201108296 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，尤其涉及—種可用於加 熱樣品之透射電鏡微柵。 【先前技# [0002]隨著材料技術尤其係奈米材料技術之發展，常需要觀測 材料樣品於不同溫度下之結構特徵。譬如，金屬材料於 奈米級時，其熔點會隨著粒徑之變化而變化，即該金屬 0 材料於奈米級時其於不同溫度下之結構特徵有所不同。 再譬如，許多催化劑於不同溫度下之活性有所差別即 該催化劑於不同溫度下之結構有所不同。故，在對該材 料樣品進行結構表徵時，不僅需要觀測該材料於室溫下 之結構，還需要觀察該材料樣品於不同溫度下之結構。 即於觀察過程中需要對該材料樣品進行加熱。 [〇〇〇3]透射電子顯微鏡係表徵材料樣品結構之一種重要工具， 通過透射電子顯微鏡賴觀測_材料樣品之高解析度 〇 <透射電鏡圖像。於該透射電子顯微射，該材料樣品 -般放置於-微栅表面。於給該材料樣品加熱時，將該 微柵放置於-加熱爐中或於該微栅周圍設置—加熱棒， 利肋加減對該㈣樣品進行加熱。可㈣解，於給 4材料樣品加熱之過程中，該微柵也同時被加熱。 [0004] 在先剛技術中，應用於透射電子顯微鏡之微柵通常係於 銅網或_等金屬_上覆蓋-層多孔有顏，再在該 有機膜上蒸鑛~~層非晶碳膜製成的。然，先前之透射電 子顯微鏡之熱穩定性不夠好，由於該金屬網格、有機膜 098129178 表單編號A0101 第3頁/共24頁 0982050027-0 201108296 及碳膜之熱容«膨脹係數不―樣，該柵網_ 該峡膜、有機膜與金屬網袼之形變合 '' /I 9不—致，從而造成 放置於該微柵表面之材料樣品產生漂移。即該材料樣。 於受熱過程中，會相對該透射電子顯微鏡產生移動。2 錄之膨脹係數遠大於非晶伽，其於受熱時 7〇隻大於 碳膜，從而導致放置其上之非晶销移動，從而使吸附 或放置於碳膜表面之材料樣品移動。然而，由於嗜透射 電子顯微鏡對材料樣品之移動非常敏感，該材^品: 受熱時產生之漂移，將使該透射電子顯微鏡難以得到高 清晰之透射電鏡圖像。V卜^ ^ ^ 门 【發明内容】 [0005] 有鑒於此，提供一種具有較好之熱穩定性之透射電鏡微 柵實為必要。 [0006] 一種透射電鏡微栅，其包括一網格、一奈米碳管臈狀結 構及至少兩個電極。該紊米碳管膜狀結構設置於該網格 表面。該至少兩個電極間隔設置jL分別與該奈米碳管膜 狀結構電連接。該奈米碳f膜狀結構包括複數均勻分佈 之奈米碳管’該複數条米碳管形成複數微孔。 [0007] —種透射電鏡微栅，其包括一網格、一奈米碳管臈狀鲈 構及兩個電極。該奈米碳管膜狀結構設置於該網格表面 。該兩個電極間隔設置且分別與該奈米碳管膜狀結構電 連接。該奈米碳管膜狀結構包括複數奈米礙管基本垂直 地交又設置，該複數奈米碳管形成複數微孔。 [0008]201108296 VI. Description of the Invention: [Technical Field] [0001] The present invention relates to a TEM micro-gate, and more particularly to a TEM micro-gate that can be used to heat a sample. [Previous Technology # [0002] With the development of material technology, especially nanomaterial technology, it is often necessary to observe the structural characteristics of material samples at different temperatures. For example, when the metal material is at the nanometer level, its melting point changes with the change of the particle size, that is, the metal 0 material has different structural characteristics at different temperatures at the nanometer level. For example, many catalysts differ in their activity at different temperatures, i.e., the structure of the catalyst varies at different temperatures. Therefore, in the structural characterization of the material sample, it is not only necessary to observe the structure of the material at room temperature, but also to observe the structure of the material sample at different temperatures. That is, the material sample needs to be heated during the observation process. [〇〇〇3] Transmission electron microscopy is an important tool for characterizing the structure of material samples. It is observed by transmission electron microscopy _ high resolution of material samples 〇 < transmission electron microscopy images. For this transmission electron microscopy, the material sample is placed on the -microgrid surface. When the material sample is heated, the micro grid is placed in a heating furnace or a heating rod is disposed around the micro grid, and the (four) sample is heated by a rib addition or subtraction. (4) The micro-gate is also heated during the heating of the material sample. [0004] In the prior art, the microgrid applied to the transmission electron microscope is usually attached to a copper mesh or a metal layer, and the layer is porous, and then the mineral film is vaporized to a layer of amorphous carbon film. Made of. However, the thermal stability of the previous transmission electron microscope is not good enough, because the metal grid, organic film 098129178 Form No. A0101 Page 3 / 24 pages 0982050027-0 201108296 and the heat capacity of the carbon film «the expansion coefficient is not the same, The grid _ the isotropic film, the organic film and the metal mesh are deformed in combination with '' / I 9 ', resulting in drift of the material sample placed on the surface of the micro-gate. That is, the material is the same. During the heating process, movement occurs relative to the transmission electron microscope. 2 The coefficient of expansion is much larger than that of amorphous gamma, which is larger than the carbon film when heated, causing the amorphous pin placed thereon to move, thereby moving the sample of material adsorbed or placed on the surface of the carbon film. However, since the transmission electron microscope is very sensitive to the movement of the material sample, the material: drift caused by heat, making it difficult to obtain a high-definition TEM image of the transmission electron microscope. [Bu] ^ ^ ^ Gate [Summary of the Invention] [0005] In view of this, it is necessary to provide a TEM microgrid with better thermal stability. A TEM microgrid comprising a grid, a carbon nanotube-shaped structure, and at least two electrodes. The membranous carbon tube membrane structure is disposed on the surface of the mesh. The at least two electrode spacing arrangements jL are electrically connected to the carbon nanotube film structure, respectively. The nanocarbon f film structure includes a plurality of uniformly distributed carbon nanotubes. The plurality of carbon nanotubes form a plurality of micropores. [0007] A TEM microgrid comprising a grid, a carbon nanotube-shaped structure, and two electrodes. The carbon nanotube film structure is disposed on the surface of the mesh. The two electrodes are spaced apart and electrically connected to the carbon nanotube film structure, respectively. The carbon nanotube film structure comprises a plurality of nano tubes which are arranged substantially perpendicularly, and the plurality of carbon tubes form a plurality of micropores. [0008]
相較於先前技術’該透射電鏡微栅利用一奈米碳管膜狀 098129178 結構承載及加熱放置於其表面之待觀察之材料樣品 表單編號A0101 第4頁/共24頁 。該 0982050027-0 201108296 Λ ❹[：_] 不未碳管膜狀結構具有較高之電熱轉換率且直接加熱該 材料樣品無需加熱整個透射電鏡微栅，即無需加埶網格 ’故於加熱過程中產生之熱量較少；同時該奈米碳管膜 狀結構具有較小之_脹餘。故，在加歸料樣品時 ’由於該奈米碳管膜狀結構產生之熱量較少且具有較小 之熱膨脹係數，其因受熱而產生之形變較小，故，㈣ 避免放置於該奈求碳管驗結構表面之材料樣品產生漂 移。 【實施方式】 以下將結合附圖對本發明作進一步之詳細說明。 [0010] 請參閱圖1及圖2，本發明實施例提供一種透射電鏡微柵 1〇〇，其包括一網格110、一奈米碳管膜狀結構13〇及兩 個電極120。該奈米碳管膜狀結構130設置於該網格110 之一表面。該兩個電極120間隔設置且分別與該奈米碳管 膜狀結構130電連接。 [0011] ❹ 該網格110具有至少―埽孔111使該奢牵碳管膜狀結構 13 0部分懸空設置，該通孔111之孔徑於1微米〜3毫米之 間。該網格110之形狀不限，可選擇為圓形、方形、橢圓 形等。該網格110之尺寸不限，可根據實際應用需求調整 ，通常應用於透射電子顯微鏡中，該網格110之尺寸為3 毫米。在本實施例中，該網格110為一圓形之多孔結構， 包括複數均勻分佈之通孔111，每一通孔111之孔徑於80 微米〜100微米之間。該網格110與奈米碳管膜狀結構130 之間絕緣。為使該網格110與奈米碳管膜狀結構130絕緣 ，可於該網格110表面形成一由絕緣耐熱材料製成之絕緣 098129178 表單編號A0101 第5頁/共24頁 0982050027-0 201108296 層，也可使整個網格110由絕緣耐熱材料製成。該絕緣耐 熱材料可為一絕緣之無機非金屬材料。具體地，該絕緣 耐熱材料包括二氧化矽、氧化矽、氮化矽、陶瓷、石英 及玻璃中之一種及任意組合。優選地，該網格11〇之熱膨 脹係數絕對值小於3，從而使該網格11〇於受熱時不容易 產生變形。在本實施例中，該網格11〇為由陶瓷製成之栅 網結構。 [0012] 该兩個電極120設置於該奈米碳管膜狀結構13〇相對之兩 端並與该奈米碳管膜狀結構130電連接。該兩個電極12〇 可設置於網格110與奈米碳管膜狀結構130之間，也可設 置於该奈米碳管膜狀結構丨3〇遠離該網格〗10之一側或將 該兩個電極120設置於該網格11〇與該奈米碳管膜狀結構 130相背之一側，當該兩個電極12〇設置於網格u〇與奈 米碳管膜狀結構13〇之間時，該兩個電極12〇可通過於該 網格110表面絲網印刷導電銀漿屬而形成。優選地，該通 過絲網印刷而形成之電極120，其本度為2奈求〜5〇奈米。 在本實施例中，該兩個電極12〇設置於網格11〇與奈米碳 管膜狀結構130之間，且該電極12〇設置於該網格11〇靠 近外緣之位置。優選地，該兩個電極12_接於該網格 110中且與該奈米碳管膜狀結構130相對之兩端電連接， 可以理解’此時，該網格Π0©向該奈米碳管膜狀結構 130應具有與該兩個電極12〇相對應之凹槽。該兩個電極 120嵌入該凹槽内，並保證該兩個電極】20面向該奈米碳 管膜狀結構130之表面與該網格110面向該奈米碳管膜狀 結構130之表面平齊’從而使該奈求碳管膜狀結構130平 098】29]78 表單編號A0101 苐6頁/共24頁 0982050027-0 201108296 [0013] Ο Ο [0014] [0015] 098129178 整地鋪設於該網格110表面。該兩個電極120之形狀不限 ’優選地，該兩個電極120為弧形電極，設置於該網格 110靠近邊緣之位置，從而使該網格110表面之奈米碳管 膜狀結構130得到充分利用，得到最大之加熱面積。另外 ’該透射電鏡微柵100還可包括多對電極120依次排佈於 該網格110外緣，此時，相鄰之兩對電極〗2〇彼此併聯。 該奈米碳管膜狀結構130鋪設於該網格11〇表面，覆蓋該 網格110之通孔111，並通過該通孔111部分懸空設置。 具體地’該奈米碳管膜狀結構13〇於覆蓋該網格110之通 孔111之位置懸空設置。該奈米碳管膜狀結構130包括複 數均勻分佈之奈米碳管，該複數奈米碳管之間通過凡德 瓦爾力相互吸引搭接，從而形成一自支撐之奈米碳管膜 狀結構130 ’該複數奈米碳管形成複數孔徑於丨奈米〜1微 米之間之微孔。可以理解，每一微孔由相鄰之奈米碳管 形成’故該微孔為多邊形或不規則形狀。優選地，該奈 米碳管膜狀結構“!)之厚度小於100奈米。所謂“自支撐 即該奈米碳管膜狀結構130無需通過設置於一基體表面 也能保持自身特定之形狀。 具體地’該奈米碳管骐狀結構130可包括至少一層奈米碳 管膜。該奈米碳管膜可為一奈米碳管絮化膜、奈米碳管 儀壓膜或奈米碳管拉骐。 °月參閱圖3 ’該奈米碳管絮化膜包括複數相互纏繞且均勻 分佈之奈米碳管。該奈米碳管之間通過凡德瓦爾力相互 吸引、纏繞，形成網路狀結構，以形成一自支撐之奈米 峻管絮化膜。該奈米碳管絮化膜各向同性。該奈米碳管 表單編號 A_1 % 7 24 % 0982050027-0 201108296 絮化膜可通過對一奈米碳管陣列絮化處理而獲得。 [0016] 該奈米碳管碾壓膜包括複數奈米碳管無序排列、沿一個 方向擇優取向排列或沿複數方向擇優取向排列，相鄰之 奈米碳管通過凡德瓦爾力結合。該奈米碳管碾壓膜可採 用一平面壓頭沿垂直於上述奈米碳管陣列生長之基底之 方向擠壓上述奈米碳管陣列而獲得，此時該奈米碳管碾 壓膜中之奈米碳管無序排列，該奈米碳管碾壓膜各向同 性；該奈米碳管碾壓膜也可採用一滾軸狀壓頭沿某一固 定方向碾壓上述奈米碳管陣列而獲得，此時該奈米碳管 碾壓膜中之奈米碳管於該固定方向擇優取向；請參閱圖4 ，該奈米碳管碾壓膜還可採用滾軸狀壓頭沿不同方向碾 壓上述奈米碳管陣列而獲得，此時該奈米碳管碾壓膜中 之奈米碳管沿不同方向擇優取向。 [0017] 請參閱圖5，該奈米碳管拉膜包括複數基本相互平行且基 本平行於奈米碳管拉膜表面排列之奈米碳管。具體地， 該奈米碳管拉膜包括複數奈米碳管通過凡德瓦爾力首尾 相連且基本沿同一方向擇優取向排列。該奈米碳管拉膜 可通過從奈米碳管陣列中直接拉取獲得，為一自支撐結 構。當該奈米碳管膜狀結構1 3 0為一奈米碳管膜時，該兩 個電極120間隔設置於奈米碳管膜之兩端，該奈米碳管膜 中之複數奈米碳管之軸向基本沿一個電極1 20向另一個電 極延伸12 0。 [0018] 進一步地，該奈米碳管膜狀結構130可包括複數奈米碳管 膜層疊設置，相鄰之奈米碳管膜通過凡德瓦爾力結合。 當該奈米碳管膜狀結構包括複數奈米碳管拉膜時，優選 098129178 表單編號A0101 第8頁/共24頁 0982050027-0 201108296 地’該奈米碳管膜狀結構包括之奈米碳管膜之層數小於 或等於ίο層。該奈米碳管膜狀結構中相鄰之奈米碳管拉 膜中之奈米碳管之間具有一交叉角“，且該“大於〇度 且小於等於90度。當相鄰之奈米碳管拉臈中之奈米碳管 之間具有-交叉角度《時，該奈米碳管相互交織形成一 網狀結構，使該奈米碳管膜狀結構13〇之機械性能增加， 同時使該奈米碳管膜狀結構13〇具有複數均勻且規則排佈 之微孔，該微孔之孔徑與奈米碳管拉媒之層數有關，層 數越多，微孔之孔徑越小。該奈米碳管骐還可進一步進 ® 行有機溶劑處理，使該杳米碳管膜收縮’增加該奈米碳 管膜之強度。在本實施例中，該奈米碳營膜狀結構13〇包 括至少兩層奈米碳管拉膜層疊設置，相鄰之奈米碳管膜 中之奈米碳管之間之交又角度α大致等於9〇度，形成一 網狀結構，即相鄰之奈米碳管膜中之奈米碳管大致相互 垂直。 [0019] 請參閱圖6至圖8，本發明實施例透射電鏡微柵結構1〇〇中 Q 之奈米碳管膜狀結構130為四層奈米碳管拉膜以9〇度角交 叉層@形成之網狀結構。每一層奈米碳管拉膜中之奈米 碳管均定向排列，相鄰兩奈米碳管拉膜之間通過凡德瓦 爾力結合，相鄰奈米碳管膜中之奈米碳管基本垂直地交 叉設置。該奈米碳管拉膜中之奈米碳管聚集成束，該奈 米碳管膜狀結構130中奈米碳管束交叉形成複數微孔結構 ，該微孔孔徑於1奈米~1微米之間。 [0020] 本實施例透射電鏡微栅100在應用時，一待觀察之材料樣 品承放於該奈米碳管膜狀結構130表面，當該材料樣品之 098129178 表單編號Α0101 第9更/共24頁 0982050027-0 201108296 尺寸大於該奈米碳管膜狀結構⑽ … 膜狀結構130中之微孔可支持該日、 品之尺寸小於該奈米碳管膜狀社構^品’而當該材料樣 粒徑小於5^㈣叫 之微糾，尤其係 管懸靠奈米碳 附作用被穩疋地吸附於奈米碳管管 使其承放於、 _色顆_觀察之：=: [0021] 當需要觀察該材料樣品成也± 電極l?n垃 ；又*、、、時之結構時，通過該兩個 入々電源，使-電流通過該兩個電極12〇傳導 ㈣咖，該奈米碳管膜狀結構⑽在 極小\厂。作為加熱單元之奈米碳管膜狀結構13〇具有 之早位面積熱容，較高之電熱轉換率及較快之溫度 =:且該奈米碳管膜狀結構⑽與材料樣品直接接觸， 給:=狀結構130發出之熱_直接、快速傳遞 :n/ 、能源利用率高。斤時，該奈米碳管膜狀 ％成之網狀結構具有較好之機械穩定性該奈米 石厌:膜狀結構13〇具有極小之熱膨脹係數絕對值具體地 °亥不米奴官膜狀結構130之熱膨脹係數絕對值範圍為 0.01〜0.5。故，該奸扭 ^ 枓樣品在受熱時，奈米碳管膜狀結 構130不容易產生形變。 該透射電鏡微柵利用—奈米碳管膜狀結構承載及加熱放 置於其表面之待觀察之材料樣品。該奈米碳管膜狀結構 具有較馬之電熱轉換率且直接加熱該材料樣品無需加熱 098129178 表單褊號A0101 第10頁/共24頁 0982050027-0 [0022] 201108296 jE'個透射電鏡微柵，即不♦毋 中產生之熱量較少；同時:太加熱網格’故於加熱過程 之熱膨脹係數。故，於管膜狀結構具有較小 管膜狀結構產生之熱量H 時，由於該奈米碳 其因受熱而產生之_心具有較小之熱膨服係數， 米碳管肺、’故’㈣㈣放置於該奈 .^ 材料樣品產生漂移。進-步地， 由於該網格也選用膨脹係數 數鮫小之陶瓷製成，且於加熱 =科樣品時’並不需要加熱該網格，朗格僅於靠近該 Ο 不未碳管膜狀結構之部分㈣熱量，即吸收之熱量非常 少’從而使該網格其因受熱㈣ 小該奈米碳管膜狀結構與網格之間因㈣變而產生之相 對移動，進-步避免放置於該奈米碳管膜麟構表面之 材料樣品產生漂移。 [_综上所述，本發日㈣已符合發明專利之要件，遂依法提 出專利申請。惟，以上所碟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 〇 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β 【圖式簡單說明】 [0024] 圖1為本發明實施例透射電鏡微栅之結構示意圖。 [0025] 圖2為圖1中透射電鏡微柵沿Π-Π線之剖視圖。 _ W3為圖1中透射電鏡微柵中用作奈米碳管膜狀結構之奈 米碳管絮化膜之掃描電鏡照片。 [_ ®4為圖1中透射電鏡微柵中用作奈米碳管膜狀結構之奈 098129178 表單編號Α0101 第11頁/共24頁 0982050027-0 201108296 米碳管碾壓膜之掃描電鏡照片。 [0028] 圖5為圖1中透射電鏡微柵中用作奈米碳管膜狀結構之奈 米碳管拉膜之掃描電鏡照片。 [0029] 圖6為本發明實施例透射電鏡微柵之掃描電鏡照片。 [0030] 圖7為圖6中之透射電鏡微栅中之奈米碳管膜狀結構之透 射電鏡照片。 [0031] 圖8為承載樣品之奈米碳管膜局部放大示意圖。Compared to the prior art, the TEM microgrid utilizes a carbon nanotube film 098129178 structure to carry and heat the sample of the material to be observed placed on its surface. Form No. A0101 Page 4 of 24 The 0982050027-0 201108296 Λ ❹[:_] does not have a carbon tube membrane structure with a high electrothermal conversion rate and directly heats the material sample without heating the entire TEM microgrid, ie no need to twist the grid 'so the heating process The heat generated is less; at the same time, the carbon nanotube membrane structure has a smaller amount of expansion. Therefore, when the sample is returned, the heat generated by the film structure of the carbon nanotube is less and has a smaller coefficient of thermal expansion, and the deformation due to heat is smaller. Therefore, (4) avoiding the placement in the sample. The carbon tube examines the material sample on the surface of the structure to drift. [Embodiment] Hereinafter, the present invention will be further described in detail with reference to the accompanying drawings. Referring to FIG. 1 and FIG. 2, an embodiment of the invention provides a TEM micro-gate 1 〇〇 comprising a grid 110, a carbon nanotube film structure 13 〇 and two electrodes 120. The carbon nanotube film structure 130 is disposed on one surface of the mesh 110. The two electrodes 120 are spaced apart and electrically connected to the carbon nanotube film structure 130, respectively. [0011] The grid 110 has at least a bore 111 for partially vacating the extra large carbon tube film structure 130, and the through hole 111 has a pore diameter of between 1 micrometer and 3 millimeters. The shape of the mesh 110 is not limited and may be selected from a circle, a square, an ellipse, and the like. The size of the grid 110 is not limited and can be adjusted according to actual application requirements, and is generally applied to a transmission electron microscope having a size of 3 mm. In the present embodiment, the grid 110 is a circular porous structure including a plurality of uniformly distributed through holes 111 each having a diameter of between 80 micrometers and 100 micrometers. The grid 110 is insulated from the carbon nanotube film structure 130. In order to insulate the grid 110 from the carbon nanotube film structure 130, an insulation made of an insulating heat-resistant material may be formed on the surface of the grid 110. 098129178 Form No. A0101 Page 5 of 24 pages 0992050027-0 201108296 Layer It is also possible to make the entire mesh 110 made of an insulating heat-resistant material. The insulating heat resistant material can be an insulating inorganic non-metallic material. Specifically, the insulating heat resistant material includes one or any combination of cerium oxide, cerium oxide, cerium nitride, ceramic, quartz, and glass. Preferably, the grid 11 has an absolute thermal expansion coefficient of less than 3, so that the grid 11 is less susceptible to deformation when heated. In the present embodiment, the grid 11 is a grid structure made of ceramic. [0012] The two electrodes 120 are disposed at opposite ends of the carbon nanotube film structure 13 and electrically connected to the carbon nanotube film structure 130. The two electrodes 12〇 may be disposed between the grid 110 and the carbon nanotube film structure 130, or may be disposed on the side of the carbon nanotube film structure 〇3〇 away from the grid 〖10 or The two electrodes 120 are disposed on one side of the grid 11 相 opposite to the carbon nanotube film structure 130, and the two electrodes 12 〇 are disposed on the grid u〇 and the carbon nanotube film structure 13 The two electrodes 12A can be formed by screen printing a conductive silver paste on the surface of the grid 110. Preferably, the electrode 120 formed by screen printing has a degree of 2 to 5 nanometers. In this embodiment, the two electrodes 12A are disposed between the grid 11〇 and the carbon nanotube film structure 130, and the electrode 12〇 is disposed at a position close to the outer edge of the grid 11〇. Preferably, the two electrodes 12_ are connected to the grid 110 and are electrically connected to opposite ends of the carbon nanotube film structure 130. It can be understood that, at this time, the grid is directed to the nanocarbon. The tubular film structure 130 should have grooves corresponding to the two electrodes 12A. The two electrodes 120 are embedded in the recess, and the surface of the two electrodes 20 facing the carbon nanotube film 130 is flush with the surface of the grid 110 facing the carbon nanotube film 130. 'Therefore, the carbon nanotube film structure 130 is flat 098】29]78 Form No. A0101 苐6 pages/ Total 24 pages 0992050027-0 201108296 [0013] Ο Ο [0014] [0015] 098129178 The whole land is laid on the grid 110 surface. The shape of the two electrodes 120 is not limited. Preferably, the two electrodes 120 are arc-shaped electrodes disposed at a position close to the edge of the mesh 110, so that the carbon nanotube film structure 130 on the surface of the mesh 110 Get the most out of it and get the largest heating area. In addition, the TEM micro-gate 100 may further include a plurality of pairs of electrodes 120 arranged in sequence on the outer edge of the grid 110. At this time, two adjacent pairs of electrodes are connected in parallel with each other. The carbon nanotube film structure 130 is laid on the surface of the grid 11 , covers the through hole 111 of the grid 110 , and is partially suspended by the through hole 111 . Specifically, the carbon nanotube film structure 13 is suspended from a position covering the through hole 111 of the mesh 110. The carbon nanotube film structure 130 includes a plurality of uniformly distributed carbon nanotubes, and the plurality of carbon nanotubes are attracted to each other by a van der Waals force to form a self-supporting carbon nanotube film structure. 130 ' The plurality of carbon nanotubes form micropores having a plurality of pore sizes between 丨 nanometers and 1 micrometer. It will be understood that each of the micropores is formed by adjacent carbon nanotubes so that the micropores are polygonal or irregular in shape. Preferably, the thickness of the carbon nanotube film structure "!" is less than 100 nm. The so-called "self-supporting", the carbon nanotube film structure 130 can maintain its own specific shape without being disposed on a substrate surface. Specifically, the carbon nanotube-shaped structure 130 may include at least one layer of carbon nanotube film. The carbon nanotube film can be a carbon nanotube film, a carbon nanotube film or a carbon nanotube. Referring to Figure 3, the carbon nanotube flocculation membrane comprises a plurality of carbon nanotubes intertwined and uniformly distributed. The carbon nanotubes are attracted and entangled by van der Waals forces to form a network structure to form a self-supporting nano tube flocculation film. The carbon nanotube film is isotropic. The carbon nanotube form number A_1 % 7 24 % 0982050027-0 201108296 The flocculated membrane can be obtained by flocculation of a carbon nanotube array. [0016] The carbon nanotube rolled film comprises a plurality of carbon nanotubes arranged in disorder, arranged in a preferred orientation in one direction or in a preferred orientation in a complex direction, and the adjacent carbon nanotubes are combined by a van der Waals force. The carbon nanotube rolled film can be obtained by extruding the carbon nanotube array in a direction perpendicular to the substrate grown by the carbon nanotube array in a planar indenter, and the carbon nanotube is laminated in the film. The carbon nanotubes are disorderly arranged, and the carbon nanotube film is isotropic; the carbon nanotube rolled film can also be rolled in a fixed direction by using a roller-shaped indenter. Obtained by the array, at which time the carbon nanotubes in the carbon nanotube rolled film are preferentially oriented in the fixed direction; referring to FIG. 4, the carbon nanotube rolled film may also adopt a roller-shaped indenter along different The direction is obtained by rolling the above-mentioned carbon nanotube array, and the carbon nanotubes in the carbon nanotube rolled film are preferentially oriented in different directions. [0017] Referring to FIG. 5, the carbon nanotube film comprises a plurality of carbon nanotubes which are substantially parallel to each other and are substantially parallel to the surface of the carbon nanotube film. Specifically, the carbon nanotube film comprises a plurality of carbon nanotubes connected end to end by van der Waals force and arranged in a preferred orientation along substantially the same direction. The carbon nanotube film can be obtained by pulling directly from the carbon nanotube array and is a self-supporting structure. When the carbon nanotube film structure 130 is a carbon nanotube film, the two electrodes 120 are disposed at two ends of the carbon nanotube film, and the plurality of nano carbons in the carbon nanotube film The axial direction of the tube extends substantially 12 along one electrode 110 to the other electrode. [0018] Further, the carbon nanotube film structure 130 may include a plurality of carbon nanotube film laminates, and adjacent carbon nanotube films are bonded by van der Waals force. When the carbon nanotube film structure comprises a plurality of carbon nanotube film, preferably 098129178 Form No. A0101 Page 8 / Total 24 page 0992050027-0 201108296 Ground 'The carbon nanotube film structure includes the nano carbon The number of layers of the tubular film is less than or equal to the ίο layer. The carbon nanotubes in the adjacent carbon nanotube film in the carbon nanotube film structure have an intersection angle ", and the "is greater than the twist and less than or equal to 90 degrees. When the carbon nanotubes in the adjacent carbon nanotubes have a -cross angle between the carbon nanotubes, the carbon nanotubes are interwoven to form a network structure, so that the carbon nanotube membrane structure 13 The mechanical properties are increased, and the carbon nanotube film structure 13〇 has a plurality of uniform and regularly arranged micropores, and the pore diameter of the micropores is related to the number of layers of the carbon nanotubes, and the number of layers is micro. The smaller the aperture of the hole. The carbon nanotubes can be further processed by an organic solvent to shrink the carbon nanotube film to increase the strength of the carbon nanotube film. In this embodiment, the nanocarbon camp membrane 13 〇 includes at least two layers of carbon nanotube film laminated, and the angle between the carbon nanotubes in the adjacent carbon nanotube film is α Roughly equal to 9 degrees, a network structure is formed, that is, the carbon nanotubes in the adjacent carbon nanotube film are substantially perpendicular to each other. Referring to FIG. 6 to FIG. 8 , in the TEM of the embodiment of the present invention, the carbon nanotube film structure 130 of the Q in the micro-gate structure is a four-layer carbon nanotube film with a 9-degree angle crossing layer. @Formed mesh structure. The carbon nanotubes in each layer of carbon nanotube film are oriented, and the adjacent two carbon nanotubes are bonded by van der Waals force, and the carbon nanotubes in the adjacent carbon nanotube film are basically Vertically cross settings. The carbon nanotubes in the carbon nanotube film are aggregated into a bundle, and the carbon nanotube bundles in the carbon nanotube membrane structure 130 intersect to form a plurality of microporous structures, and the pore diameter is from 1 nm to 1 μm. between. [0020] In the present embodiment, when the TEM microgrid 100 is applied, a sample of the material to be observed is placed on the surface of the carbon nanotube film structure 130, when the material sample is 098129178, the form number is Α0101, the 9th/total 24 Page 0982050027-0 201108296 The size is larger than the carbon nanotube film structure (10) ... The micropores in the film structure 130 can support the day, the size of the product is smaller than the nano carbon tube film structure, and when the material The sample particle size is less than 5^(4), which is called micro-correction. In particular, the tube-supported nano-carbon attachment is stably adsorbed on the carbon nanotube tube to be placed on it, _color _ observation:=: [0021 When it is necessary to observe that the material sample is also ±electrode l?n waste; and *,,, and the time structure, through the two input power sources, the current is conducted through the two electrodes 12 (four) coffee, the nai The carbon tube membrane structure (10) is at a very small plant. The carbon nanotube film structure 13 as a heating unit has an early surface area heat capacity, a higher electrothermal conversion rate and a faster temperature =: and the carbon nanotube film structure (10) is in direct contact with the material sample, Give: the heat generated by the = structure 130 _ direct, fast transfer: n /, high energy efficiency. At the time of jin, the nano-carbon tube membrane-like mesh structure has good mechanical stability. The nano-stone is anaerobic: the membrane-like structure 13 〇 has a very small thermal expansion coefficient, and the absolute value is specifically The thermal expansion coefficient of the structure 130 has an absolute value ranging from 0.01 to 0.5. Therefore, when the sample is heated, the carbon nanotube film structure 130 is less likely to be deformed. The TEM microgrid utilizes a carbon nanotube film structure to carry and heat a sample of the material to be observed placed on its surface. The carbon nanotube film structure has a higher electrothermal conversion rate and directly heats the material sample without heating 098129178 Form No. A0101 Page 10 / Total 24 page 0992050027-0 [0022] 201108296 jE' TEM microgrid, That is to say, the heat generated in the crucible is less; at the same time: the heating coefficient of the heating grid is too heated. Therefore, when the tubular membrane structure has a small heat generated by the tubular membrane-like structure, since the nanocarbon is heated due to heat, the core has a small thermal expansion coefficient, and the carbon nanotubes are lungs, 'so' (d) (d) placed in the na.. material sample drift. Step by step, because the grid is also made of ceramic with a small expansion coefficient, and when heating = the sample, 'there is no need to heat the grid, Lange is only close to the Ο, no carbon tube film Part of the structure (4) heat, that is, the amount of heat absorbed is very small', so that the grid is heated by heat (4). The relative movement between the membrane structure of the carbon nanotube and the grid due to (4) changes, and further avoids placement. A sample of the material on the surface of the carbon nanotube film is drifted. [_ In summary, this issue (4) has met the requirements of the invention patent and has filed a patent application in accordance with the 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 in this case. Equivalent modifications or variations made by those skilled in the art of the present invention should be included in the scope of the following claims. [FIG. 1] FIG. 1 is a transmission electron microscope according to an embodiment of the present invention. Schematic diagram of the structure of the micro grid. 2 is a cross-sectional view of the TEM micro-gate of FIG. 1 along a Π-Π line. [0025] FIG. _ W3 is a scanning electron micrograph of a carbon nanotube flocculation film used as a film structure of a carbon nanotube in the transmission electron microstrip of Fig. 1. [_®4 is used as a carbon nanotube film-like structure in the TEM microgrid in Fig. 1 098129178 Form No. Α0101 Page 11 of 24 0982050027-0 201108296 Scanning electron micrograph of a carbon tube rolled film. 5 is a scanning electron micrograph of a carbon nanotube film used as a film structure of a carbon nanotube in the TEM microgrid of FIG. 1. 6 is a scanning electron micrograph of a transmission electron microstrip micro-gate according to an embodiment of the present invention. 7 is a transmission electron micrograph of a film structure of a carbon nanotube in the TEM microgrid of FIG. 6. [0031] FIG. 8 is a partially enlarged schematic view of a carbon nanotube film carrying a sample.
[0032] 圖9為應用本發明實施例透射電鏡微栅觀察奈米金顆粒之 高分辨透射電鏡照片。 【主要元件符號說明】 [0033] 透射電鏡微柵 100 網格 110 通孔 111 電極 120 奈米碳管膜狀結構 1309 is a high-resolution transmission electron micrograph of a nano-particle observed by a transmission electron microstrip micro-gate according to an embodiment of the present invention. [Major component symbol description] [0033] TEM microgrid 100 Grid 110 Through hole 111 Electrode 120 Carbon nanotube film structure 130
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