurality of carbon nanotube membranes or a plurality of nanocarbon pipelines, or a plurality of nanometer magnets, the s-shaped structure is The preparation method of the TEM micro-gate 5〇 is to set a part of the carbon nanotube structure in the carbon nanotube structure 5 2 2 to the first through hole 516 of the carrier 510, the nanometer Another part of the carbon nanotube structure is disposed on the first through hole 536 of the fixed body 530; and the fixed body 53〇Y having a carbon nanotube and the carrier having the carbon nanotube structure are further laminated 51〇, to form the nano carbon g support 520, and the carbon nanotube support 52 is disposed between the first through hole 516 and the second through hole 536. [0073] The invention also provides a method for preparing a plurality of TEM micro-gates, the method comprising the steps of: (Sli) providing a plurality of carriers 51, the plurality of carriers 510 being spaced apart from each other on a substrate surface, each carrier 51〇 Having a first through hole 516; (S120) providing a carbon nanotube structure 522, covering the carbon nanotube structure 522 a plurality of first through holes 516 of the plurality of carriers 51; (S130) providing a plurality of fixing bodies 530, each of the fixing bodies 530 having a second through hole 536, and each of the fixing bodies 53 and the carrier 510 corresponding to the stacking arrangement such that the carbon nanotube structure 522 is fixed between the plurality of carriers 51〇 and the plurality of fixing bodies 530; and (S140) disconnecting between the plurality of carriers 51〇 The carbon nanotube structure 522 is formed to form a plurality of transmission electron micromirrors. 099112611 Form No. A0101 Page 27 of 56 0992022305-0 201137921 [0074] wherein the said bottom of the step (silO) is a flat surface, the material of which is not limited, and may be ceramic pottery, glass or the like. The distance between the adjacent two carriers 51〇 cannot be too large or too small, and the excessively large is beneficial to improve the production efficiency of the TEM microgrid 5G. If the distance is too small, the processing difficulty of the carbon nanotube structure 522 in the subsequent y steps is increased, which is disadvantageous. In order to reduce the production cost*, when using the laser beam irradiation method at the one-meter carbon tube structure 522 in the step of the request, the difference between the adjacent two carriers 510 should be larger than that of the laser beam irradiated on the carbon nanotubes. The light beam 1 formed on the surface of the structure 522 is directly controlled. The distance between the two adjacent carriers 51〇 is preferably 5〇~2〇〇«Into v' to improve the utilization of the carbon nanotube structure 522. cut. 1] The plurality of carriers 51 can be closely and regularly arranged on the surface of the substrate. It can be understood that the carrier 510 and the fixing body 530 are the carriers and the fixing bodies in the fourth to fourth embodiments. Structure [0075] wherein the step (S120) is the same as the embodiment of the small scale (S2G). The step (S1 30) is the same as the embodiment of the small step (S3〇). The number of the fixed bodies 53 is the same as the number of the carriers 510, and each of the commission carriers 51 has a solid body 53 〇. [0076] The step (S140) may irradiate the carbon nanotube structure 52 2 between the adjacent carriers 510 by a laser beam. Specifically, the following three methods can be adopted: [0077] Method 1: irradiating the carbon nanotube structure 522-week along the outer edge region of each carrier 510 by using a laser beam to make the cover on the carrier 51〇 The carbon nanotube structure 522 has a diameter less than or equal to the outer root of the carrier 51〇, forming a separation region surrounding the carrier 51〇 along the outer edge of the carrier 510, thereby allowing the nanocarbon covering the plurality of carriers 510. Tube 0992022305-0 099112611 Meter No. A0101 Page 28 of 56 201137921 [0078] Structure 522 is separated from the carbon nanotube structure ^2 that covers the plurality of carriers 51〇. Method 2: Moving the laser beam, illuminating the carbon carbon structure 522 ' between all the carriers 510 to remove the carbon nanotube structure between all the carriers 51 522 [0079] Ο [0080] [0082] [0082 Method : [0083] Method 3: When the plurality of carriers 510 are arranged on the surface of the substrate in an array, the laser beam is moved, and the carbon nanotubes covering the inter-row and inter-column spaces of the plurality of carriers 510 are irradiated along a straight line. Structure 522, thereby breaking the carbon nanotube structure 52 2 between the plurality of carriers 51 0 . In the step of disconnecting the carbon nanotube structure 522 between the plurality of carriers 510, the line of the laser beam moving and illuminating can be controlled by a computer program 〇/1. %-V . :·;.;. The order of implementation of the step gamma (S130) and (S140) may be in any order, and may be selected in actual situations. Referring to Figures 12 and 13, a sixth embodiment of the present invention provides a transmission micromirror 60. The transmissive mirror microgrid 60 includes a carrier 610, a carbon nanotube support 620, and a fixed body 630. The carbon nanotube support 620 is disposed between the carrier 610 and the fixed body 630. Preferably, the TEM microgrid 60 has an outer diameter of 3 mm and a land structure of 3 to 20 micrometers. The carrier 610 is a disk-shaped porous structure, and includes a first wafer-shaped body 611. The first wafer-shaped body 611 includes a first ring 612 and a first mesh structure 614. The first circle The ring 612 has a through hole, and the first mesh structure 614 is disposed at the through hole, and forms a plurality of 099112611 form number A0101 page 29 / 56 pages 0992022305-0 201137921 a through hole 616. The fixed body 630 is a disk-shaped porous structure, and includes a second disk-shaped body 631. The second disk-shaped body 631 includes a second ring 632 and a second mesh structure 634. The ring 632 has a through hole, and the second mesh structure 634 is disposed at the through hole, and forms a plurality of second through holes 636. An edge of the carrier 610 and an edge of the fixing body 630 are disposed in contact with each other, and a soldering element 640 is disposed at the contact portion. [0084] The structure of the carrier 610 and the fixing body 630 is the same as that of the TEM microgrid 10 of the first embodiment. The structure of the carrier 610 and the fixing body 630 are similar, except that the edge of the first wafer-shaped body 611 and the edge of the second wafer-shaped body 631 form a surface-to-line contact. Specifically, the first ring 612 has a first surface 618, that is, the first surface 618 of the first ring 612 is a planar structure. The cross section of the first ring 612 has a shape of a rectangular shape, a semicircular shape, a triangular shape, or a trapezoidal shape. The second ring 632 has a second surface 638. The shape of the second surface 638 of the second ring 632 may be a curved surface or a ridge line. Therefore, when the edge of the first ring 612 is in contact with the edge of the second ring 632, it is a face-to-line contact. The specific structure of the carrier 610 and the fixing body 630 is not limited as long as the edge of the fixing body 630 and the edge of the carrier 610 can achieve line-to-plane contact to form a line contact, for example, When the surface of the carrier 610 in contact with the carbon nanotube support 620 is a flat surface, the fixed body 630 may also be composed of a second ring 632 or a second ring 632 and a plurality of strip structures. The surface of the second ring 632 contacting the carbon nanotube support 620 is a curved surface or a ridge line. The cross section of the first ring 61 2 in this embodiment is a rectangle, and the cross section of the second ring 099112611 form number A0101 page 30 / page 56 0992022305-0 201137921 632 is circular; therefore, the The first surface 618 of the first ring 612 and the second surface 638 of the second ring 632 may be in line contact. [0085] The carbon nanotube support 620 is the same as the carbon nanotube support 120 in the first embodiment, and includes at least one carbon nanotube film, or a nanometer composed of at least one nano tube. Carbon tube network structure. In this embodiment, the carbon nanotube support body 620 includes two layers of carbon nanotube membranes stacked, and the carbon nanotubes in the two layers of carbon nanotube membranes are vertically disposed to form a plurality of ❹ [0086 Uniform and regularly arranged micropores, the pores of which may be nanometers q micron, the soldering elements 640 are formed by soldering the carrier 61〇 and the fixed body 63〇 and are located at the The contact of a ring 612 with the second ring 632 'specifically' the welding element 640 is disposed on the line of the first surface 618 of the first ring 612 and the second surface 638 of the second ring 632 a contact portion; the first ring 612 and the second ring 632 are welded together by spot welding, brazing, or the like at the line contact to fix the carrier 61〇 and the fixing body 630; thereby making the nano The carbon tube support 620 is fixed between the carrier 610 and the fixed body 630. In this embodiment, the soldering component 640 is a plurality of spot solder joints. [0087] The present invention also provides a method for preparing a TEM microgrid by soldering, the method comprising the steps of: providing a carrier, a carbon nanotube structure, and a fixing body, wherein the carrier has a first through hole, the fixing body has a second through hole; the fixing body is stacked with the carrier, and the carbon nanotube structure is disposed between the carrier and the fixed body; The carrier and the fixing body are welded and fixed. 099112611 Form No. 101 0101 Page 31 / Total 56 Page 0992022305-0 201137921 [0088] The carrier has a first ring, the first ring has a through hole, and the at least one first hole is disposed in the first The through hole of the ring. The fixing body has a second annular ring, the second annular ring has a through hole, and the at least one second through hole is disposed at the through hole of the second annular ring. The first ring has a first surface, and the second ring has a second surface opposite to the first surface. [0089] The carbon nanotube structure is at least one carbon nanotube membrane, at least one nanocarbon pipeline, or at least one nanocarbon tubular network. The at least one carbon nanotube membrane or at least one nano-barrier line is directly extracted from a nanometer carbon nanotube array. The carbon nanotube network structure is composed of the at least one nanocarbon line woven or combined in a certain order. [0090] The step of laminating the fixed body and the carrier further comprises treating the carbon nanotube structure with an organic solvent. When the fixing body is stacked with the carrier, the edge of the fixing body forms a line-to-face contact with the edge of the carrier, which is advantageous for achieving alignment between the fixing body and the carrier, in particular It is a reality that the first through hole and the second through hole are aligned. Referring to FIG. 14, the embodiment specifically provides a method for preparing the TEM micro-gate 60 described above. The preparation method comprises the steps of: (W10) providing the carrier 610, a carbon nanotube structure 622, and the fixing body 630; (W20) laminating the fixing body 630 and the carrier 610, and arranging the nai The carbon nanotube structure 622 is disposed between the carrier 610 and the fixed body 630; and (W30) the carrier 610 and the fixed body 630 are soldered and fixed. 099112611 Form No. A0101 Page 32 / Total 56 Page 0992022305-0 201137921 [0093 The carbon nanotube structure 622 in the step (W10) and the preparation method thereof are the same as the carbon nanotube structure 522 in the preparation method of the TEM microgrid 50 provided in the fifth embodiment, and a preparation method thereof. The first ring 612 has a first surface 618, and the first surface 618 is a flat surface. The second ring 632 has a second surface 638. The second surface 638 is a curved surface or a ridge line. The shape may be in line-to-face contact with the first surface 618 of the first ring 612. [0094]

[0095][0095]

可以理解,所述奈米碳管結構6 2 2還可以為至少一奈米碳 管網狀結構或裘少一奈米碳管線。 步驟(W20)包括以下步驟:(W21)將所述奈米碳管結 構622設置於所述載體610的第一圓環612的第一表面618 ;(W22)採用置於一容器66〇中的有機溶劑662處理所 述覆蓋所述載艏610的第一通孔616的奈米碳管結構622 ;(W23)丧除多餘的奈米碳管結構622,以形成所述奈 米碳管支撐髏620 ;以及(W24)將所述固定體630設置 於所述奈米碳管支撐體620上,使得所述第二通孔636與 所述第一通孔616至少部分重疊設置。具體地,該步驟( W24)使所述第二圓環632的第二表面638與所述第一溷 環612的第""表面618正對設置,且所述第二通孔636與 所述第一通孔616一一對應重疊設置。其中,所述步驟( W21)至(W23)中具體採用的方法與夕驟(S21)至( S23)中具禮採用的方法相同。所述少棘(W21)、( W22)以及(tf23)的先後順序可以根據需要確定。如 099112611 可以將所述梦騍(W21)與步驟(W22)的先後順序互換 表單編號A0101 第33頁/共56頁 0992022305-0 201137921 的,即可以先用有機溶劑處理所述奈米碳管結構622,然 後再將該奈米碳管結構6 22設置於所述載體610的表面。 [0096] 步驟(W30 )具體包括以下步驟:首先,採用一焊接系統 在所述第一圓環612及第二圓環632處施加壓力,使得所 述第一圓環612的第一表面618與第二圓環632的第二表 面638線接觸;然後,在該第一圓環612的第一表面gig 與第二圓環632的第二表面638的線接觸處進行焊接。在 該焊接過程中’所述線接觸處產生大量的熱,將中心最 熱區域的第一圓環612及第二圓環632的材料很快加熱至 溶化狀態’繼續施加壓力.》待苐一圓環612及第二圓環 632冷卻後’該第一圓環612及第二圓環632焊接在一起 ’在該焊接處形成所述焊接元件640·。所以.,所述焊接元 件640的材料與所述第一圓環612及第二圓環632的材料 相同。本實施例中’所述焊接系統為點焊機,所述焊接 元件640為焊點。該步驟(W30)通過線與平面的接觸使 得所述載體610及固定體630焯接在一起,可以比較容易 地實現該載體61〇及固定體630的對準。 [0097] 另外’當步驟(Wl〇)提供的所述奈米碳管結構622包括 複數個奈米碳管膜或複數個奈米碳管線,或複數個奈米 故管網狀結構時’所述透射電鏡微拇60的製備方法還可 以為:所述步驟(W10)保持不變’所述步驟(w2〇)可 以通過將所述奈米被管結構6 2 2中的部分奈米碳管纟士構咬 置於所述載體61〇的第一通孔616上,將所述奈米碳管結 構622中的另一部分奈米碳管結構設置於所述固定體63〇 的第二通孔636上。然後將具有奈米碳管結構的固定體 099112611 表單編號A0101 第34頁/共56頁 0992022305-0 201137921 [0098] Ο [0099] G [0100] 630與具有奈米碳管結構的載體610正對設置,並形成所 述^米碳管支撐體620,從而使得該奈米碳管支撐體62〇 固疋於所述載體610與固定體630之間。 本發明還提供~種可以製備複數個透射電鏡微栅60的方 、該方去包括以下步驟:(ff 11 0 )提供複數個間隔設 置的載體610,每個載體610具有-第-通孔616;( W120)提供_奈米碳管結構622,並將所述奈米碳管結構 622覆蓋所述複數個載體610的第一通孔616 ; (W130) 提供複數個固定體630 ’使每個固定體63〇與所述載體 610 對應層疊設置,使得所述奈米碳管結構622設置 於所述複數個載體61〇與所述複數個固定體63〇之間;( W140)將每個固定體63〇與所述截艘61〇焊接固定;以及 (W150)斷開所述複數個載體61〇之間的奈米碳管結構 622,從而形成複數個透射電鏡微栅6〇。 其中’所述步驟(Wll〇)、(wl2〇)及(W150)依次與 所述步驟(S110) ' (si2〇)及(S140)的實施方法相 同°其中’所述載體61Ό與所述固定體63{)可以係獨立的 、分離結構;亦可以係—體結構。 所述步驟(W130)的實施方式與所述步驟(W24)的步驟 基本相同。其中’所述固定體630的數量與所述載體610 的數量係相同的’每個載體61〇均與一個固定體630層疊 設置° 所述步驟(W140)的實施方式與步驟(W3〇)的實施方式 基本相同。每個載體61〇均與一個固定體63〇焊接設置。 099112611 表弟編號A0101 第35頁/共56頁 0992022305-0 [0101] 201137921 [_可以理解,第二實施例、第三實施例、第四實施例q 第五實施例亦可以通過上述方法,使所述栽體及固定體 焊接在一起來製備透射電鏡微柵。可以理解,本發明實 施例中的載體與固定體的結構係可以互換的。 [0103] 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:第…所述奈米碳管結構設置於所述載體及固 定體之間,在使用所述透射電鏡微柵時,可以防止挾持 該透射電鏡微柵的器具與所述奈米碳管結構直接接觸, 而由於奈米碳管結構的質量較輕引起該奈米碳管結構的 飄移,同時亦減少了挾持器具對奈米碳管結構的污染, 從而有利於提高採用該透射電鏡微柵的透射電鏡進行成 分分析時的準確性及解析度。第二,所述載體及固定體 通過卡扣、焊接等方式固定在一起,使得所述奈米碳管 結構固定於該載體及固定體之間,奈米碳管結構不至於 飄移,從而更有利於提高採用該透射電鏡微柵的透射電 鏡進行成分分析時的準確性及解折度:第三,本發明實 施例提供的透射電鏡微柵的輯備方法簡單、快捷,比較 容易使得所述奈米碳管結構固定於該透射電鏡微柵中, 而且亦比較容易實現載體與固定體的對準,尤其係比較 容易實現第一通孔與第二通孔的精確對準。 [0104] 综上所述,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。 099112611 表單編號A0101 第36頁/共56頁 0992022305-0 201137921 t圖式簡單說明】 [0105] 圖1係本發明第一實施例提供的透射電鏡微柵的立體分解 圖。 [0106] 圖2係本發明第一實施例提供的透射電鏡微柵的立體圖。 [0107] 圖3係本發明第二實施例提供的透射電鏡微柵的立體分解 圖。 [0108] 圖4係本發明第二實施例提供的透射電鏡微柵的立體圖。 [0109] 〇 圖5係本發明第三實施例提供的透射電鏡微柵的立體分解 圖。 [0110] 圖6係本發明第三實施例提供的透射電鏡微柵的立體圖。 [0111] 圖7係本發明第四實施例提供的透射電鏡微柵的立體分解 圖。 [0112] 圖8係本發明第四實施例提供的透射電鏡微栅的立體圖。 [0113] 圖9係本發明第五實施例提供的透射電鏡微柵的立體分解 圖。 [0114] 圖10係本發明第五實施例提供的透射電鏡微柵的立體圖 〇 [0115] 圖11係本發明第五實施例提供的透射電鏡微柵的製備流 程圖。 [0116] [0117] 圖1 2係本發明第六實施例提供的透射電鏡微柵中的載體 及固定體的立體圖。 圖13係本發明第六實施例提供的透射電鏡微柵的剖面圖 099112611 表單編號A0101 第37頁/共56頁 0992022305-0 [0117] 201137921 [0118] 圖14係本發明第六實施例提供的透射電鏡微柵的製備流 程圖。 【主要元件符號說明】 [0119] 透射電鏡微栅:1〇 ; 20 ; 30 ; 40 ; 50 ; 60 [0120] 載體:110 ; 210 ; 310 ; 410 ; 510 ; 610 [0121] 第一圓片狀本體:111;211;311;511;611 [0122] 第一圓環:112 ; 212 ; 312 ; 412 ; 512 ; 612 [0123] 第一網狀結構:114 ; 314 ; 514 ; 614 [0124] 第一通孔:116 ; 216 ; 316 ; 416 ; 516 ; 616 [0125] 狹縫:118 ; 218 ; 318 ; 418 ; 518 [0126] 奈米碳管支撐體:120 ; 220 ; 320 ; 420 ; 520 ; 620 [0127] 固定體:130 ; 230 ; 330 ; 430 ; 530 ; 1含0 [0128] 第二圓片狀本體:131 ; 231 ; 431 ; 531 ; 631 [0129] 第二圓環:132 ; 232 ; 332 ; 432 ; 532 ; 632 [0130] 第二網狀結構:134 ; 534 ; 634 [0131] 第二通孔:136 ; 236 ; 336 ; 436 ; 536 ; 636 [0132] 卡扣:138 ; 238 ; 338 ; 438 ; 538 [0133] 第三通孔:150 [0134] 第一條狀結構:214 099112611 表單編號A0101 第38頁/共56頁 0992022305-0 201137921It will be appreciated that the carbon nanotube structure 62 may also be at least one carbon nanotube network or one nanocarbon line. The step (W20) includes the steps of: (W21) disposing the carbon nanotube structure 622 on the first surface 618 of the first ring 612 of the carrier 610; (W22) being placed in a container 66〇 The organic solvent 662 processes the carbon nanotube structure 622 covering the first through hole 616 of the carrier 610; (W23) ruining the excess carbon nanotube structure 622 to form the carbon nanotube support 髅The fixing body 630 is disposed on the carbon nanotube support 620 such that the second through hole 636 is at least partially overlapped with the first through hole 616. Specifically, the step (W24) causes the second surface 638 of the second ring 632 to face the "" surface 618 of the first ankle ring 612, and the second through hole 636 is The first through holes 616 are arranged in an overlapping manner one by one. The method specifically adopted in the steps (W21) to (W23) is the same as the method adopted in the evenings (S21) to (S23). The order of the fewer spines (W21), (W22), and (tf23) can be determined as needed. For example, 099112611, the sequence of the nightmare (W21) and the step (W22) can be interchanged with the form number A0101, page 33 / 56 pages 0992022305-0 201137921, that is, the carbon nanotube structure can be treated first with an organic solvent. 622, and then the carbon nanotube structure 6 22 is disposed on the surface of the carrier 610. [0096] Step (W30) specifically includes the following steps: First, a pressure is applied to the first ring 612 and the second ring 632 by a welding system such that the first surface 618 of the first ring 612 is The second surface 638 of the second ring 632 is in line contact; then, welding is performed at a line contact of the first surface gig of the first ring 612 with the second surface 638 of the second ring 632. During the welding process, a large amount of heat is generated at the line contact, and the materials of the first ring 612 and the second ring 632 in the hottest region of the center are quickly heated to a molten state to continue to apply pressure. After the ring 612 and the second ring 632 are cooled, the first ring 612 and the second ring 632 are welded together to form the welding element 640· at the weld. Therefore, the material of the welding element 640 is the same as that of the first ring 612 and the second ring 632. In the present embodiment, the welding system is a spot welding machine, and the welding element 640 is a solder joint. In this step (W30), the contact between the carrier 610 and the fixed body 630 is made by the contact of the wire with the plane, and the alignment of the carrier 61〇 and the fixed body 630 can be relatively easily realized. [0097] In addition, when the carbon nanotube structure 622 provided in the step (W1) comprises a plurality of carbon nanotube membranes or a plurality of nano carbon pipelines, or a plurality of nanotube networks, The preparation method of the transmission electron micro-figure 60 can also be: the step (W10) remains unchanged. The step (w2〇) can be performed by passing a portion of the carbon nanotubes in the nano-tube structure 6 2 2 a gentleman is placed on the first through hole 616 of the carrier 61〇, and another part of the carbon nanotube structure in the carbon nanotube structure 622 is disposed on the second through hole of the fixed body 63〇. 636. Then, the fixed body having a carbon nanotube structure 099112611 Form No. A0101 Page 34 / 56 pages 0992022305-0 201137921 [0099] G [0100] 630 is directly opposite to the carrier 610 having a carbon nanotube structure The carbon nanotube support 620 is disposed and formed such that the carbon nanotube support 62 is clamped between the carrier 610 and the fixed body 630. The present invention also provides a method for preparing a plurality of TEM micro-gates 60, the method comprising the steps of: (ff 11 0 ) providing a plurality of spaced-apart carriers 610, each carrier 610 having a --via 616 (W120) providing a carbon nanotube structure 622, and covering the first via hole 616 of the plurality of carriers 610 with the carbon nanotube structure 622; (W130) providing a plurality of fixing bodies 630' for each The fixing body 63〇 is disposed in a corresponding manner with the carrier 610 such that the carbon nanotube structure 622 is disposed between the plurality of carriers 61〇 and the plurality of fixing bodies 63〇; (W140) each fixed The body 63〇 is welded and fixed to the intercepting vessel 61; and (W150) the carbon nanotube structure 622 between the plurality of carriers 61〇 is broken, thereby forming a plurality of transmission electron micromirrors 6〇. Wherein the steps (W11), (wl2〇), and (W150) are the same as the steps of the steps (S110)' (si2〇) and (S140), wherein the carrier 61Ό and the fixed The body 63{) may be a separate, separate structure; it may also be a body structure. The embodiment of the step (W130) is substantially the same as the step of the step (W24). Wherein the number of the fixed bodies 630 is the same as the number of the carriers 610. Each of the carriers 61 is stacked with a fixed body 630. Embodiments and steps (W3) of the step (W140) The implementation is basically the same. Each carrier 61 is welded to a fixed body 63. 099112611 Cousin No. A0101 Page 35 / Total 56 Page 0992022305-0 [0101] 201137921 [_ It can be understood that the second embodiment, the third embodiment, the fourth embodiment q The fifth embodiment can also be made by the above method The carrier and the fixed body are welded together to prepare a transmission electron microscope microgrid. It will be understood that the structure of the carrier and the anchor in the embodiment of the invention may be interchanged. The TEM micro-gate provided by the embodiment of the present invention and the preparation method thereof have the following advantages: the carbon nanotube structure is disposed between the carrier and the fixed body, and when the TEM micro-gate is used The device for holding the TEM microgrid can be prevented from directly contacting the nano carbon tube structure, and the nano carbon tube structure is drifted due to the light weight of the carbon nanotube structure, and the pair of holding devices is also reduced. The contamination of the carbon nanotube structure is beneficial to improve the accuracy and resolution of the composition analysis using the transmission electron microscopy of the TEM. Secondly, the carrier and the fixing body are fixed together by snapping, welding, etc., so that the carbon nanotube structure is fixed between the carrier and the fixed body, and the carbon nanotube structure is not drifted, thereby being more advantageous. The accuracy and the degree of disassembly of the TEM are improved by using the TEM of the TEM micro-gate. Thirdly, the method for preparing the TEM micro-gate provided by the embodiment of the present invention is simple, quick, and relatively easy to make the The carbon nanotube structure is fixed in the TEM micro-gate, and it is relatively easy to achieve alignment between the carrier and the fixed body, and in particular, it is relatively easy to achieve precise alignment of the first through hole and the second through hole. [0104] In summary, the present invention has indeed met the requirements of the invention patent, and the patent application is filed according to law. 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. 099112611 Form No. A0101 Page 36 of 56 0992022305-0 201137921 t Brief Description of Drawings [0105] FIG. 1 is an exploded perspective view of a TEM micro-gate provided by a first embodiment of the present invention. 2 is a perspective view of a TEM micro-gate provided by a first embodiment of the present invention. 3 is an exploded perspective view of a TEM micro-gate provided by a second embodiment of the present invention. 4 is a perspective view of a TEM micro-gate provided by a second embodiment of the present invention. [0109] FIG. 5 is an exploded perspective view of a TEM micro-gate provided by a third embodiment of the present invention. 6 is a perspective view of a TEM micro-gate provided by a third embodiment of the present invention. 7 is a perspective exploded view of a TEM micro-gate provided by a fourth embodiment of the present invention. 8 is a perspective view of a TEM micro-gate provided by a fourth embodiment of the present invention. 9 is a perspective exploded view of a TEM micro-gate provided by a fifth embodiment of the present invention. 10 is a perspective view of a TEM micro-gate provided by a fifth embodiment of the present invention. [0115] FIG. 11 is a flow chart showing the preparation of a TEM micro-gate provided by a fifth embodiment of the present invention. [0117] FIG. 1 is a perspective view of a carrier and a fixed body in a TEM microgrid according to a sixth embodiment of the present invention. 13 is a cross-sectional view of a TEM micro-gate provided by a sixth embodiment of the present invention. 099112611 Form No. A0101 Page 37/56 of 0992022305-0 [0117] FIG. 14 is a sixth embodiment of the present invention. Flow chart of preparation of TEM micro-gate. [Description of main component symbols] [0119] Transmission electron microstrip: 1 〇; 20; 30; 40; 50; 60 [0120] Carrier: 110; 210; 310; 410; 510; 610 [0121] Body: 111; 211; 311; 511; 611 [0122] First ring: 112; 212; 312; 412; 512; 612 [0123] First mesh structure: 114; 314; 514; 614 [0124] a through hole: 116; 216; 316; 416; 516; 616 [0125] slit: 118; 218; 318; 418; 518 [0126] carbon nanotube support: 120; 220; 320; 420; 520; 620 [0127] Fixed body: 130; 230; 330; 430; 530; 1 with 0 [0128] Second disk-shaped body: 131; 231; 431; 531; 631 [0129] Second ring: 132; 332; 432; 532; 632 [0130] second mesh structure: 134; 534; 634 [0131] second via: 136; 236; 336; 436; 536; 636 [0132] snap: 138; ; 338 ; 438 ; 538 [0133] Third through hole: 150 [0134] First line structure: 214 099112611 Form number A0101 Page 38 / Total 56 page 0992022305-0 201137921

[0135] [0136] [0137] [0138] [0139] [0140] [0141] [0142] [0143] 第二條狀結構:234 第三通孔:250 折疊部:5 5 0 第一表面:618 奈米碳管結構:522 ; 622 第二表面:638 焊接元件:640 容器:560 ; 660 有機溶劑:562 ; 662 ❹ 099112611 表單編號A0101 第39頁/共56頁 0992022305-0[0138] [0140] [0143] [0143] Second strip structure: 234 Third through hole: 250 Folding portion: 5 5 0 First surface: 618 carbon nanotube structure: 522; 622 second surface: 638 welding component: 640 container: 560; 660 organic solvent: 562; 662 ❹ 099112611 Form No. A0101 Page 39 / Total 56 Page 0992022305-0

Claims (1)

201137921 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: 提供一載體、一奈米碳管結構,以及一固定體,所述載體 具有第一通孔,所述固定體具有第二通孔; 將所述固定體與所述載體層疊設置,並將所述奈米碳管結 構設置於所述載體與所述固定體之間;以及 將所述載體及固定體焊接固定。 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, 其中,所述奈米碳管結構包括從奈米碳管陣列中直接抽取 出來的至少一奈米碳管膜或至少一奈米礙管線。 3 .如申請專利範圍第2項所述的透射電鏡微柵的製備方法, 其中,所述奈米碳管結構為至少一奈米碳管線組成的奈米 碳管網狀結構。 4 .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,所述將固定體與所述載體層疊設置的步驟包括將所 述奈米碳管結構覆蓋所述載體的第一通孔的步驟。 5 .如申請專利範圍第4項所述的透射電鏡微柵的製備方法, 其中,進一步包括採用有機溶劑處理覆蓋所述載體的第一 通孔的奈米碳管結構的步驟。 6 .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,層疊設置所述固定體與所述載體時,使所述固定體 的第二通孔與所述載體的第一通孔至少部分重疊。 7 .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,所述固定體與所述載體層疊設置時,所述固定體的 邊緣與所述載體的邊緣形成線與面的接觸。 099112611 表單編號A0101 第40頁/共56頁 0992022305-0 201137921 8 .如申請專利範圍第7項所述的透射電鏡微柵的製備方法, 其中,所述載體包括一第一圓環’該第一圓環具有一第一 表面;所述固定體包括/第二圓環,該第二圓環具有一與 所述第一圓環的第一表面相對設置的第二表面,將所述奈 米碳管結構設置於所述第一圓環的第一表面與所述第二圓 環的第二表面之間,使该第二表面與第一表面形成線與面 的接觸。 9 ·如申請專利範圍第8項所述的透射電鏡微柵的製備方法, 其中,所述第一圓環的第一表面為平面’所述第二圓環的 〇 第二表面為弧形面或棱.缘。 10 . —種透射電鏡微柵的製備方法’包括以下步驟: 提供複數個間隔設置的載體’每個載體具有—第一通孔; 提供一奈米碳管結構,將該奈米碳管結構覆蓋所述複數個 載體的第一通孔; 提供複數個固定體,每個固定體具有一第二通孔,使每個 固定體與所述載體—對應層疊設置,使得所述奈米碳管 結構設置於所述複數個載體與所述複數個固定體之間; 〇 將所述每個固定體與所述載艘焊接固定,以及 斷開所述複數個載體之間的奈米碳管結構,從而形成複數 個透射電鏡微柵。 11 . 12 . 如申請專利範圍第項所述的透射電鏡微柵的製備方法, 其中’所述斷開複數個載體之間的奈米碳管結構的方法為 採用雷射光束照射相鄰的載體之間的奈米碳管結構。 如申請專利範圍第10項所述的透射電鏡微栅的製備方法, 其中,所述斷開複數個載體之間的奈米碳管結構的方法為 採用雷射光束沿著每個载體的外邊沿照射,使覆蓋所述載 099112611 表單編號A0101 第41頁/兴56頁 0992022305-0 201137921 體的奈米碳管結構沿載體的外邊沿斷開。 099112611 表單編號A0101 第42頁/共56頁 0992022305-0201137921 VII. Patent application scope: 1. A method for preparing a transmission electron microstrip, comprising the steps of: providing a carrier, a carbon nanotube structure, and a fixing body, the carrier having a first through hole, the fixing The body has a second through hole; the fixing body is laminated with the carrier, and the carbon nanotube structure is disposed between the carrier and the fixed body; and the carrier and the fixed body are welded fixed. 2. The method of preparing a TEM microgrid according to claim 1, wherein the carbon nanotube structure comprises at least one carbon nanotube film directly extracted from the carbon nanotube array or at least One nanometer obstructs the pipeline. 3. The method of preparing a TEM micro-gate according to claim 2, wherein the carbon nanotube structure is a nano-carbon tube network structure composed of at least one nano carbon line. 4. The method of preparing a TEM micro-gate according to claim 1, wherein the step of laminating the fixed body and the carrier comprises covering the carbon nanotube structure with the carrier. A step of a through hole. 5. The method of producing a TEM microgate according to claim 4, further comprising the step of treating the carbon nanotube structure covering the first through hole of the carrier with an organic solvent. 6. The method for producing a TEM micro-gate according to claim 1, wherein, when the fixing body and the carrier are stacked, the second through hole of the fixing body and the carrier are A through hole at least partially overlaps. 7. The method for producing a TEM micro-gate according to claim 1, wherein the edge of the fixed body forms a line and a surface with the edge of the carrier when the fixed body is stacked with the carrier. s contact. The method of preparing a TEM micro-gate according to claim 7, wherein the carrier includes a first ring 'the first The ring has a first surface; the fixed body includes/the second ring, the second ring has a second surface disposed opposite the first surface of the first ring, the nanocarbon The tube structure is disposed between the first surface of the first ring and the second surface of the second ring such that the second surface forms a line-to-face contact with the first surface. The method of manufacturing the TEM micro-gate according to Item 8, wherein the first surface of the first ring is a plane, and the second surface of the second ring is a curved surface. Or edge. 10 . A method for preparing a TEM micro-grid comprises the steps of: providing a plurality of spaced-apart carriers each having a first through-hole; providing a carbon nanotube structure to cover the carbon nanotube structure a plurality of first through holes of the plurality of carriers; a plurality of fixing bodies are provided, each of the fixing bodies having a second through hole, such that each of the fixing bodies and the carrier are stacked correspondingly, so that the carbon nanotube structure Provided between the plurality of carriers and the plurality of fixing bodies; 焊接 fixing each of the fixing bodies to the carrier, and disconnecting the carbon nanotube structure between the plurality of carriers, Thereby a plurality of TEM micro-gates are formed. 11. The method for preparing a TEM micro-grid according to the invention of claim 1, wherein the method of disconnecting the carbon nanotube structure between the plurality of carriers is to irradiate the adjacent carrier with a laser beam The structure of the carbon nanotubes between them. The method for preparing a TEM micro-gate according to claim 10, wherein the method of disconnecting the carbon nanotube structure between the plurality of carriers is to use a laser beam along each carrier The edge of the carrier is closed along the outer edge of the carrier covering the carrier 099112611 Form No. A0101 Page 41 / Hing 56 Page 0992022305-0 201137921. 099112611 Form No. A0101 Page 42 of 56 0992022305-0
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