TWI400738B - Transmission electron microscope grid - Google Patents
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本發明涉及一種透射電鏡微柵，尤其涉及一種可用於加熱樣品之透射電鏡微柵。 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.
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。 With the development of materials 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 material has different structural characteristics at different temperatures at the nanometer level. For example, many catalysts differ in their activity at different temperatures, ie, the structure of the catalyst varies at different temperatures. Therefore, when structurally characterizing 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.
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能夠觀測到該材料樣品之高解析度之透射電鏡圖像。於該透射電子顯微鏡中，該材料樣品一般放置於一微柵表面。於給該材料樣品加熱時，將該微柵放置於一加熱爐中或於該微柵周圍設置一加熱棒，利用該加熱爐對該材料樣品進行加熱。可以理解，於給該材料樣品加熱之過程中，該微柵也同時被加熱。 Transmission electron microscopy is an important tool for characterizing the structure of a material sample. A high-resolution TEM image of the material sample can be observed by transmission electron microscopy. In the transmission electron microscope, the material sample is typically placed on a 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 material sample is heated by the heating furnace. It will be appreciated that the microgrid is also heated during the heating of the material sample.
在先前技術中，應用於透射電子顯微鏡之微柵通常係於銅網或鎳網等金屬網格上覆蓋一層多孔有機膜，再在該有機膜上蒸鍍一層非晶碳膜製成的。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 及碳膜之熱容與熱膨脹係數不一樣，該柵網於受熱時，該碳膜、有機膜與金屬網格之形變會不一致，從而造成放置於該微柵表面之材料樣品產生漂移。即該材料樣品於受熱過程中，會相對該透射電子顯微鏡產生移動。如鎳之膨脹係數遠大於非晶碳膜，其於受熱時之形變大於碳膜，從而導致放置其上之非晶碳膜移動，從而使吸附或放置於碳膜表面之材料樣品移動。然而，由於該透射電子顯微鏡對材料樣品之移動非常敏感，該材料樣品於受熱時產生之漂移，將使該透射電子顯微鏡難以得到高清晰之透射電鏡圖像。 In the prior art, a microgrid applied to a transmission electron microscope is usually formed by coating a porous organic film on a metal mesh such as a copper mesh or a nickel mesh, and then depositing an amorphous carbon film on the organic film. However, the thermal stability of previous transmission electron microscopes is not good enough due to the metal grid, organic film The heat capacity of the carbon film and the coefficient of thermal expansion are different. When the grid is heated, the deformation of the carbon film, the organic film and the metal mesh may be inconsistent, thereby causing drift of the material sample placed on the surface of the micro-gate. That is, the material sample moves relative to the transmission electron microscope during heating. If the expansion coefficient of nickel is much larger than that of the amorphous carbon film, it deforms when heated to be larger than that of the carbon film, thereby causing the amorphous carbon film placed thereon to move, thereby moving the material sample 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 drift of the material sample upon heating causes the transmission electron microscope to have a high-definition TEM image.
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。 In view of this, it is necessary to provide a TEM microgrid with better thermal stability.
一種透射電鏡微柵，其包括一網格、一奈米碳管膜狀結構及至少兩個電極。該奈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均勻分佈之奈米碳管，該複數奈米碳管形成複數微孔。 A transmission electron microstrip microgrid comprising a grid, a carbon nanotube film structure and at least two electrodes. The carbon nanotube film structure is disposed on the surface of the mesh. The at least two electrodes are spaced apart and electrically connected to the carbon nanotube film structure, respectively. The carbon nanotube film structure comprises a plurality of uniformly distributed carbon nanotubes, and the plurality of carbon nanotubes form a plurality of micropores.
一種透射電鏡微柵，其包括一網格、一奈米碳管膜狀結構及兩個電極。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碳管基本垂直地交叉設置，該複數奈米碳管形成複數微孔。 A transmission electron microstrip microgrid comprising a grid, a carbon nanotube film 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 carbon nanotubes arranged substantially vertically, and the plurality of carbon nanotubes form a plurality of micropores.
相較於先前技術，該透射電鏡微柵利用一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柵，即無需加熱網格，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熱膨脹係數。故，在加熱材料樣品時，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，能夠避免放置於該奈米碳管膜狀結構表面之材料樣品產生漂移。 Compared to the prior art, 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 The carbon nanotube film structure has a high electrothermal conversion rate and directly heats the material sample without heating the entire TEM microgrid, that is, there is no need to heat the grid, so less heat is generated during the heating process; The tubular membrane structure has a small coefficient of thermal expansion. Therefore, when the material sample is heated, since the carbon nanotube film-like structure generates less heat and has a small coefficient of thermal expansion, the deformation due to heat is small, so that the nano carbon can be prevented from being placed on the nano carbon. The material sample on the surface of the tubular membrane structure drifts.
以下將結合附圖對本發明作進一步之詳細說明。 The invention will be further described in detail below with reference to the accompanying drawings.
請參閱圖1及圖2，本發明實施例提供一種透射電鏡微柵100，其包括一網格110、一奈米碳管膜狀結構130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。 Referring to FIG. 1 and FIG. 2 , an embodiment of the present invention provides a TEM micro-gate 100 including a grid 110 , a carbon nanotube film structure 130 , 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.
該網格110具有至少一通孔111使該奈米碳管膜狀結構130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 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110之熱膨脹係數絕對值小於3，從而使該網格110於受熱時不容易產生變形。在本實施例中，該網格110為由陶瓷製成之柵網結構。 The mesh 110 has at least one through hole 111 for partially floating the carbon nanotube film structure 130, and the through hole 111 has a hole diameter of between 1 micrometer and 3 millimeters. The shape of the mesh 110 is not limited, and may be circular, square, elliptical or 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 mesh 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 mesh 110. The layer also allows the entire grid 110 to be made of an insulating heat resistant material. The insulating heat resistant material may be an insulating inorganic non-metal 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 110 has an absolute value of thermal expansion coefficient of less than 3, so that the grid 110 is less susceptible to deformation when heated. In the present embodiment, the grid 110 is a grid structure made of ceramic.
該兩個電極120設置於該奈米碳管膜狀結構130相對之兩端並與該奈米碳管膜狀結構130電連接。該兩個電極120可設置於網格110與奈米碳管膜狀結構130之間，也可設置於該奈米碳管膜狀結構130遠離該網格110之一側或將該兩個電極120設置於該網格110與該奈米碳管膜狀結構130相背之一側。當該兩個電極120設置於網格110與奈米碳管膜狀結構130之間時，該兩個電極120可通過於該網格110表面絲網印刷導電銀漿層而形成。優選地，該通過絲網印刷而形成之電極120，其厚度為2奈米~50奈米。在本實施例中，該兩個電極120設置於網格110與奈米碳管膜狀結構130之間，且該電極120設置於該網格110靠近外緣之位置。優選地，該兩個電極120嵌接於該網格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110面向該奈米碳管膜狀結構130應具有與該兩個電極120相對應之凹槽。該兩個電極120嵌入該凹槽內，並保證該兩個電極120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，從而使該奈米碳管膜狀結構130平 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120彼此併聯。 The two electrodes 120 are disposed at opposite ends of the carbon nanotube film structure 130 and are electrically connected to the carbon nanotube film structure 130. The two electrodes 120 may be disposed between the mesh 110 and the carbon nanotube film structure 130, or may be disposed on the side of the carbon nanotube film structure 130 away from the mesh 110 or the two electrodes. 120 is disposed on one side of the grid 110 opposite to the carbon nanotube film structure 130. When the two electrodes 120 are disposed between the grid 110 and the carbon nanotube film structure 130, the two electrodes 120 may be formed by screen printing a conductive silver paste layer on the surface of the mesh 110. Preferably, the electrode 120 formed by screen printing has a thickness of 2 nm to 50 nm. In this embodiment, the two electrodes 120 are disposed between the grid 110 and the carbon nanotube film structure 130, and the electrode 120 is disposed at a position near the outer edge of the grid 110. Preferably, the two electrodes 120 are in the grid 110 and are electrically connected to opposite ends of the carbon nanotube film 130. It can be understood that, at this time, the grid 110 faces the carbon nanotube. The film structure 130 should have grooves corresponding to the two electrodes 120. The two electrodes 120 are embedded in the recess, and the surfaces of the two electrodes 120 facing the carbon nanotube film 130 are flush with the surface of the grid 110 facing the carbon nanotube film 130. Thereby making the carbon nanotube film structure 130 flat The ground is laid on the surface of the grid 110. The shape of the two electrodes 120 is not limited. Preferably, the two electrodes 120 are arc-shaped electrodes disposed at positions near 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 sequentially arranged on the outer edge of the grid 110. At this time, the adjacent two pairs of electrodes 120 are connected in parallel with each other.
該奈米碳管膜狀結構130鋪設於該網格110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130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1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130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。 The carbon nanotube film structure 130 is laid on the surface of the mesh 110, covers the through hole 111 of the mesh 110, and is partially suspended by the through hole 111. Specifically, the carbon nanotube film structure 130 is suspended at 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 1 nm and 1 μm. It can be understood that each micropores are formed by adjacent carbon nanotubes, so the micropores are polygonal or irregular in shape. Preferably, the carbon nanotube film structure 130 has a thickness of less than 100 nanometers. The so-called "self-supporting" means that the carbon nanotube film structure 130 can maintain its own specific shape without being disposed on a surface of a substrate.
具體地，該奈米碳管膜狀結構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、奈米碳管碾壓膜或奈米碳管拉膜。 Specifically, the carbon nanotube film 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 film.
請參閱圖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碳管絮化膜。該奈米碳管絮化膜各向同性。該奈米碳管 絮化膜可通過對一奈米碳管陣列絮化處理而獲得。 Referring to FIG. 3, the carbon nanotube flocculation membrane comprises a plurality of carbon nanotubes which are 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 carbon nanotube flocculation film. The carbon nanotube film is isotropic. The carbon nanotube The flocculated membrane can be obtained by flocculation of a carbon nanotube array.
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。 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 along 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.
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130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120向另一個電極120延伸。 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 directly pulling 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 carbon nanotubes in the carbon nanotube film are The axial direction extends substantially along one electrode 120 toward the other electrode 120.
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 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10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度α，且該α大於0度且小於等於90度。當相鄰之奈米碳管拉膜中之奈米碳管之間具有一交叉角度α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130之機械性能增加，同時使該奈米碳管膜狀結構130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膜之層數有關，層數越多，微孔之孔徑越小。該奈米碳管膜還可進一步進行有機溶劑處理，使該奈米碳管膜收縮，增加該奈米碳管膜之強度。在本實施例中，該奈米碳管膜狀結構130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叉角度α大致等於90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。 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 The carbon nanotube film structure comprises a layer of carbon nanotube film having a layer of less than or equal to 10 layers. The carbon nanotubes in the adjacent carbon nanotube film in the carbon nanotube film structure have an intersection angle α between the carbon nanotubes, and the α is greater than 0 degrees and less than or equal to 90 degrees. When the carbon nanotubes in the adjacent carbon nanotube film have an intersection angle α, the carbon nanotubes are interwoven to form a network structure, so that the carbon nanotube film structure 130 is mechanical. The performance is increased, and the carbon nanotube film structure 130 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 nanotube film, and the more the number of layers, the micropores The smaller the aperture. The carbon nanotube film can be further subjected to an organic solvent treatment to shrink the carbon nanotube film and increase the strength of the carbon nanotube film. In this embodiment, the carbon nanotube film structure 130 includes at least two layers of carbon nanotube film laminated, and the intersection angle α between the carbon nanotubes in the adjacent carbon nanotube film is substantially equal to At 90 degrees, a network structure is formed, that is, the carbon nanotubes in the adjacent carbon nanotube film are substantially perpendicular to each other.
請參閱圖6至圖8，本發明實施例透射電鏡微柵100中之奈米碳管膜狀結構130為四層奈米碳管拉膜以90度角交叉層疊形成之網狀結構。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。 Referring to FIG. 6 to FIG. 8 , the carbon nanotube film structure 130 in the TEM micro-gate 100 of the embodiment of the present invention is a network structure in which four layers of carbon nanotube film are laminated at a 90 degree angle. 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.
本實施例透射電鏡微柵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 尺寸大於該奈米碳管膜狀結構130之微孔時，該奈米碳管膜狀結構130中之微孔可支持該材料樣品，而當該材料樣品之尺寸小於該奈米碳管膜狀結構130之微孔時，尤其係粒徑小於5nm之奈米顆粒時，該材料樣品主要係靠奈米碳管之吸附作用被穩定地吸附於奈米碳管管壁表面，從而使其承放於該奈米碳管膜狀結構130表面。請參閱圖9，圖中黑色顆粒為待觀察之奈米金顆粒。該奈米金顆粒穩定地吸附於奈米碳管管壁邊沿，有利於觀察奈米金顆粒之高分辨像。 In the embodiment, the TEM microgrid 100 is applied, and a material sample to be observed is placed on the surface of the carbon nanotube film structure 130, when the material sample is When the size is larger than the micropores of the carbon nanotube film structure 130, the micropores in the carbon nanotube film structure 130 can support the material sample, and when the material sample size is smaller than the carbon nanotube film shape When the pores of the structure 130 are especially nano particles having a particle diameter of less than 5 nm, the material sample is stably adsorbed on the surface of the carbon nanotube tube wall by the adsorption of the carbon nanotubes, thereby allowing the substrate to be placed. On the surface of the carbon nanotube film structure 130. Referring to Figure 9, the black particles are the nano gold particles to be observed. The nano gold particles are stably adsorbed on the edge of the carbon nanotube tube wall, which is favorable for observing the high resolution image of the nano gold particles.
當需要觀察該材料樣品於受熱時之結構時，通過該兩個電極120接入一電源，使一電流通過該兩個電極120傳導至該奈米碳管膜狀結構130，該奈米碳管膜狀結構130在通電時發熱。作為加熱單元之奈米碳管膜狀結構130具有極小之單位面積熱容，較高之電熱轉換率及較快之溫度回應，且該奈米碳管膜狀結構130與材料樣品直接接觸，由奈米碳管膜狀結構130發出之熱量能夠直接、快速傳遞給該材料樣品，能源利用率高。同時，該奈米碳管膜狀結構130形成之網狀結構具有較好之機械穩定性，該奈米碳管膜狀結構130具有極小之熱膨脹係數絕對值，具體地，該奈米碳管膜狀結構130之熱膨脹係數絕對值範圍為0.01~0.5。故，該材料樣品在受熱時，奈米碳管膜狀結構130不容易產生形變。 When it is necessary to observe the structure of the material sample when heated, a power source is connected through the two electrodes 120, and a current is conducted through the two electrodes 120 to the carbon nanotube film structure 130, the carbon nanotube The film structure 130 generates heat when energized. The carbon nanotube film structure 130 as a heating unit has a very small heat capacity per unit area, a high electrothermal conversion rate and a relatively fast temperature response, and the carbon nanotube film structure 130 is in direct contact with the material sample, The heat generated by the carbon nanotube film structure 130 can be directly and quickly transferred to the material sample, and the energy utilization rate is high. Meanwhile, the mesh structure formed by the carbon nanotube film structure 130 has good mechanical stability, and the carbon nanotube film structure 130 has an extremely small absolute value of thermal expansion coefficient, specifically, the carbon nanotube film The absolute expansion coefficient of the thermal expansion coefficient of the structure 130 ranges from 0.01 to 0.5. Therefore, when the material sample is heated, the carbon nanotube film structure 130 is not easily deformed.
該透射電鏡微柵利用一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 整個透射電鏡微柵，即不需要加熱網格，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熱膨脹係數。故，於加熱材料樣品時，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，能夠避免放置於該奈米碳管膜狀結構表面之材料樣品產生漂移。進一步地，由於該網格也選用膨脹係數較小之陶瓷製成，且於加熱材料樣品時，並不需要加熱該網格，該網格僅於靠近該奈米碳管膜狀結構之部分吸收熱量，即吸收之熱量非常少，從而使該網格其因受熱而形變也比較少。故，可減小該奈米碳管膜狀結構與網格之間因為形變而產生之相對移動，進一步避免放置於該奈米碳管膜狀結構表面之材料樣品產生漂移。 The TEM microgrid utilizes a carbon nanotube film structure to carry and heat a sample of the material to be observed placed on the surface thereof. The carbon nanotube film structure has a high electrothermal conversion rate and directly heats the material sample without heating The entire TEM microgrid, that is, does not need to heat the grid, so the heat generated during the heating process is less; and the carbon nanotube film structure has a smaller thermal expansion coefficient. Therefore, when the material sample is heated, since the carbon nanotube film-like structure generates less heat and has a small coefficient of thermal expansion, the deformation due to heat is small, so that the nano carbon can be prevented from being placed on the nano carbon. The material sample on the surface of the tubular membrane structure drifts. Further, since the grid is also made of ceramic having a small expansion coefficient, and when heating the material sample, it is not necessary to heat the grid, and the grid is only absorbed near the film structure of the carbon nanotube. The heat, that is, the amount of heat absorbed, is so small that the mesh is less deformed by heat. Therefore, the relative movement between the film structure of the carbon nanotube and the mesh due to the deformation can be reduced, and the material sample placed on the surface of the film structure of the carbon nanotube can be further prevented from drifting.
綜上所述，本發明確已符合發明專利之要件，遂依法提出專利申請。惟，以上所述者僅為本發明之較佳實施例，自不能以此限制本案之申請專利範圍。舉凡習知本案技藝之人士援依本發明之精神所作之等效修飾或變化，皆應涵蓋於以下申請專利範圍內。 In summary, the present invention has indeed met the requirements of the invention patent, and has filed a patent application 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.
100‧‧‧透射電鏡微柵 100‧‧‧ Transmission electron microscopy
110‧‧‧網格 110‧‧‧Grid
111‧‧‧通孔 111‧‧‧through hole
120‧‧‧電極 120‧‧‧electrode
130‧‧‧奈米碳管膜狀結構 130‧‧‧Nano carbon tube membrane structure
圖1為本發明實施例透射電鏡微柵之結構示意圖。 FIG. 1 is a schematic structural view of a transmission electron microscope micro-gate according to an embodiment of the present invention.
圖2為圖1中透射電鏡微柵沿Ⅱ-Ⅱ線之剖視圖。 2 is a cross-sectional view of the TEM microgate of FIG. 1 taken along line II-II.
圖3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。 3 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.
圖4為圖1中透射電鏡微柵中用作奈米碳管膜狀結構之奈 米碳管碾壓膜之掃描電鏡照片。 Figure 4 is a view of the nanostructure of the carbon nanotube film used in the transmission electron microstrip of Figure 1. Scanning electron micrograph of a carbon nanotube rolled film.
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。 Fig. 5 is a scanning electron micrograph of a carbon nanotube film used as a film structure of a carbon nanotube in the transmission electron microstrip of Fig. 1.
圖6為本發明實施例透射電鏡微柵之掃描電鏡照片。 6 is a scanning electron micrograph of a transmission electron microstrip micro-gate according to an embodiment of the present invention.
圖7為圖6中之透射電鏡微柵中之奈米碳管膜狀結構之透射電鏡照片。 Fig. 7 is a transmission electron micrograph of a film structure of a carbon nanotube in the transmission electron microstrip of Fig. 6.
圖8為承載樣品之奈米碳管膜局部放大示意圖。 Figure 8 is a partially enlarged schematic view of a carbon nanotube film carrying a sample.
圖9為應用本發明實施例透射電鏡微柵觀察奈米金顆粒之高分辨透射電鏡照片。 Fig. 9 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.
100‧‧‧透射電鏡微柵 100‧‧‧ Transmission electron microscopy
110‧‧‧網格 110‧‧‧Grid
111‧‧‧通孔 111‧‧‧through hole
120‧‧‧電極 120‧‧‧electrode
130‧‧‧奈米碳管膜狀結構 130‧‧‧Nano carbon tube membrane structure
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| US4163900A (en) * | 1977-08-17 | 1979-08-07 | Connecticut Research Institute, Inc. | Composite electron microscope grid suitable for energy dispersive X-ray analysis, process for producing the same and other micro-components |
| US4250127A (en) * | 1977-08-17 | 1981-02-10 | Connecticut Research Institute, Inc. | Production of electron microscope grids and other micro-components |
| CN1206697C (en) * | 2003-02-26 | 2005-06-15 | 李巧玲 | Micro grating for transmissive electron microscope and its making process |
| US20060169975A1 (en) * | 2005-01-24 | 2006-08-03 | The Regents Of The University Of California | Lipid bilayers on nano-templates |
| TW200830348A (en) * | 2007-01-11 | 2008-07-16 | Promos Technologies Inc | Carrier and method for preparing specimen of transmission electron microscope |
| TW200842105A (en) * | 2007-04-20 | 2008-11-01 | Hon Hai Prec Ind Co Ltd | Transmission electron microscope grid and method for making same |
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| US4163900A (en) * | 1977-08-17 | 1979-08-07 | Connecticut Research Institute, Inc. | Composite electron microscope grid suitable for energy dispersive X-ray analysis, process for producing the same and other micro-components |
| US4250127A (en) * | 1977-08-17 | 1981-02-10 | Connecticut Research Institute, Inc. | Production of electron microscope grids and other micro-components |
| CN1206697C (en) * | 2003-02-26 | 2005-06-15 | 李巧玲 | Micro grating for transmissive electron microscope and its making process |
| US20060169975A1 (en) * | 2005-01-24 | 2006-08-03 | The Regents Of The University Of California | Lipid bilayers on nano-templates |
| TW200830348A (en) * | 2007-01-11 | 2008-07-16 | Promos Technologies Inc | Carrier and method for preparing specimen of transmission electron microscope |
| TW200842105A (en) * | 2007-04-20 | 2008-11-01 | Hon Hai Prec Ind Co Ltd | Transmission electron microscope grid and method for making same |
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