scholarly journals Elasticity of Cross-Linked Titania Nanocrystal Assemblies Probed by AFM-Bulge Tests

Nanomaterials ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 1230 ◽  
Author(s):  
Hensel ◽  
Schröter ◽  
Schlicke ◽  
Schulz ◽  
Riekeberg ◽  
...  

In order to enable advanced technological applications of nanocrystal composites, e.g., as functional coatings and layers in flexible optics and electronics, it is necessary to understand and control their mechanical properties. The objective of this study was to show how the elasticity of such composites depends on the nanocrystals’ dimensionality. To this end, thin films of titania nanodots (TNDs; diameter: ~3–7 nm), nanorods (TNRs; diameter: ~3.4 nm; length: ~29 nm), and nanoplates (TNPs; thickness: ~6 nm; edge length: ~34 nm) were assembled via layer-by-layer spin-coating. 1,12-dodecanedioic acid (12DAC) was added to cross-link the nanocrystals and to enable regular film deposition. The optical attenuation coefficients of the films were determined by ultraviolet/visible (UV/vis) absorbance measurements, revealing much lower values than those known for titania films prepared via chemical vapor deposition (CVD). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images showed a homogeneous coverage of the substrates on the µm-scale but a highly disordered arrangement of nanocrystals on the nm-scale. X-ray photoelectron spectroscopy (XPS) analyses confirmed the presence of the 12DAC cross-linker after film fabrication. After transferring the films onto silicon substrates featuring circular apertures (diameter: 32–111 µm), freestanding membranes (thickness: 20–42 nm) were obtained and subjected to atomic force microscopy bulge tests (AFM-bulge tests). These measurements revealed increasing elastic moduli with increasing dimensionality of the nanocrystals, i.e., 2.57 ± 0.18 GPa for the TND films, 5.22 ± 0.39 GPa for the TNR films, and 7.21 ± 1.04 GPa for the TNP films.

2008 ◽  
Vol 18 (04) ◽  
pp. 901-910
Author(s):  
RAGNAR KIEBACH ◽  
ZHENRUI YU ◽  
MARIANO ACEVES-MIJARES ◽  
DONGCAI BIAN ◽  
JINHUI DU

The formation of nano sized Si structures during the annealing of silicon rich oxide (SRO) films was investigated. These films were synthesized by low pressure chemical vapor deposition (LPCVD) and used as precursors, a post-deposition thermal annealing leads to the formation of Si nano crystals in the SiO 2 matrix and Si nano islands ( Si nI ) at c-Si /SRO interface. The influences of the excess Si concentration, the incorporation of N in the SRO precursors, and the presence of a Si concentration gradient on the Si nI formation were studied. Additionally the influence of pre-deposition substrate surface treatments on the island formation was investigated. Therefore, the substrate surface was mechanical scratched, producing high density of net-like scratches on the surface. Scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) were used to characterize the synthesized nano islands. Results show that above mentioned parameters have significant influences on the Si nIs . High density nanosized Si islands can epitaxially grow from the c-Si substrate. The reported method is very simple and completely compatible with Si integrated circuit technology.


2002 ◽  
Vol 747 ◽  
Author(s):  
M. P. Singh ◽  
C. S. Thakur ◽  
N. Bhat ◽  
S. A. Shivashankar

ABSTRACTWe report the characterization of carbonaceous aluminium oxide, Al2O3:C, films grown on Si(100) by metalorganic chemical vapor deposition. The focus is on the study of the effects of carbon on the dielectric properties of aluminium oxide in a qualitative manner. The carbon present in the aluminium oxide film derives from aluminium acetylacetonate used as the source of aluminium. As-grown films comprise nanometer-sized grains of alumina (∼ 20–50 nm) in an amorphous carbonaceous matrix, as examined by X-ray diffractometry (XRD) and transmission electron microscopy (TEM). The films are shiny; they are smooth as observed by scanning electron microscopy (SEM). An attempt has been made to explore the defects (viz., oxide charge density) in the aluminium oxide films using room temperature high frequency capacitance – voltage (C-V) and current–voltage (I-V) measurements. The hysteresis and stretch-out in the high frequency C-V plots is indicative of charge trapping. The role of heteroatoms, as characterized by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) spectroscopy, in the transport of charge in Al2O3:C films is discussed.


1986 ◽  
Vol 1 (3) ◽  
pp. 420-424 ◽  
Author(s):  
T.R. Jervis ◽  
L.R. Newkirk

Dielectric breakdown of gas mixtures can be used to deposit thin films by chemical vapor deposition with appropriate control of flow and pressure conditions to suppress gas-phase nucleation and particle formation. Using a pulsed CO2 laser operating at 10.6 μ where there is no significant resonant absorption in any of the source gases, homogeneous films from several gas-phase precursors have been sucessfully deposited by gas-phase laser pyrolysis. Nickel and molybdenum from the respective carbonyls representing decomposition chemistry and tungsten from the hexafluoride representing reduction chemistry have been demonstrated. In each case the gas precursor is buffered with argon to reduce the partial pressure of the reactants and to induce breakdown. Films have been characterized by Auger electron spectroscopy, x-ray diffraction, transmission electron microscopy, pull tests, and resistivity measurements. The highest quality films have resulted from the nickel depositions. Detailed x-ray diffraction analysis of these films yields a very small domain size consistent with the low temperature of the substrate and the formation of metastable nickel carbide. Transmission electron microscopy supports this analysis.


1990 ◽  
Vol 202 ◽  
Author(s):  
Garth B. Freeman ◽  
Woo Y. Lee ◽  
W. J. Lackey ◽  
John A. Hanigofsky ◽  
Karren More

ABSTRACTThis paper discusses the variation in microstructures encountered during the separate depositions of boron nitride (BN) and aluminum nitride (A1N) as well as during the codeposition of BNߝA1N dispersed phase ceramic coatings. This combination was chosen in order to take advantage of the self lubricating properties of hexagonal BN along with the hard, erosion resistance of A1N. Films were characterized using scanning and transmission electron microscopy (SEM and TEM), x-ray photoelectron spectroscopy (XPS), and x-ray diffraction (XRD).A range of coating microstructures are possible depending on the conditions of deposition. The best films produced, in terms of hardness, density, and tenacity, were a fine mixture of turbostratic BN and preferentially oriented A1N whiskers aligned with the whisker axis perpendicular to the substrate surface as seen by both electron microscopy and x-ray diffraction.


2002 ◽  
Vol 745 ◽  
Author(s):  
M. P. Singh ◽  
C. S. Thakur ◽  
N. Bhat ◽  
S. A. Shivashankar

ABSTRACTWe report the characterization of carbonaceous aluminium oxide, Al2O3:C, films grown on Si(100) by metalorganic chemical vapor deposition. The focus is on the study of the effects of carbon on the dielectric properties of aluminium oxide in a qualitative manner. The carbon present in the aluminium oxide film derives from aluminium acetylacetonate used as the source of aluminium. As-grown films comprise nanometer-sized grains of alumina (∼ 20–50 nm) in an amorphous carbonaceous matrix, as examined by X-ray diffractometry (XRD) and transmission electron microscopy (TEM). The films are shiny; they are smooth as observed by scanning electron microscopy (SEM). An attempt has been made to explore the defects (viz., oxide charge density) in the aluminium oxide films using room temperature high frequency capacitance – voltage (C-V) and current–voltage (I-V) measurements. The hysteresis and stretch-out in the high frequency C-V plots is indicative of charge trapping. The role of heteroatoms, as characterized by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) spectroscopy, in the transport of charge in Al2O3:C films is discussed.


2021 ◽  
Vol 21 (6) ◽  
pp. 3183-3191
Author(s):  
Shanmugam Mahalingam ◽  
Mani Durai ◽  
Chinnasamy Sengottaiyan ◽  
Young-Ho Ahn

Here we reports an effective synthetic method for the preparation of N-graphene upon thermal annealing of prepared graphene oxide in the existence of ammonia. N-doped graphene oxide was analysed using different characterization techniques like X-ray diffraction, field emission scanning electron microscopy, high resolution transmission electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The nitrogen atom showed good binding with the graphene sheets, that are analysed by the X-ray photoelectron spectroscopy. The synthesized N-graphene have shown higher thermal stability compared with GO and graphene. The elcerochemnical performance like Cyclic voltammetry as well chronopotentiometry charge–discharge calculations revealed that the N-doped graphene exhibits remarkable behaviour favors a specific capacitance value about 209 F g−1 at 5 mV s−1 and 270 F g−1 for 1 A g−1 applied current density including outsanding charge–discharge stability about 98% of the initial capacitance subsequent 1000 cycles at 5 A g−1. The N-content in the graphene material with the optimized reaction parameters potentially improved electrode active material for energy storage applications.


MRS Advances ◽  
2018 ◽  
Vol 3 (4) ◽  
pp. 191-197
Author(s):  
José E. Nocua ◽  
Gerardo Morell

ABSTRACTBoron nitride (BN) has a very high thermal conductivity and excellent thermal shock resistance. These properties make BN an important material for industrial applications involving surfaces in contact with molten metals. These applications require straightforward deposition methods that produce uniform BN coatings. Using borazine (B3N3H6) as a precursor, we deposited BN coatings on silicon substrates by cold-wall chemical vapor deposition (CVD). The microstructure, composition, and morphology of the coatings were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and electron energy loss spectroscopy (EELS). These characterizations show that the BN coatings deposited are uniform, predominantly of hexagonal structure, and N-rich.


2004 ◽  
Vol 19 (10) ◽  
pp. 3009-3018 ◽  
Author(s):  
Kyung-Hwan Lee ◽  
Jin-Kook Yoon ◽  
Gyeung-Ho Kim ◽  
Jung-Mann Doh ◽  
Kyung-Tae Hong ◽  
...  

Growth behavior and microstructure of oxide scale formed on MoSi2 coating by cyclic oxidation testing in air at 500 °C were investigated using field emission scanning electron microscopy, cross-sectional transmission electron microscopy, glancing angle x-ray diffraction, and x-ray photoelectron spectroscopy. MoSi2 coating was prepared by chemical vapor deposition of Si on a Mo substrate at 1100 °C for 5 h using SiCl4–H2 precursor gas mixtures. After the incubation period of about 454 cycles, accelerated oxidation behavior was observed in MoSi2 coating and the weight gain increased linearly with increasing oxidation cycles. Microstructural analyses revealed that pest oxide scale was formed in three sequential processes. Initially, nanometer-sized crystalline Mo4O11 particles were formed with an amorphous SiO2 matrix at MoSi2 interface region. Inward diffusing oxygen reacted with Mo4O11 to form Mo9O26 nano-sized particles. At final stage of oxidation, MoO3 was formed from Mo9O26 with oxygen and growth of MoO3 took place forming massive precipitates with irregular and wavy shapes. The internal stress caused by the growth of massive MoO3 precipitates and the volatilization of MoO3 was attributed to the formation of many lateral cracks into the matrix leading to pest oxidation of MoSi2 coating.


Author(s):  
N. D. Evans ◽  
M. K. Kundmann

Post-column energy-filtered transmission electron microscopy (EFTEM) is inherently challenging as it requires the researcher to setup, align, and control both the microscope and the energy-filter. The software behind an EFTEM system is therefore critical to efficient, day-to-day application of this technique. This is particularly the case in a multiple-user environment such as at the Shared Research Equipment (SHaRE) User Facility at Oak Ridge National Laboratory. Here, visiting researchers, who may oe unfamiliar with the details of EFTEM, need to accomplish as much as possible in a relatively short period of time.We describe here our work in extending the base software of a commercially available EFTEM system in order to automate and streamline particular EFTEM tasks. The EFTEM system used is a Philips CM30 fitted with a Gatan Imaging Filter (GIF). The base software supplied with this system consists primarily of two Macintosh programs and a collection of add-ons (plug-ins) which provide instrument control, imaging, and data analysis facilities needed to perform EFTEM.


Author(s):  
L. Hultman ◽  
C.-H. Choi ◽  
R. Kaspi ◽  
R. Ai ◽  
S.A. Barnett

III-V semiconductor films nucleate by the Stranski-Krastanov (SK) mechanism on Si substrates. Many of the extended defects present in the films are believed to result from the island formation and coalescence stage of SK growth. We have recently shown that low (-30 eV) energy, high flux (4 ions per deposited atom), Ar ion irradiation during nucleation of III-V semiconductors on Si substrates prolongs the 1ayer-by-layer stage of SK nucleation, leading to a decrease in extended defect densities. Furthermore, the epitaxial temperature was reduced by >100°C due to ion irradiation. The effect of ion bombardment on the nucleation mechanism was explained as being due to ion-induced dissociation of three-dimensional islands and ion-enhanced surface diffusion.For the case of InAs grown at 380°C on Si(100) (11% lattice mismatch), where island formation is expected after ≤ 1 monolayer (ML) during molecular beam epitaxy (MBE), in-situ reflection high-energy electron diffraction (RHEED) showed that 28 eV Ar ion irradiation prolonged the layer-by-layer stage of SK nucleation up to 10 ML. Otherion energies maintained layer-by-layer growth to lesser thicknesses. The ion-induced change in nucleation mechanism resulted in smoother surfaces and improved the crystalline perfection of thicker films as shown by transmission electron microscopy and X-ray rocking curve studies.


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