Nickel Mediated Transformation of Amorphous Carbon to Graphite

1994 ◽  
Vol 349 ◽  
Author(s):  
Toshio Itoh ◽  
Robert Sinclair

ABSTRACTReactions between Ni and amorphous carbon (a-C) below 600°C have been investigated using differential scanning calorimetry (DSC) and in situ annealing in a transmission electron microscopy (TEM) of Ni/a-C layered films deposited by DC sputtering. DSC data show that there are two exothermic peaks in the temperature range around 200-600°C. One is a weak and broad peak below 500°C and the other is a strong and sharp peak at around 530°C. In situ heating in the TEM revealed that the low temperature peak corresponds to a series of reactions for nickel carbide (Ni3C) formation and decomposition into Ni and carbon, most likely in a glassy state. The higher temperature peak was found to correspond to graphitization of a-C by a solution-precipitation mechanism. Graphite formed in this process is strongly textured with the (0002) graphite basal planes parallel to the original Ni/a-C interface.

1991 ◽  
Vol 237 ◽  
Author(s):  
Toyohiko J. Konno ◽  
Robert Sinclair

ABSTRACTThe crystallization of sputter-deposited Si/Al amorphous alloys was examined by transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). In-situ high-resolution TEM reveals the existence of an Al layer between the amorphous matrix and the growing crystalline phase. The activation energy for the growth is about 1.2eV, roughly corresponding to the activation energy of Si diffusion in Al. These two observations support the view that a crystallization mechanism, in which an Al buffer layer provides the shortest reaction path, is responsible for the reaction. The product microstructure exhibits secondary crystallization at a higher temperature.


2002 ◽  
Vol 8 (4) ◽  
pp. 288-304 ◽  
Author(s):  
Robert Sinclair ◽  
Toshio Itoh ◽  
Richard Chin

The reactions which occur between amorphous carbon and a number of first transition metals (Ti, Cr, Fe, Co, Ni, and Cu) have been studied by transmission electron microscopy (TEM). The materials are in thin-film form with the metal layer sandwiched between thicker carbon layers. In four cases, the predominant reaction is the graphitization of the amorphous carbon, at temperatures well below 800°C. This is brought about by the elements themselves in the case of Co and Ni, and by metastable carbides in the case of Fe (Fe3C) and Cr (Cr3C2−x). The Ti–C and Cu–C systems do not exhibit graphitization. For the former, only TiC is produced up to 1000°C, while the carbon does not react at all with copper. In situ TEM studies show the mechanism to be of the dissolution-precipitation type, which is equivalent to the metal-mediated crystallization process for amorphous silicon and germanium. The heat of graphitization is found to be 18–19 kcal/mol-C by differential scanning calorimetry.


Author(s):  
Mihaela Albu ◽  
Bernd Panzirsch ◽  
Hartmuth Schröttner ◽  
Stefan Mitsche ◽  
Klaus Reichmann ◽  
...  

Powder and SLM additively manufactured parts of X5CrNiCuNb17-4 maraging steel were systematically investigated by electron microscopy to understand the relationship between the properties of the powder grains and the microstructure of the printed parts. We prove that satellites, irregularities and superficial oxidation of powder particles can be transformed into an advantage through the formation of nanoscale (AlMnSiTiCr)-oxides in the matrix during the printing process. The nano-oxides showed extensive stability in terms of size, spherical morphology, chemical composition and crystallographic disorder upon in situ heating up to 950°C in the scanning transmission electron microscope. Their presence thus indicates a potential for oxide-dispersive strengthening of this steel, which may be beneficial for creep resistance at elevated temperatures. The nucleation of copper clusters and their evolution into nanoparticles as well as the precipitation of Ni and Cr particles upon in situ heating have as well been systematically documented.


2008 ◽  
Vol 1066 ◽  
Author(s):  
Ram Kishore ◽  
Renu Sharma ◽  
Satoshi Hata ◽  
Noriyuki Kuwano ◽  
Yoshitsuga Tomokiyo ◽  
...  

ABSTRACTThe interaction of amorphous silicon and aluminum films to achieve polycrystalline silicon has been investigated using transmission electron microscope equipped with in-situ heating holder. Carbon coated nickel grids were used for TEM studies. An ultra high vacuum cluster tool was used for the deposition of a ∼50nm a-Si films and a vacuum deposition system was used to deposit a ∼50nm Al films on a-Si film. The microstructural features and electron diffraction in the plain view mode were observed with increase in temperature starting from room temperature to 275 °C. The specimen was loaded inside TEM heating holder. The temperature was measured and kept constant for 5 minutes during which the microstructure at fixed magnification of X63K was recorded and the electron diffraction pattern of the same area was also recorded. The temperature was then increase and fixed at desired value and microstructure and EDP were again recorded. The temperatures used in this experiment were 30, 100, 150, 200, 225, 275°C. A sequential change in microstructural features and electron diffraction pattern due to interfacial diffusion of boundary between Al and amorphous Si was investigated. Evolution of polycrystalline silicon with randomly oriented grains as a result of a-Si and Al interaction was revealed. After the in-situ heating experiment the specimen was subjected to high resolution TEM and EDS investigations after removing the excess Al. The EDS analysis of the crystallized specimen was performed to locate the Al distribution in the crystallized silicon. These studies show that the Al induced crystallization process can be used to prepare polycrystalline as well as nanocrystalline silicon by controlling the in-situ annealing parameters. The investigations are very useful as the nanocrystalline silicon is being investigated for its use in developing high efficiency silicon solar structures.


1993 ◽  
Vol 311 ◽  
Author(s):  
Robert Sinclair ◽  
Toyohiko J. Konno

ABSTRACTWe have studied the reactions at metal-metalloid interfaces using high resolution transmission electron microscopy, including in situ observation, and differential scanning calorimetry. There is contrasting behavior depending on the affinity for interaction or segregation. For reactive systems, compound formation ultimately results, but this can be preceded by solidstate amorphization. For non-reactive systems, crystallization of the metalloid is often achieved with nucleation and growth mediated by the metal phase.


2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.


2020 ◽  
Vol 321 ◽  
pp. 11035
Author(s):  
E. Sukedai ◽  
E. Aeby-Gautier ◽  
M. Dehmas

A Ti-5553 specimen was continuously heated to 923 K and simultaneously in-situ HEXRD profiles were taken. In addition, specimens heated at the same rate to several temperatures up to 923 K and further quenched were observed by transmission electron microscopy. Based on both results obtained, transformation sequence was clarified, precipitations of ω-, α”iso- and α-phases were confirmed, and size and density of these precipitates were measured. Hardness values of those specimens were also measured. The hardening mechanism was considered as shearing-mechanism for specimens aged at lower temperatures and by-pass one for specimens aged at higher temperature. An attempt of distinction between α”iso - and α-precipitates was also tried. Both precipitates were in needle-like shape and a possibility was suggested by measuring angles between two needle-shape precipitates on {110} of the matrix and comparing with each other.


1996 ◽  
Vol 439 ◽  
Author(s):  
P. Werner ◽  
U. Gösele ◽  
H. Kohda

AbstractHighly carbon doped GaAs layers grown by metal organic vapor phase epitaxy (MOVPE) Has been investigated by transmission electron microscopy (TEM). Electron irradiation has been applied to generate point defects interacting with native defects, e.g., substitutional carbon. This irradiation induces periodically arranged striations perpendicular to the growth direction, which were observed in situ by TEM. Furthermore, precipitates (Ø= 10–15nm) were formed containing non-crystalline material, which most likely is gallium. To explain these phenomena a precipitation mechanism is proposed. It involvs small fluctuations of the incorporated C as well as the interaction of irradiation induced point defects, mainly As and C interstitials and As vacancies.


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