A special method to evaluate the strong adhesion between brittle coating and ductile substrate

The evaluation of the interfacial adhesion of coating system has always been a rough task. In this paper, a special testing method of cross-sectional indentation is applied on a model coating system, i.e. electroplated chromium on a steel substrate which is generally regarded as an example of materials pair with strong adhesion. Based on fractography analysis with SEM and interfacial stress simulation with FEM, it is found that interfacial shear stress may induce coating spalling. More interestingly, spalling location is sensitive to substrate pretreatment process. This shows the feasibility of cross-sectional indentation to distinguish interfacial strength at a high level.

Control of wettability of carbon nanotube array by reversible dry oxidation for superhydrophobic coating and supercapacitor applications

In this thesis, dry chemical modification methods involving UV/ozone, oxygen plasma, and vacuum annealing treatments are explored to precisely control the wettability of CNT arrays. By varying the exposure time of these treatments the surface concentration of oxygenated groups adsorbed on the CNT arrays can be controlled. CNT arrays with very low amount of oxygenated groups exhibit a superhydrophobic behavior. In addition to their extremely high static contact angle, they cannot be dispersed in DI water and their impedance in aqueous electrolytes is extremely high. These arrays have an extreme water repellency capability such that a water droplet will bounce off of their surface upon impact and a thin film of air is formed on their surface as they are immersed in a deep pool of water. In contrast, CNT arrays with very high surface concentration of oxygenated functional groups exhibit an extreme hydrophilic behavior. In addition to their extremely low static contact angle, they can be dispersed easily in DI water and their impedance in aqueous electrolytes is tremendously low. Since the bulk structure of the CNT arrays are preserved during the UV/ozone, oxygen plasma, and vacuum annealing treatments, all CNT arrays can be repeatedly switched between superhydrophilic and superhydrophobic, as long as their O/C ratio is kept below 18%.

The effect of oxidation using UV/ozone and oxygen plasma treatments is highly reversible as long as the O/C ratio of the CNT arrays is kept below 18%. At O/C ratios higher than 18%, the effect of oxidation is no longer reversible. This irreversible oxidation is caused by irreversible changes to the CNT atomic structure during the oxidation process. During the oxidation process, CNT arrays undergo three different processes. For CNT arrays with O/C ratios lower than 40%, the oxidation process results in the functionalization of CNT outer walls by oxygenated groups. Although this functionalization process introduces defects, vacancies and micropores opening, the graphitic structure of the CNT is still largely intact. For CNT arrays with O/C ratios between 40% and 45%, the oxidation process results in the etching of CNT outer walls. This etching process introduces large scale defects and holes that can be obviously seen under TEM at high magnification. Most of these holes are found to be several layers deep and, in some cases, a large portion of the CNT side walls are cut open. For CNT arrays with O/C ratios higher than 45%, the oxidation process results in the exfoliation of the CNT walls and amorphization of the remaining CNT structure. This amorphization process can be implied from the disappearance of C-C sp2 peak in the XPS spectra associated with the pi-bond network.

The impact behavior of water droplet impinging on superhydrophobic CNT arrays in a low viscosity regime is investigated for the first time. Here, the experimental data are presented in the form of several important impact behavior characteristics including critical Weber number, volume ratio, restitution coefficient, and maximum spreading diameter. As observed experimentally, three different impact regimes are identified while another impact regime is proposed. These regimes are partitioned by three critical Weber numbers, two of which are experimentally observed. The volume ratio between the primary and the secondary droplets is found to decrease with the increase of Weber number in all impact regimes other than the first one. In the first impact regime, this is found to be independent of Weber number since the droplet remains intact during and subsequent to the impingement. Experimental data show that the coefficient of restitution decreases with the increase of Weber number in all impact regimes. The rate of decrease of the coefficient of restitution in the high Weber number regime is found to be higher than that in the low and moderate Weber number. Experimental data also show that the maximum spreading factor increases with the increase of Weber number in all impact regimes. The rate of increase of the maximum spreading factor in the high Weber number regime is found to be higher than that in the low and moderate Weber number. Phenomenological approximations and interpretations of the experimental data, as well as brief comparisons to the previously proposed scaling laws, are shown here.

Dry oxidation methods are used for the first time to characterize the influence of oxidation on the capacitive behavior of CNT array EDLCs. The capacitive behavior of CNT array EDLCs can be tailored by varying their oxygen content, represented by their O/C ratio. The specific capacitance of these CNT arrays increases with the increase of their oxygen content in both KOH and Et4NBF4/PC electrolytes. As a result, their gravimetric energy density increases with the increase of their oxygen content. However, their gravimetric power density decreases with the increase of their oxygen content. The optimally oxidized CNT arrays are able to withstand more than 35,000 charge/discharge cycles in Et4NBF4/PC at a current density of 5 A/g while only losing 10% of their original capacitance.

High fidelity probe and mitigation of mirror thermal fluctuations

Thermal noise arising from mechanical loss in high reflective dielectric coatings is a significant source of noise in precision optical measurements. In particular, Advanced LIGO, a large scale interferometer aiming to observed gravitational wave, is expected to be limited by coating thermal noise in the most sensitive region around 30–300 Hz. Various theoretical calculations for predicting coating Brownian noise have been proposed. However, due to the relatively limited knowledge of the coating material properties, an accurate approximation of the noise cannot be achieved. A testbed that can directly observed coating thermal noise close to Advanced LIGO band will serve as an indispensable tool to verify the calculations, study material properties of the coating, and estimate the detector’s performance.

This dissertation reports a setup that has sensitivity to observe wide band (10Hz to 1kHz) thermal noise from fused silica/tantala coating at room temperature from fixed-spacer Fabry–Perot cavities. Important fundamental noises and technical noises associated with the setup are discussed. The coating loss obtained from the measurement agrees with results reported in the literature. The setup serves as a testbed to study thermal noise in high reflective mirrors from different materials. One example is a heterostructure of Al_xGa_1−xAs (AlGaAs). An optimized design to minimize thermo–optic noise in the coating is proposed and discussed in this work.

Magnetic alignment of high-aspect ratio microwires into vertical arrays

Fundamental studies of magnetic alignment of highly anisotropic mesostructures can enable the clean-room-free fabrication of flexible, array-based solar and electronic devices, in which preferential orientation of nano- or microwire-type objects is desired. In this study, ensembles of 100 micron long Si microwires with ferromagnetic Ni and Co coatings are oriented vertically in the presence of magnetic fields. The degree of vertical alignment and threshold field strength depend on geometric factors, such as microwire length and ferromagnetic coating thickness, as well as interfacial interactions, which are modulated by varying solvent and substrate surface chemistry. Microwire ensembles with vertical alignment over 97% within 10 degrees of normal, as measured by X-ray diffraction, are achieved over square cm scale areas and set into flexible polymer films. A force balance model has been developed as a predictive tool for magnetic alignment, incorporating magnetic torque and empirically derived surface adhesion parameters. As supported by these calculations, microwires are shown to detach from the surface and align vertically in the presence of magnetic fields on the order of 100 gauss. Microwires aligned in this manner are set into a polydimethylsiloxane film where they retain their vertical alignment after the field has been removed and can subsequently be used as a flexible solar absorber layer. Finally, these microwires arrays can be protected for use in electrochemical cells by the conformal deposition of a graphene layer.

High-efficiency reflective diffraction gratings in fused silica as (de)multiplexers at 1.55 mu m for dense wavelength division multiplexing application

We describe high-efficiency, high-dispersion reflection gratings fabricated in bulk fused Silica illuminated by incident lights in the C + L bands as (de)multiplexers for dense wavelength division multiplexing (DWDM) application. Based on the phenomenon of total internal reflection, gratings with optimized profile parameters exhibit diffraction efficiencies of more than 90% under TM- and TE-polarized incident lights for 101-nm spectral bandwidths (1520-1620 nm) and can reach an efficiency of greater than 97% for both polarizations at a wavelength of 1550 nm. Without loss of metal absorption, without coating of dielectric film layers, and independent of tooth shape, this new kind of grating should be of great interest for DWDM application. (C) 2005 Optical Society of America.

Synthesis of nickel(II) complexes of alpha-isoxazolylazo-beta-diketones and their absorption of spin-coating films and thermal properties for HD-DVD-R

Three kinds of new nickel(II) complexes of alpha-isoxazolylazo-beta-diketones with blue-violet light absorption were synthesized. Their structures were postulated based on elemental analysis, MS and FT-IR spectra. Smooth films on K9 glass substrates were prepared using the spin-coating method. The absorption properties and thermal stability of these complexes were discussed. The static optical recording test for high density digital versatile disc-recordable (HD-DVD-R) system was also studied. (c) 2005 Elsevier B.V. All rights reserved.

Preparation, characterization and gas sensing properties of nickel octa-iso-pentyloxynaphthalocyanine spin-coating films

Spin-coated films of nickel 1,6,10,15,19,24,28,33-octa-iso-pentyloxy-2,3-naphthalocyanine complex were obtained and characterized by UV-vis absorption spectroscopy. A linear relationship between the absorbance and solution concentration was observed. Low concentration solutions could afford smooth and homogeneous film surfaces as indicated by atomic force microscopy. The film structure was studied by small angle X-ray diffraction. The films were used for NO2 sensing experiments. The results indicate that the elevation of sensing temperature can shorten the response time and increase recovery ratio and response magnitude of the sensing films. High NO2 concentration can also shorten response time. (C) 2008 Elsevier B.V. All rights reserved.

Rare earth dibenzoylmethane complexes for potential application as high-density recordable optical recording materials

Three kinds of rare earth complexes derived from dibenzoylmethane (DBM) ligand were synthesized by reacting free ligand and different rare earth ions(La (3+), Sm3+ and Gd3+). Their contents and structures were postulated based on elemental analysis, LDI-TOF-MS, FT-IR spectra and UV-Vis spectra. Smooth films on K9 glass substrates were prepared using the spin-coating method. Their solubility in organic solvents, absorption and reflection properties of thin film and thermal stability of these complexes were evaluated. These complexes would be a promising recording material for high-density digital versatile disc-recordable (HD-DVD-R) system. (c) 2007 Elsevier B.V. All rights reserved.

Investigation on the properties of high reflective mirror prepared by ion-beam sputtering

The single-sided and dual-sided high reflective mirrors were deposited with ion-beam sputtering (IBS). When the incident light entered with 45 degrees, the reflectance of p-polarized light at 1064 nm exceeded 99.5%. Spectrum was gained by spectrometer and weak absorption of coatings was measured by surface thermal lensing (STL) technique. Laser-induced damage threshold (LIDT) was determined and the damage morphology was observed with Lecia-DMRXE microscope simultaneously. The profile of coatings was measured with Mark III-GPI digital interferometer. It was found that the reflectivity of mirror exceeded 99.9% and its absorption was as low as 14 ppm. The reflective bandwidth of the dual-sided sample was about 43 nm wider than that of single-sided sample, and its LIDT was as high as 28 J/cm2, which was 5 J/cm2 higher than that of single-sided sample. Moreover, the profile of dual-sided sample was better than that of substrate without coatings.

Comparison of femtosecond and nanosecond laser-induced damage in HfO2 single-layer film and HfO2-SiO2 high reflector

HfO2 single layers, 800 run high-reflective (HR) coating, and 1064 ran HR coating were prepared by electron-beam evaporation. The laser-induced damage thresholds (LIDTs) and damage morphologies of these samples were investigated with single-pulse femtosecond and nanosecond lasers. It is found that the LIDT of the HfO2 single layer is higher than the HfO2-SiO2 HR coating in the femtosecond regime, while the situation is opposite in the nanosecond regime. Different damage mechanisms are applied to study this phenomenon. Damage morphologies of all samples due to different laser irradiations are displayed. (c) 2007 Optical Society of America.

Effect of SiO2 protective layer on the femtosecond laser-induced damage of HfO2/SiO2 multilayer high-reflective coatings

Two kinds of HfO2/SiO2 800 nm high-reflective (HR) coatings, with and without SiO2 protective layer were deposited by electron beam evaporation. Laser-induced damage thresholds (LIDT) were measured for all samples with femtosecond laser pulses. The surface morphologies and the depth information of all samples were observed by Leica optical microscopy and WYKO surface profiler, respectively. It is found that SiO2 protective layer had no positive effect on improving the LIDT of HR coating. A simple model including the conduction band electron production via multiphoton ionization and impact ionization is used to explain this phenomenon. Theoretical calculations show that the damage occurs first in the SiO2 protective layer for HfO2/SiO2 HR coating with SiO2 protective layer. The relation of LIDT for two kinds of HfO2/SiO2 HR coatings in calculation agrees with the experiment result. (c) 2006 Elsevier B.V. All rights reserved.

Photosynthetic responses of trees in high-elevation forests: comparing evergreen species along an elevation gradient in the Central Andes

Plant growth at extremely high elevations is constrained by high daily thermal amplitude, strong solar radiation and water scarcity. These conditions are particularly harsh in the tropics, where the highest elevation treelines occur. In this environment, the maintenance of a positive carbon balance involves protecting the photosynthetic apparatus and taking advantage of any climatically favourable periods. To characterize photoprotective mechanisms at such high elevations, and particularly to address the question of whether these mechanisms are the same as those previously described in woody plants along extratropical treelines, we have studied photosynthetic responses in Polylepis tarapacana Philippi in the central Andes (18 degrees S) along an elevational gradient from 4300 to 4900 m. For comparative purposes, this gradient has been complemented with a lower elevation site (3700 m) where another Polylepis species (P. rugulosa Bitter) occurs. During the daily cycle, two periods of photosynthetic activity were observed: one during the morning when, despite low temperatures, assimilation was high; and the second starting at noon when the stomata closed because of a rise in the vapour pressure deficit and thermal dissipation is prevalent over photosynthesis. From dawn to noon there was a decrease in the content of antenna pigments (chlorophyll b and neoxanthin), together with an increase in the content of xanthophyll cycle carotenoids. These results could be caused by a reduction in the antenna size along with an increase in photoprotection. Additionally, photoprotection was enhanced by a partial overnight retention of de-epoxized xanthophylls. The unique combination of all of these mechanisms made possible the efficient use of the favourable conditions during the morning while still providing enough protection for the rest of the day. This strategy differs completely from that of extratropical mountain trees, which uncouple light-harvesting and energy-use during long periods of unfavourable, winter conditions.

High speed titanium coatings by supersonic laser deposition

The importance of metal coating technologies drives the continuous improvement of metal deposition techniques for application in a wide range of industrial sectors. This work presents the foundations of a new process technology for the deposition of titanium coatings on steel tube substrates using supersonic powder streams and impact site laser heating, known as Supersonic Laser Deposition (SLD). Metallic deposits are obtained under appropriate impact conditions without the need for exceeding the melting point of the deposited material or substrate leading to improved coating quality. Details of the experimental approach are presented along with the general characteristics of the titanium coating produced using this novel coatings method. © 2011 Elsevier B.V. All rights reserved.

Effect of laser heating temperature on coating characteristics of Stellite 6 deposited by cold spray

Laser-assisted cold spray (LCS) is a new coating and fabrication process which combines some advantages of CS: solid-state deposition, retain their initial composition and high build rate with the ability to deposit materials which are either difficult or impossible to deposit using cold spray alone. Stellite 6 powder is deposited on medium carbon steels by LCS using N 2 as carrier gas pressure. The topography, cross section thickness, structure of the coatings is examined by SEM, optical microscopy, EDX. The results show that thickness and fluctuation of coating are improved with increased deposition site temperature. Porosity of coating is affected by N 2 and deposition site temperature. In this paper, it presents optimal coating using N 2 at a pressure of 3 MPa and temperature of 450°C and deposition site temperature of 1100°C.

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

A novel fiber coated with novel sol-gel (5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix[4]arene/hydroxy-terminated silicone oil; diglycidyloxy-C[4]/OH-TSO) was prepared for use with headspace solid-phase microextraction (HS-SPME) combined with gas chromatography (GC) and electron capture detection (ECD), which was applied in order to determine nine chlorobenzenes in soil matrices. Due to the improved fiber preparation, which increases the percentage of calixarene in the coating, the new calixarene fiber exhibits very high extraction selectivity and sensitivity to chlorine-substituted compounds. Various parameters affecting the extraction efficiency were optimized in order to maximize the sensitivity during the chlorobenzene analysis. Interferences from different soil matrices with different characteristics were investigated, and the amount extracted was strongly influenced by the matrix. Therefore, a standard addition protocol was performed on the real soil samples. The linear ranges of detection for the chlorobenzenes tested covered three orders of magnitude, and correlation coefficients > 0.9976 and relative standard deviations (RSD) < 8% were observed. The detection limits were found at sub-ng/g of soil levels, which were about an order of magnitude lower than those given by the commercial poly(dimethylsiloxane) (PDMS) coating for most of the compounds. The recoveries ranged from 64 to 109.6% for each analyte in the real kaleyard soil matrix when different concentration levels were determined over the linear range, which confirmed the reliability and feasibility of the HS-SPME/GC-ECD approach using the fiber coated with diglycidyloxy-C[4]/OH-TSO for the ultratrace analysis of chlorobenzenes in complex matrices.