JP2005249414A - Cross-sectional observation method for carbon nanotube - Google Patents
Cross-sectional observation method for carbon nanotube Download PDFInfo
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本発明は、カーボンナノチューブの断面観察方法に関し、特にカーボンナノチューブの断面を観察可能な部位の頻度を向上させることのできるカーボンナノチューブの断面観察方法に関する。 The present invention relates to a method for observing a cross section of a carbon nanotube, and more particularly, to a method for observing a cross section of a carbon nanotube that can improve the frequency of a portion where the cross section of the carbon nanotube can be observed.
近年、ガス吸蔵材としてのカーボンナノチューブ（以下、「カーボンナノチューブ」をＣＮＴと称することがある。）の特性が注目を集めてきている。ＣＮＴを高性能ガス吸蔵材として用いる場合、ＣＮＴのチューブ径やＣＮＴのバンドル構造を最適化する必要がある。 In recent years, the characteristics of carbon nanotubes (hereinafter, “carbon nanotubes” are sometimes referred to as CNTs) as gas storage materials have attracted attention. When CNT is used as a high-performance gas storage material, it is necessary to optimize the CNT tube diameter and the CNT bundle structure.
透過電子顕微鏡（以下、「透過電子顕微鏡」をＴＥＭと称することがある。）は、ＣＮＴのナノ構造を評価するのに欠くことのできない方法である。ＴＥＭにより透過電子像を得るためには、試料厚さを薄くしなければならない。このため、ＣＮＴをＴＥＭ観察する際には、通常アルコール中にＣＮＴを超音波分散して希薄化し、これをＣＮＴ用メッシュに滴下、乾燥させて薄膜化した試料をＴＥＭ観測用試料に供する。 The transmission electron microscope (hereinafter, “transmission electron microscope” may be referred to as TEM) is an indispensable method for evaluating the nanostructure of CNT. In order to obtain a transmission electron image by TEM, the sample thickness must be reduced. For this reason, when CNTs are observed with a TEM, a sample obtained by ultrasonically dispersing CNTs in alcohol and diluting them, dropping them onto a CNT mesh and drying them to form a thin film is used as a TEM observation sample.
しかし、このようにして調製した試料では、ＣＮＴを乾燥させる際に、アルコール中ではランダム配向していたＣＮＴが、アルコールが引けるにつれてＴＥＭ用メッシュ面に配向するように寝てしまうため、ＣＮＴの断面を観察することが困難であった。 However, in the sample prepared in this way, when the CNTs are dried, the CNTs that are randomly oriented in the alcohol sleep so that they are oriented on the TEM mesh surface as the alcohol is drawn. It was difficult to observe.
この問題を解決するため、ＣＮＴ微小塊をＴＥＭ用メッシュ上に載せ、その上からメタノールを滴下することにより観測用試料を調製し、透過電子像を得る方法が報告されている（例えば、非特許文献１又は２参照。）。
ＴＥＭ観察用試料調製のため、ＣＮＴ微小塊をＴＥＭ用メッシュ上に載せる作業は、通常ピンセットなどを用いて行われる。しかし、ＣＮＴ微小塊がピンセットに付着してしまい、ＣＮＴ微小塊をＴＥＭ用メッシュ上に載せることが困難であった。 In order to prepare a sample for TEM observation, the operation of placing the CNT micro-lumps on the TEM mesh is usually performed using tweezers or the like. However, the CNT minute lump adheres to the tweezers, and it is difficult to place the CNT minute lump on the TEM mesh.
そこで上記問題に鑑み、本発明は、ＣＮＴ微小塊をＴＥＭ用メッシュ上に容易に載せることができ、ＣＮＴのチューブ径の測定やＣＮＴのバンドル構造の観察等の、ＣＮＴの断面観察を容易に行うことを可能とするカーボンナノチューブの断面観察方法の提供を目的とする。 Therefore, in view of the above problems, the present invention can easily place a CNT micro-lumps on a TEM mesh, and easily perform cross-sectional observation of the CNT, such as measurement of the CNT tube diameter and observation of the CNT bundle structure. An object of the present invention is to provide a method for observing a cross section of a carbon nanotube that makes it possible.
即ち、本発明は、
＜１＞ 少なくとも、透過電子顕微鏡用メッシュを湿潤用有機溶剤で湿らせる湿潤工程と、前記湿潤用有機溶剤で湿らせた前記透過電子顕微鏡用メッシュにカーボンナノチューブ微小塊を載せる配置工程と、前記カーボンナノチューブ微小塊に滴下用有機溶剤を滴下する溶剤滴下工程と、前記滴下用有機溶剤を乾燥して前記カーボンナノチューブ微小塊を前記透過電子顕微鏡用メッシュに固定する固定化工程と、前記透過電子顕微鏡用メッシュに固定された前記カーボンナノチューブ微小塊の断面を透過電子顕微鏡で観察する観察工程と、を有するカーボンナノチューブの断面観察方法である。
That is, the present invention
<1> At least a wetting step of moistening a transmission electron microscope mesh with a moistening organic solvent, an arrangement step of placing a carbon nanotube fine mass on the transmission electron microscope mesh moistened with the moistening organic solvent, and the carbon A solvent dropping step of dropping a dropping organic solvent on the nanotube micro-lumps, an immobilization step of drying the dropping organic solvent and fixing the carbon nanotube micro-lumps to the transmission electron microscope mesh, and the transmission electron microscope An observation step of observing a cross section of the carbon nanotube fine mass fixed to the mesh with a transmission electron microscope.
本発明によれば、ＣＮＴ微小塊をＴＥＭ用メッシュ上に容易に載せることができるため、ＣＮＴの断面観察を容易に行うことができる。 According to the present invention, since the CNT minute lump can be easily placed on the TEM mesh, it is possible to easily observe the cross section of the CNT.
本発明のＣＮＴの断面観察方法は、少なくとも、ＴＥＭ用メッシュを湿潤用有機溶剤で湿らせる湿潤工程と、前記湿潤用有機溶剤で湿らせた前記ＴＥＭ用メッシュにＣＮＴ微小塊を載せる配置工程と、前記ＣＮＴ微小塊に滴下用有機溶剤を滴下する溶剤滴下工程と、前記滴下用有機溶剤を乾燥して前記ＣＮＴ微小塊を前記ＴＥＭ用メッシュに固定する固定化工程と、前記ＴＥＭ用メッシュに固定された前記ＣＮＴ微小塊の断面を透過電子顕微鏡で観察する観察工程とを有する。
以下、各工程について詳細に説明する。
The method for observing a cross section of a CNT of the present invention includes at least a wetting step in which a TEM mesh is moistened with a wetting organic solvent, and an arrangement step in which CNT micro-lumps are placed on the TEM mesh moistened with the wetting organic solvent, Fixed to the TEM mesh, a solvent dropping step of dropping the organic solvent for dropping on the CNT fine mass, an immobilizing step of drying the organic solvent for dropping and fixing the CNT fine mass to the TEM mesh, and the TEM mesh And an observing step of observing a cross section of the CNT minute block with a transmission electron microscope.
Hereinafter, each step will be described in detail.
−湿潤工程−
前記湿潤工程で用いられる湿潤用有機溶剤は特に限定されないが、前記湿潤用有機溶剤としては、前記ＴＥＭ用メッシュに馴染むある程度の濡れ性を有し、適度に速やかに蒸発する（２０℃での蒸気圧が２０〜２００ｍｍＨｇが好ましい。）ことが好ましく、その具体例として、例えば、アルコール類、ケトン類、エーテル類及び有機塩素系溶剤等が挙げられる。これらの中でも、マイクログリッドメッシュなどに用いられているコロジョン膜に与えるダメージが少ないことからエチルアルコール、メチルアルコール、トルエン、テトラクロロエチレンが好ましい。
-Wetting process-
The wetting organic solvent used in the wetting step is not particularly limited, but the wetting organic solvent has a certain degree of wettability that is compatible with the TEM mesh and evaporates moderately and quickly (vapor at 20 ° C. The pressure is preferably 20 to 200 mmHg.), And specific examples thereof include alcohols, ketones, ethers and organic chlorine solvents. Among these, ethyl alcohol, methyl alcohol, toluene, and tetrachloroethylene are preferable because they give less damage to the colloid film used in the microgrid mesh.
湿潤用有機溶剤を用いてＴＥＭ用メッシュを湿らせる方法は特に限定されるものではないが、ＴＥＭ用メッシュをろ紙上に置いた状態で湿潤用有機溶剤をＴＥＭ用メッシュに滴下することにより、ＴＥＭ用メッシュ表面を濡らすのに必要な量以外の余分な湿潤用有機溶剤を吸収除去し、作業性を向上させることができるため好ましい。 The method of moistening the TEM mesh using the wetting organic solvent is not particularly limited, but by dropping the wetting organic solvent onto the TEM mesh with the TEM mesh placed on the filter paper, This is preferable because excess wet organic solvent other than the amount necessary for wetting the mesh surface can be absorbed and workability can be improved.
ＴＥＭ用メッシュをろ紙上に置いた状態で湿潤用有機溶剤を滴下する際の、湿潤用有機溶剤の滴下量は、１ｍｇ以上１０ｍｇ以下が好ましく、１ｍｇ以上２ｍｇ以下がさらに好ましく、１ｍｇ程度が特に好ましい。、湿潤用有機溶剤の滴下量が１ｍｇ以上１０ｍｇ以下であると、湿潤用有機溶剤の滴下後ＴＥＭ用メッシュに試料を載せるまでの０．５〜１．５分の間、ＴＥＭ用メッシュ表面を適度な湿潤状態に保つことができるため好ましい。 When the organic solvent for wetting is dropped with the TEM mesh placed on the filter paper, the amount of the organic solvent for wetting added is preferably 1 mg to 10 mg, more preferably 1 mg to 2 mg, and particularly preferably about 1 mg. . When the amount of the organic solvent for wetting is 1 mg or more and 10 mg or less, the surface of the TEM mesh is moderated for 0.5 to 1.5 minutes after the organic solvent for wetting is dropped until the sample is placed on the TEM mesh. It is preferable because it can be kept in a wet state.
本発明に用いることのできるＴＥＭ用メッシュの種類としては、例えば、グリッドメッシュ、マイクログリッドメッシュ、プラスチック支持膜メッシュ等が挙げられる。 Examples of the type of TEM mesh that can be used in the present invention include a grid mesh, a microgrid mesh, and a plastic support membrane mesh.
−配置工程−
配置工程で用いられるＣＮＴ微小塊は、通常のＴＥＭの測定に用いられる程度の大きさの、目視でかろうじて確認できる程度の微小なＣＮＴの塊である。ＣＮＴの塊が大きいと、測定試料をＴＥＭに装填したときに試料が落下する可能性がある。ＣＮＴ微小塊は、ＣＮＴをピンセットなどを用いてよくほぐすことにより調製される。
-Placement process-
The CNT minute lump used in the arranging step is a minute CNT lump of a size that can be barely confirmed visually with a size that can be used for a normal TEM measurement. If the mass of CNT is large, the sample may fall when the measurement sample is loaded on the TEM. The CNT micro-lumps are prepared by loosening CNTs using tweezers or the like.
前記湿潤工程により湿らせたＴＥＭ用メッシュが乾ききらないうちに、ＣＮＴ微小塊をピンセットでつまみ、これを湿らせたＴＥＭ用メッシュに接触させて素早くピンセットをＴＥＭ用メッシュからはなすことにより、ＴＥＭ用メッシュにＣＮＴ微小塊を載せることができる。このとき、ＴＥＭ用メッシュ面に残っている湿潤用有機溶剤がＣＮＴ微小塊に触れ、湿潤用有機溶剤の表面張力によって接着力が生じＣＮＴ微小塊がピンセットから離れるのを容易にする。 Before the TEM mesh moistened by the wetting process is completely dried, the CNT micro-lumps are picked up with tweezers and brought into contact with the moistened TEM mesh to quickly remove the tweezers from the TEM mesh. A CNT minute lump can be placed on the mesh. At this time, the wetting organic solvent remaining on the TEM mesh surface touches the CNT minute mass, and an adhesive force is generated by the surface tension of the wetting organic solvent to facilitate the separation of the CNT minute mass from the tweezers.
ＴＥＭ用メッシュが完全に乾燥していると、ＣＮＴ微小塊はピンセットから離れ難く、また、ＴＥＭ用メッシュが濡れすぎていると湿潤用有機溶剤がＣＮＴ微小塊全体に浸透してピンセットとＣＮＴ微小塊との接触点にまで到達してしまい、この場合もＣＮＴ微小塊がピンセットから離れ難くなることがある。 When the TEM mesh is completely dry, the CNT micro-lumps are difficult to separate from the tweezers. When the TEM mesh is too wet, the wetting organic solvent penetrates the entire CNT micro-lumps and the tweezers and the CNT micro-lumps. The CNT micro-lumps may be difficult to separate from the tweezers.
そのため、前記湿潤工程によりＴＥＭ用メッシュを湿らせてから、ＣＮＴ微小塊をＴＥＭ用メッシュに載せるまでの時間（乾燥時間）は、ＴＥＭ用メッシュに滴下される湿潤用有機溶剤の種類及び量にもよるが、好ましくは０．５〜５分以内、さらに好ましくは０．５〜２分以内、特に好ましくは１〜１．５分以内である。０．５〜５分以内であれば、ＣＮＴ微小塊をＴＥＭ用メッシュに容易に載せることができる。 Therefore, the time (drying time) from the time when the TEM mesh is moistened by the wetting process until the CNT fine mass is placed on the TEM mesh depends on the kind and amount of the wetting organic solvent dripped onto the TEM mesh. However, it is preferably within 0.5 to 5 minutes, more preferably within 0.5 to 2 minutes, and particularly preferably within 1 to 1.5 minutes. If it is within 0.5 to 5 minutes, the CNT minute lump can be easily placed on the TEM mesh.
−溶剤滴下工程−
前記配置工程においてＴＥＭ用メッシュに載せられたＣＮＴ微小塊に、滴下用有機溶剤を滴下する。滴下用有機溶剤としては、炭素材料（ＣＮＴ）に馴染むある程度の親油性を有し、適度に速やかに蒸発し（２０℃での蒸気圧が２０〜２００ｍｍＨｇが好ましい。）滴下用有機溶剤が蒸発する過程で液相が引けるときにＣＮＴを分散する作用を及ぼすだけの凝集力のある（２０℃での表面張力が１０〜３０ｄｙｎｅ／ｃｍが好ましい。）ことが好ましく、具体的には、アルコール類、ケトン類、エーテル類及び有機塩素系溶剤等が挙げられる。これらの中でも、マイクログリッドメッシュなどに用いられているコロジョン膜に与えるダメージが少ないことからメチルアルコール、エチルアルコール、トルエン又はテトラクロロエチレンが好ましい。
-Solvent dripping process-
In the arrangement step, the dropping organic solvent is dropped on the CNT minute lump placed on the TEM mesh. The organic solvent for dropping has a certain degree of lipophilicity that is compatible with the carbon material (CNT), and evaporates moderately and quickly (the vapor pressure at 20 ° C. is preferably 20 to 200 mmHg), and the organic solvent for dropping evaporates. It is preferable to have a cohesive force sufficient to disperse CNTs when the liquid phase is drawn in the process (surface tension at 20 ° C. is preferably 10 to 30 dyne / cm), specifically, alcohols, Examples include ketones, ethers, and organic chlorine solvents. Among these, methyl alcohol, ethyl alcohol, toluene, or tetrachloroethylene is preferable because damage to the colloid film used for a microgrid mesh or the like is small.
滴下用有機溶剤の滴下量としては、１ｍｇ以上１０ｍｇ以下が好ましく、１ｍｇ以上２ｍｇ以下がさらに好ましく、１ｍｇ程度が特に好ましい。 The amount of the organic solvent for dripping is preferably 1 mg or more and 10 mg or less, more preferably 1 mg or more and 2 mg or less, and particularly preferably about 1 mg.
ＣＮＴ微小塊に滴下用有機溶剤を滴下する際、ＴＥＭ用メッシュをろ紙上に置いた状態で滴下することにより、ＣＮＴ微小塊の分散に必要な量以外の余分な滴下用有機溶剤を吸収除去し、分散性及び作業性を向上させることができるため好ましい。 When dropping the organic solvent for dripping onto the CNT micro-lumps, by dropping with the TEM mesh placed on the filter paper, the extra organic solvent for dripping other than the amount necessary for the dispersion of the CNT micro-lumps is absorbed and removed. , Because dispersibility and workability can be improved.
滴下された滴下用有機溶剤の大部分は、ＴＥＭ用メッシュを通過してろ紙に吸い取られ、残った滴下用有機溶剤は蒸発する。これらの過程で、ＣＮＴ微小塊は、ＣＮＴの断面観察を容易に行うことができる程度に分散される。 Most of the dropped organic solvent drops are absorbed by the filter paper through the TEM mesh, and the remaining dropping organic solvent evaporates. In these processes, the CNT micro-lumps are dispersed to such an extent that the cross-sectional observation of the CNT can be easily performed.
なお、前記湿潤用有機溶剤と前記滴下用有機溶剤とは、同じであっても異なっていてもよい。 The wetting organic solvent and the dropping organic solvent may be the same or different.
−固定化工程−
滴下用有機溶剤の滴下されたＣＮＴ微小塊を乾燥させることにより、ＴＥＭ用メッシュのメッシュ面に平行なＣＮＴは、ファンデルワールス力等の物理的な力でメッシュ面に接着され、ＣＮＴ微小塊は全体としてＴＥＭ用メッシュに固定される。ＴＥＭ用メッシュに固定されたＣＮＴ微小塊は、ＴＥＭ観察に供される。
-Immobilization process-
By drying the dropped CNT fine mass of the dropping organic solvent, the CNT parallel to the mesh surface of the TEM mesh is adhered to the mesh surface by a physical force such as van der Waals force. It is fixed to the TEM mesh as a whole. The CNT minute block fixed to the TEM mesh is used for TEM observation.
上述の工程においては、微小な試料を扱うため、それらが飛散しないように適当な風防を用いることが好ましい。 In the above-mentioned process, since a minute sample is handled, it is preferable to use an appropriate windshield so that they are not scattered.
−観察工程−
上述の工程を経て調製されたＣＮＴのＴＥＭ観察用試料を用いて、ＣＮＴの断面観察を行う。加速電圧２００〜３００ｋＶの高分解のＴＥＭを用い、ＴＥＭ用メッシュ上のＣＮＴ微小塊中に存在する断面結像部位を探し、多波格子像による鮮明なコントラストを得ることができる。
-Observation process-
CNT cross-sectional observation is performed using the CNT TEM observation sample prepared through the above-described steps. Using a high-resolution TEM having an acceleration voltage of 200 to 300 kV, a cross-sectional imaging site existing in a CNT micro-lumb on the TEM mesh can be searched for, and a clear contrast by a multiwave lattice image can be obtained.
例えば、２５万倍の観察倍率において、ＣＮＴ微小塊中の濃淡コントラストを見極め濃い部分で焦点調整を行うと、ＣＮＴが束になったバンドル断面を高い確率で発見することができる。次に、回折コントラストによって焦点調整を行い、ＣＮＴ断面の透過電子顕微鏡写真を得ることができる。 For example, at an observation magnification of 250,000 times, if the contrast of the CNT minute mass is determined and focus adjustment is performed at a dark portion, a bundle cross section in which CNTs are bundled can be found with high probability. Next, the focus is adjusted by the diffraction contrast, and a transmission electron micrograph of the CNT cross section can be obtained.
本発明のカーボンナノチューブの断面観察方法は、必要に応じてその他の工程を有していてもよい。 The carbon nanotube cross-sectional observation method of the present invention may have other steps as necessary.
以下、本発明を下記実施例に従いさらに詳細に説明するが、本発明は下記実施例により限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated further in detail according to the following Example, this invention is not limited by the following Example.
［実施例１］
工業用エチルアルコールを精密ピンセットですくい、ろ紙上に載せたＴＥＭ用メッシュに１滴（約１ｍｇ）滴下した。滴下後３０秒から１分の間に、乾燥させた精密ピンセットでＣＮＴ微小塊をつかみ、これを湿潤したＴＥＭ用メッシュに近づけ、ＣＮＴ微小塊を接触、移着させた。その後、精密ピンセットで工業用エチルアルコールを１〜２滴（１〜１０ｍｇ程度）滴下し、ＴＥＭ用メッシュ上でＣＮＴ微小塊を分散させた。その後、ＣＮＴ微小塊を乾燥してＴＥＭ用メッシュ上に固定することによりＴＥＭ観察用試料を調製した。
[Example 1]
Industrial ethyl alcohol was scooped with precision tweezers, and 1 drop (about 1 mg) was dropped onto a TEM mesh placed on a filter paper. Between 30 seconds and 1 minute after the dropping, the CNT minute mass was grasped with a dry precision tweezers, and this was brought close to a wet TEM mesh to contact and transfer the CNT minute mass. Thereafter, 1 to 2 drops (about 1 to 10 mg) of industrial ethyl alcohol was dropped with precision tweezers to disperse the CNT micro-lumps on the TEM mesh. Then, the sample for TEM observation was prepared by drying and fixing on a TEM mesh the CNT minute lump.
得られたＴＥＭ観察用試料を用い、Ｈ−９０００ＵＨＲ（日立製、加速電圧３００ｋＶ、倍率×２，０００，０００、フォーカス＆コントラスト：回折コントラスト（多波格子像コントラスト））によりＴＥＭ写真を撮影した。図１にその結果を示す。 Using the obtained TEM observation sample, a TEM photograph was taken with H-9000UHR (manufactured by Hitachi, acceleration voltage 300 kV, magnification x 2,000,000, focus & contrast: diffraction contrast (multiwave lattice image contrast)). The result is shown in FIG.
［比較例１］
ＴＥＭ用メッシュを湿潤させないで、ＴＥＭ用メッシュ上にＣＮＴ微小塊を載せようとしたが、ＣＮＴ微小塊を精密ピンセットからＴＥＭ用メッシュに移着させることが困難であった。ＣＮＴ微小塊として、ある程度大きなものを用いれば移着させることは容易であったが、その場合、一旦ＴＥＭ用メッシュ上に移着させたＣＮＴ微小塊が、ＴＥＭ装置内でＴＥＭ用メッシュ表面から剥離、落下して、ＴＥＭ写真を撮影できない場合があった。
[Comparative Example 1]
An attempt was made to place the CNT fine mass on the TEM mesh without wetting the TEM mesh, but it was difficult to transfer the CNT fine mass from the precision tweezers to the TEM mesh. It was easy to transfer CNT micro-lumps if they were used to some extent, but in that case, the CNT micro-lumps once transferred onto the TEM mesh were peeled off from the surface of the TEM mesh within the TEM device. In some cases, the TEM photograph could not be taken due to falling.
Claims (1)
前記湿潤用有機溶剤で湿らせた前記透過電子顕微鏡用メッシュにカーボンナノチューブ微小塊を載せる配置工程と、
前記カーボンナノチューブ微小塊に滴下用有機溶剤を滴下する溶剤滴下工程と、
前記滴下用有機溶剤を乾燥して前記カーボンナノチューブ微小塊を前記透過電子顕微鏡用メッシュに固定する固定化工程と、
前記透過電子顕微鏡用メッシュに固定された前記カーボンナノチューブ微小塊の断面を透過電子顕微鏡で観察する観察工程と、
を有するカーボンナノチューブの断面観察方法。 At least a wetting step of wetting the transmission electron microscope mesh with a wetting organic solvent;
An arrangement step of placing the carbon nanotube micro-lumps on the transmission electron microscope mesh moistened with the wet organic solvent;
A solvent dropping step of dropping an organic solvent for dropping into the carbon nanotube micro-lumps;
An immobilization step of drying the organic solvent for dripping and fixing the carbon nanotube fine mass to the mesh for transmission electron microscope;
An observation step of observing a cross-section of the carbon nanotube fine mass fixed to the mesh for the transmission electron microscope with a transmission electron microscope;
Sectional observation method of carbon nanotube having
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| US8294098B2 (en) | 2007-03-30 | 2012-10-23 | Tsinghua University | Transmission electron microscope micro-grid |
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