In-situ Fluid Experiments in Carbon Nanotubes

2000 ◽  
Vol 633 ◽  
Author(s):  
Yury Gogotsi ◽  
Joseph A. Libera ◽  
Almila GüvenÇ Yazicioglu ◽  
Constantine M. Megaridis

AbstractClosed-end multi-wall carbon nanotubes, which contain an encapsulated aqueous multi-phase fluidunder high pressure, have been produced by hydrothermal synthesis. These nanotubes are leak-tight by virtue of holding the fluid at the high vacuum of a transmission electron microscope (TEM) and can be used as a testplatform for unique in-situ nanofluidic experiments in TEM. They form an experimental apparatus, which is at least two orders of magnitude smaller than the smallest capillaries used in fluidic experiments so far. Excellent wettability of the carbon tube walls by the liquid and a dynamic behavior similar to that in micro-capillaries demonstrates the possibility of use of nanoscale (<100 nm) tubes in nanofluidic devices.However, complex interface behavior that can potentially create hurdles to fluid transport is also demonstratedherein.

2013 ◽  
Vol 67 (8) ◽  
Author(s):  
Elena Tomšík ◽  
Zuzana Morávková ◽  
Jaroslav Stejskal ◽  
Miroslava Trchová ◽  
Petr Šálek ◽  
...  

AbstractPolyaniline coating was deposited on the surface of multi-wall carbon nanotubes of Russian and Taiwanese origin in situ during the polymerization of aniline. The deposited polyaniline film was subsequently carbonized under an inert atmosphere at various temperatures to produce coaxial coating of the carbon nanotubes with nitrogen-containing carbon. The new materials were investigated by infrared and Raman spectroscopies, which demonstrated the conversion of the polyaniline coating to a carbonized structure. X-ray photoelectron spectroscopy proved that the carbonized overlayer contains nitrogen atoms in various covalent bonding states. Transmission electron microscopy confirmed the coaxial structure of the composites. The Brunauer-Emmett-Teller method was used to estimate the specific surface area, the highest being 272 m2 g−1. The conductivity of 0.9–16 S cm−1 was measured by the four-point method, and it was only a little affected by the carbonization of the polyaniline coating.


Author(s):  
Xianghong Tong ◽  
Oliver Pohland ◽  
J. Murray Gibson

The nucleation and initial stage of Pd2Si crystals on Si(111) surface is studied in situ using an Ultra-High Vacuum (UHV) Transmission Electron Microscope (TEM). A modified JEOL 200CX TEM is used for the study. The Si(111) sample is prepared by chemical thinning and is cleaned inside the UHV chamber with base pressure of 1x10−9 τ. A Pd film of 20 Å thick is deposited on to the Si(111) sample in situ using a built-in mini evaporator. This room temperature deposited Pd film is thermally annealed subsequently to form Pd2Si crystals. Surface sensitive dark field imaging is used for the study to reveal the effect of surface and interface steps.The initial growth of the Pd2Si has three stages: nucleation, growth of the nuclei and coalescence of the nuclei. Our experiments shows that the nucleation of the Pd2Si crystal occurs randomly and almost instantaneously on the terraces upon thermal annealing or electron irradiation.


Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.


Author(s):  
Michael T. Marshall ◽  
Xianghong Tong ◽  
J. Murray Gibson

We have modified a JEOL 2000EX Transmission Electron Microscope (TEM) to allow in-situ ultra-high vacuum (UHV) surface science experiments as well as transmission electron diffraction and imaging. Our goal is to support research in the areas of in-situ film growth, oxidation, and etching on semiconducter surfaces and, hence, gain fundamental insight of the structural components involved with these processes. The large volume chamber needed for such experiments limits the resolution to about 30 Å, primarily due to electron optics. Figure 1 shows the standard JEOL 2000EX TEM. The UHV chamber in figure 2 replaces the specimen area of the TEM, as shown in figure 3. The chamber is outfitted with Low Energy Electron Diffraction (LEED), Auger Electron Spectroscopy (AES), Residual Gas Analyzer (RGA), gas dosing, and evaporation sources. Reflection Electron Microscopy (REM) is also possible. This instrument is referred to as SHEBA (Surface High-energy Electron Beam Apparatus).The UHV chamber measures 800 mm in diameter and 400 mm in height. JEOL provided adapter flanges for the column.


2008 ◽  
Vol 1142 ◽  
Author(s):  
Hideto Yoshida ◽  
Seiji Takeda ◽  
Tetsuya Uchiyama ◽  
Hideo Kohno ◽  
Yoshikazu Homma

ABSTRACTNucleation and growth processes of carbon nanotubes (CNTs) in iron catalyzed chemical vapor deposition (CVD) have been observed by means of in-situ environmental transmission electron microscopy. Our atomic scale observations demonstrate that solid state iron carbide (Fe3C) nanoparticles act as catalyst for the CVD growth of CNTs. Iron carbide nanoparticles are structurally fluctuated in CVD condition. Growth of CNTs can be simply explained by bulk diffusion of carbon atoms since nanoparticles are carbide.


1990 ◽  
Vol 181 ◽  
Author(s):  
J. M. Gibson ◽  
D. Loretto ◽  
D. Cherns

ABSTRACTWe have studied the formation of metal silicides in-situ in an ultra-high vacuum transmission electron microscope. Metals were deposited on in-situ cleaned, reconstructed silicon surfaces and annealed. For the metals Ni and Co, we find that the phase sequence in ultra-thin films is different from that seen in ≈1000 Å thick films, and attribute this to the high surface-to-volume ratio. In general reactions occur at room temperature, to form an epitaxial phase if possible. We report preliminary new results on the formation of Pd2Si.


2007 ◽  
Vol 1026 ◽  
Author(s):  
Li Sun ◽  
John E. Pearson ◽  
Judith C. Yang

AbstractThe nucleation and growth of Cu2O and NiO islands due to oxidation of Cu-24%Ni(001) films were monitored at various temperatures by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands were observed to form with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. Similar to Cu oxidation, the cross-sectional area growth rate of the oxide island is linear indicating oxygen surface diffusion is the primary mechanism of oxide growth.


1997 ◽  
Vol 3 (S2) ◽  
pp. 583-584
Author(s):  
J. C. Yang ◽  
M. Yeadon ◽  
B. Kolasa ◽  
J. M. Gibson

We studied the beginning oxidation stage of a model metal system by in-situ transmission electron microscopy (TEM) in order to gain insights into the initial kinetics of oxidation. In-situ TEM experiments can distinguish between nucleation and growth since individual oxide islands are imaged. We chose to investigate Cu, since it is a simple face-centered cubic metal. Also, Cu is a highly promising metal interconnect material because of its low resistivity and good electromigration properties as compared to Al.Single crystal -1000Å 99.999% purity copper films were grown on irradiated NaCl in an UHV e-beam evaporator system. The free-standing copper film was placed on a specially designed holder, which permits resistive heating of the sample. The microscope used for this experiment is a modified ultra-high vacuum, with base pressure of 10−9 torr, JEOL200CX, operated at l00kV. To remove the native oxide formed during exposure in air, the Cu film was annealed at ∼350°C


2003 ◽  
Vol 776 ◽  
Author(s):  
Xicheng Ma ◽  
Yuanhua Cai ◽  
Xia Li ◽  
Ning Lun ◽  
Shulin Wen

AbstractHigh-quality cobalt-filled carbon nanotubes (CNTs) were prepared in situ in the decomposition of benzene over Co/silica-gel nano-scale catalysts. Unlike the previous reports, the catalysts needn't be pre-reduced prior to the forming of Co-filled CNTs, thus the advantage of this method is that Co-filled CNTs can be produced in one step, at a relatively low cost. Transmission electron microscopy (TEM) investigation showed that the products contained abundance of CNTs and most of them were filled with metallic nanoparticles or nanorods. High-resolution TEM (HRTEM), selected area electron diffraction (SAED) patterns and energy dispersive X-ray spectroscopy (EDS) confirmed the presence of Co inside the nanotubes. The encapsulated Co was further identified always as high temperature alpha-Co phase with fcc structure, which frequently consists of twinned boundaries and stacking faults. Based on the experimental results, a possible growth mechanism of the Co-filled CNTs was proposed.


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