Facile Synthesis of Pure Boron Nanotubes and Nanofibers

2011 ◽  
Vol 1307 ◽  
Author(s):  
Jinwen Liu ◽  
Zafar Iqbal
Keyword(s):  
Chemical Vapor ◽  
Catalyst Precursor ◽  
Magnesium Boride ◽  
Transmission Electron ◽  
Structure Morphology ◽  
High Resolution Tem ◽  
Crystalline Boron ◽  
Boron Nanostructures ◽  
20 Nm ◽  
Electron Energy Loss

ABSTRACTA facile and scalable chemical vapor deposition (CVD) process in flowing argon using a solid instead of a reactive gaseous boron precursor has been carried out to synthesize crystalline boron nanostructures comprising of relatively straight boron nanotubes (BNTs) and nanofibers (BNFs). The synthesis involves the use of solid magnesium boride as the boron and magnesium catalyst precursor, nickel boride as co-catalyst, and MCM-41 zeolite as the growth template. The BNTs and BNFs produced have a narrow distribution of diameters between about 10 nm to 20 nm and lengths from about 500 nm to above 1 μm. Scanning and transmission electron microscope (SEM and TEM) imaging together with electron energy loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) have been conducted to characterize the structure, morphology and growth mechanism of these novel nanostructures. High resolution TEM imaging has been used to identify BNTs and BNFs in the nanostructures synthesized.

Low Energy Ar Ion Milling of FIB TEM Specimens from 14 nm and Future FinFET Technologies

2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione
Keyword(s):  
Field Effect Transistor ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
High Resolution Tem ◽  
Effect Transistor ◽  
20 Nm ◽  
Argon Ion

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.

Design and Applications of Environmental Cell Transmission Electron Microscope for In Situ Observations of Gas–Solid Reactions

2001 ◽  
Vol 7 (6) ◽  
pp. 494-506 ◽  
Author(s):  
Renu Sharma
Keyword(s):  
Chemical Vapor ◽  
Atomic Level ◽  
Chemical Information ◽  
Oxidation Reduction ◽  
Transmission Electron ◽  
Recent Developments ◽  
Level Information ◽  
Resolution Imaging ◽  
Electron Energy Loss

AbstractThe environmental transmission electron microscopy (E-TEM) is a budding technique for in situ study of gas–solid chemical reactions with numerous applications. Recent improvements in the design have made it possible not only to obtain atomic level information but also the chemical information during the reaction by incorporating an imaging filter or electron energy-loss spectrometer to an E-TEM. We have been involved in modifying a couple of microscopes to incorporate environmental cells in order to convert them into E-TEMs. These microscopes have been used to obtain atomic level information of the structural and chemical changes during dynamic processes by in situ electron diffraction, high-resolution imaging, and electron energyloss spectroscopy. The applications include, but are not limited to, oxidation, reduction, polymerization, nitridation, dehydroxylation, hydroxylation, chemical vapor deposition, etc. We report recent developments in the design and application along with the limitations of an E-TEM.

Fe-encapsulating carbon nano onionlike fullerenes from heavy oil residue

2008 ◽  
Vol 23 (5) ◽  
pp. 1393-1397 ◽  
Author(s):  
Yongzhen Yang ◽  
Xuguang Liu ◽  
Bingshe Xu
Keyword(s):  
Electron Microscopy ◽  
Heavy Oil ◽  
Chemical Vapor ◽  
Catalyst Precursor ◽  
X Ray Diffraction ◽  
Self Assembling ◽  
Transmission Electron ◽  
Oil Residue ◽  
Heavy Oil Residue ◽  
Graphite Sheets

Fe-encapsulating carbon nano onionlike fullerenes (NOLFs) were obtained by chemical vapor deposition (CVD) using heavy oil residue as carbon source and ferrocene as catalyst precursor in an argon flow of 150 mL/min at 900 °C for 30 min. Field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive spectroscopy (EDS), x-ray diffraction (XRD), and Raman spectroscopy were used to characterize morphology and microstructure of the products. The results show that Fe-encapsulating NOLFs collected at the outlet zone of quartz tube had core/shell structures with sizes ranging from 3 to 6 nm and outer shells composed of poorly crystallized graphitic layers. Their growth followed particle self-assembling growth mechanism, and all atoms in the graphite sheets primarily arose from Fe-carbide nanoparticles.

Comparison of Aluminum Nitride Nanowire Growth with and without Catalysts via Chemical Vapor Deposition

2011 ◽  
Vol 1324 ◽  
Author(s):  
Kasif Teker ◽  
Joseph A. Oxenham
Keyword(s):  
Electron Microscopy ◽  
Chemical Vapor Deposition ◽  
Vapor Deposition ◽  
Chemical Vapor ◽  
Systematic Investigation ◽  
Efficient Catalyst ◽  
Force Microscopy ◽  
Transmission Electron ◽  
Direct Nitridation ◽  
20 Nm

ABSTRACTThis paper presents a systematic investigation of AlN nanowire synthesis by chemical vapor deposition using Al and NH3 on SiO2/Si substrate and direct nitridation of mixture of Al-Al2O3 by NH3. A wide variety of catalyst materials, in both discrete nanoparticle and thin film forms, have been used (Co, Au, Ni, and Fe). The growth runs have been carried out at temperatures between 800 and 1100oC mainly under H2 as carrier gas. It was found that the most efficient catalyst in terms of nanowire formation yield was 20-nm Ni film. The AlN nanowire diameters are about 20-30 nm, about the same thickness as the Ni-film. Further studies of direct nitridation of mixture of Al-Al2O3 by NH3 have resulted in high density one-dimensional nanostructure networks at 1100oC. It was observed that catalyst-free nanostructures resulted from the direct nitridation were significantly longer than that with catalysts. The analysis of the grown nanowires has been carried out by scanning electron microscopy, transmission electron microscopy, atomic force microscopy, and x-ray diffraction.

Synthesis and Characterization of Exotic Carbon Fibers with Branched Spurs Using Nickel Catalyst Precursor

2013 ◽  
Vol 645 ◽  
pp. 3-9
Author(s):  
Qian Zhang ◽  
Qiu Xiang Wang ◽  
Hong Zhou Dong ◽  
Li Feng Dong
Keyword(s):  
Electron Microscopy ◽  
Nickel Catalyst ◽  
Carbon Fibers ◽  
Vapor Deposition ◽  
Chemical Vapor ◽  
Chemical Vapor Deposition Method ◽  
Catalyst Precursor ◽  
X Ray ◽  
Transmission Electron

In this paper, we have synt hesized exotic carbon fibers with branched spurs by a chemical vapor deposition method using nickel catalyst precursor at 600 °C. No catalyst particles were found at the base of the carbon spurs, suggesting that the ni ckel catalyst particles, which were decomposed from the nickel catalyst precursor, facilitated the growth of the carbon fibers but not the spurs. The formation of the spurs resulted from the fluctuation of the carbon source gas acetylene flow. The samples were characterized by field emission sc anning electron microscopy, transmission electron microscopy, and X-ray powder diffraction.

Structure of Frilled Carbon Nanowires Synthesized by Sulfur-assisted Chemical Vapor Deposition

2001 ◽  
Vol 706 ◽  
Author(s):  
Tadashi Mitsui ◽  
Takashi Sekiguchi ◽  
Mikka Nishitani-Gamo ◽  
Yafei Zhang ◽  
Toshihiro Ando
Keyword(s):  
Energy Loss ◽  
Electron Energy ◽  
Microwave Plasma ◽  
Chemical Vapor ◽  
Carbon Phase ◽  
Transmission Electron ◽  
Diamond Substrate ◽  
Thin Film Catalyst ◽  
Electron Energy Loss ◽  
Electron Energy Loss Spectra

AbstractEffects of hydrogen sulfide on the structure of carbon nanotubes (CNTs) were studied using high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS). The CNTs were synthesized with an iron thin-film catalyst by microwave plasma-assisted CVD on the diamond substrate. The HRTEM images revealed that essentially all of the CNTs obtained in this study were multiwall (MWCNT). The addition of H2S resulted in nanotubes with split skins as cornhusks and/or frills. Electron energy loss spectra of the cornhusks indicated that they consist of sp2, sp3 and amorphous carbon phase. The spectra revealed that the sp3 to sp2 ratio at the points where cornhusks divide from the main stem was more than that at the edge of the cornhusks. No evidence of sulfur incorporation into the MWCNTs grown with the H2S addition was found. We speculate that the chemical nature of sulfur on the CNT growth yields such anomalous structure.

Nanocrystallization of gas atomized Cu47Ti33Zr11Ni8Si1 metallic glass

2006 ◽  
Vol 21 (3) ◽  
pp. 597-607 ◽  
Author(s):  
S. Venkataraman ◽  
S. Scudino ◽  
J. Eckert ◽  
T. Gemming ◽  
C. Mickel ◽  
...  
Keyword(s):  
Metallic Glass ◽  
Primary Crystallization ◽  
Nanocrystalline Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Transmission Electron ◽  
High Resolution Tem ◽  
20 Nm ◽  
Annealing Experiments

Cu47Ti33Zr11Ni8Si1 metallic glass powder was prepared by gas atomization. Decomposition in the amorphous alloy and primary crystallization has been studied by differential scanning calorimetry (DSC), x-ray diffraction (XRD), and transmission electron microscopy (TEM). The glassy powder exhibits a broad DSC exotherm prior to bulk crystallization. Controlled annealing experiments reveal that this exotherm corresponds to a combination of structural relaxation and nanocrystallization. A uniform featureless amorphous contrast is observed in the TEM prior to the detection of nanocrystals of 4–6 nm in size. High-resolution TEM studies indicate that this nanocrystalline phase has a close crystallographic relationship with the γ–CuTi phase having a tetragonal structure. The product of the main crystallization event is also nanocrystalline, hexagonal Cu51Zr14, having dimensions of 20 nm. However, there is no evidence for possible amorphous phase separation prior to the nanocrystallization events.

Effects of N2O Fluence on the PECVD-grown Si-rich SiOx with Buried Si Nanocrystals

2005 ◽  
Vol 862 ◽  
Author(s):  
Chun-Jung Lin ◽  
Hao-Chung Kuo ◽  
Chia-Yang Chen ◽  
Yu-Lun Chueh ◽  
Li-Jen Chou ◽  
...  
Keyword(s):  
Room Temperature ◽  
Silicon Oxide ◽  
Chemical Vapor ◽  
Blue Shift ◽  
Annealing Process ◽  
Room Temperature Photoluminescence ◽  
Transmission Electron ◽  
Si Nanocrystals ◽  
20 Nm ◽  
Oxidation Effect

AbstractThe optimized N2O fluence is demonstrated for plasma enhanced chemical vapor deposition (PECVD) of Si-rich substoichiometric silicon oxide (SiOx) films with buried Si nanocrystals. Strong room-temperature photoluminescence (PL) at 550-870 nm has been observed in SiOx films grown by PECVD under a constant SiH4 fluence of 20 sccm with an N2O fluence varying from 105 sccm to 130 sccm. A 22-nm-redshift in the central PL wavelength has been detected after annealing from 15 min to 180 min. The maximum PL irradiance is observed from the SiOx film grown at the optimal N2O fluence of 120 sccm after annealing for 30 minutes. Larger N2O fluence or longer annealing time leads to a PL band that is blue-shifted by 65 nm and 20 nm, respectively. Such a blue shift is attributed to shrinkage in the size of the Si nanocrystals with the participation of oxygen atoms from N2O incorporated within the SiOx matrix. The (220)-oriented Si nanocrystals exhibit radii ranging from 4.4 nm to 5.0 nm as determined by transmission electron microscopy (TEM). The luminescent lifetime lengthens to 52 μs as the nc-Si size increase to > 4 nm. Optimal annealing times for SiOx films prepared at different N2O fluences are also reported. A longer annealing process results in a stronger oxidation effect in SiOx films prepared at higher N2O fluences, yielding a lower PL irradiance at shorter wavelengths. In contrast, larger Si nanocrystals can be precipitated when the N2O fluence becomes lower; however, such a SiOx film usually exhibits weaker PL at longer wavelength due to a lower nc-Si density. These results indicate that a N2O/SiH4 fluence ratio of 6:1 is the optimized PECVD growth condition for the Si-rich SiO2 wherein dense Si nanocrystals are obtained after annealing.

HRTEM and EELS Study for Superconducting and Non-Superconducting (Cu,Cr)-1212 Cuprates

2001 ◽  
Vol 7 (S2) ◽  
pp. 402-403
Author(s):  
Y. Anan ◽  
T. Asaka ◽  
H. Kurami ◽  
J. Hatano ◽  
S. Tsutsumi ◽  
...  
Keyword(s):  
Structural Information ◽  
Conduction Block ◽  
Partial Replacement ◽  
One Dimensional ◽  
Superconducting Cuprates ◽  
Transmission Electron ◽  
High Resolution Tem ◽  
Pressure Synthesis ◽  
Electron Energy Loss ◽  
Ba Substitution

The crystal structures of high temperature superconducting cuprates consist of alternative stacking of charge-reservoir (CR) block and conduction block. in case of YBa2Cu3Oy, (YBCO), CR block contains one-dimensional Cu(I)-O chain and BaO layers, and conduction block contains two-dimensional Cu(II)O2 planes and Y layers. YSr2Cu3Oy (YSCO), where Ba-sites of the YBCO are replaced by Sr completely can be obtained only by high-pressure synthesis. However, by replacing Cu(I) partly by Cr, YSr2Cu3-xCrxOy can be obtained even under ambientpressure conditions. The compound YSr2Cu2.8Cr0.2Oy (x=0.2) is non-superconductive, but, superconductivity is induced by partial replacement of Sr-sites with Ba; the compounds with YSr2-xBaxCu2.8Cr0.2Oy (x≤0.5) is non-superconductive, but the compound with x≥1.0 is superconductive. in order to obtain the structural information about the transition to superconducting phases, the effect of the Ba substitution is investigated by transmission electron microscopy (TEM).In the present study, the compounds with YSr2-xBaxCu2.8Cr0.2Oy (x=0-1.5) are examined by high resolution TEM (HRTEM) and electron energy-loss spectroscopy (EELS) to elucidate structural and electrical modification induced by Ba-substitution.

The Atomic, Electronic and Defect Structure of the Dynamically Formed Cu2O/Cu Interfaces

2007 ◽  
Vol 1026 ◽  
Author(s):  
Xuetian Han ◽  
Judith C. Yang
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Island Growth ◽  
Cross Sectional ◽  
Dual Beam ◽  
Transmission Electron ◽  
Initial Stage ◽  
Cu Film ◽  
High Resolution Tem ◽  
Electron Energy Loss

AbstractTo gain fundamental insights into metal oxidation, the dynamically formed Cu/Cu2O interface was investigated by cross-sectional TEM (Transmission Electron Microscopy) methods. Copper (001) films were oxidized in oxygen within a UHV chamber to create Cu2O islands that formed epitaxially with respect to the Cu film. The cross-sectional Cu2O/Cu TEM sample was prepared by dual beam (DB) focused ion beam (FIB) instrument and the interface was probed by high-resolution TEM (HREM) and electron energy loss spectrum (EELS). It is found that Cu2O {110} layer distance significantly decreases from the interface area to the bulk Cu2O region, which is about 3∼4 unit cell thickness in Cu2O side; while the {100Cu2O layer distance increases with increasing distance from the interface region. The chemical Cu/Cu2O interface thickness has been measured with EELS analysis, which is about 2nm where the oxidation state of Cu gradually changes from Cu0 to Cu+1. This transition region indicates the area where Cu/Cu2O interface exists and suggests the existence of metastable Cu oxides. The Cu2O island growth mechanism of predominantly anion interfacial diffusion at the initial stage oxidation has been proposed.

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