Search results for: deposition temperature

Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

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Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750 C analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry

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Authors: E. Chávez-Vargas, M. de la L. Olvera-Amador, A. Jimenez-Gonzalez, A. Maldonado

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Undoped and fluorine doped zinc oxide (ZnO) thin films were deposited on sodocalcic glass substrates by the ultrasonic chemical spray technique. As the main goal is the manufacturing of transparent electrodes, the effects of both the solution composition and the substrate temperature on both the electrical and optical properties of ZnO thin films were studied. As a matter of fact, the effect of fluorine concentration ([F]/[F+Zn] at. %), solvent composition (acetic acid, water, methanol ratios) and ageing time, regarding solution composition, were varied. In addition, the substrate temperature and the deposition time, regarding the chemical spray technique, were also varied. Structural studies confirm the deposition of polycrystalline, hexagonal, wurtzite type, ZnO. The results show that the increase of ([F]/[F+Zn] at. %) ratio in the solution, decreases the sheet resistance, RS, of the ZnO:F films, reaching a minimum, in the order of 1.6 Ωcm, at 60 at. %; further increase in the ([F]/[F+Zn]) ratio increases the RS of the films. The same trend occurs with the variation in substrate temperature, as a minimum RS of ZnO:F thin films was encountered when deposited at TS= 450 °C. ZnO:F thin films deposited with aged solution show a significant decrease in the RS in the order of 100 ΩS. The transmittance of the films was also favorable affected by the solvent ratio and, more significantly, by the ageing of the solution. The whole evaluation of optical and electrical characteristics of the ZnO:F thin films deposited under different conditions, was done under Haacke’s figure of Merit in order to have a clear and quantitative trend as transparent conductors application.

Keywords: zinc oxide, ZnO:F, TCO, Haacke’s figure of Merit

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Authors: Nikki A. Barla, P. K. Ghosh, Sourav Das

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Two different groove sizes 13.6 mm (narrow groove) and 7.5 mm (ultra-narrow groove) of 304 LN austenitic stainless steel (ASS) plate was welded using pulse gas metal arc welding (P-GMAW). These grooves were welded using multi-pass single seam per layer (MSPPL) deposition technique with full assurance of groove wall fusion. During bead on plate deposition process, the thermal cycle was recorded using strain buster (temperature measuring device). Both the groove has heat affected Zone (HAZ) width of 1-2 mm. After welding, the microstructure studies was done which revealed that there was higher sensitization (Chromium carbide formation in grain boundary) in the HAZ of 13.6 mm groove weldment as compared to the HAZ of 7.5 mm weldment. Electrochemical potentiokinetic reactivation test (EPR) was done in 0.5 N H₂SO₄ + 1 M KSCN solution to study the degree of sensitization (DOS) and it was observed that 7.5 mm groove HAZ has lower DOS. Mass deposition in the 13.6 mm weld is higher than 7.5mm groove weld, which naturally induces higher residual stress in 13.6 mm weld. Comparison between microstructural studies and corrosion test summarized that the residual stress affects the sensitization property of welded ASS.

Keywords: austenitic stainless steel (ASS), electrochemical potentiokinetic reactivation test (EPR), microstructure, pulse gas metal arc welding (P-GMAW), sensitization

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Authors: A. Mavrikos, N. Petsas, E. Kaltsi, D. Kaliampakos

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The lignite-fired power plants in the Western Macedonia Lignite Center produce more than 8 106 t of fly ash per year. Approximately 90% of this quantity is used for restoration-reclamation of exhausted open-cast lignite mines and slope stabilization of the overburden. The purpose of this work is to evaluate the environmental behavior of the mixture of waste rock and fly ash that is being used in the external deposition site of the South Field lignite mine. For this reason, a borehole was made within the site and 86 samples were taken and subjected to chemical analyses and leaching tests. The results showed very limited leaching of trace elements and heavy metals from this mixture. Moreover, when compared to the limit values set for waste acceptable in inert waste landfills, only few excesses were observed, indicating only minor risk for groundwater pollution. However, due to the complexity of both the leaching process and the contaminant pathway, more boreholes and analyses should be made in nearby locations and a systematic groundwater monitoring program should be implemented both downstream and within the external deposition site.

Keywords: co-deposition, fly ash, leaching tests, lignite, waste rock

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Authors: Matthew Ferguson, Tatyana Konkova, Ioannis Violatos

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Microstructure analysis of additively manufactured (AM) materials is an important step in understanding the interrelationship between mechanical properties and materials performance. Literature on the effect of laser-based AM process parameters on the microstructure in the substrate-deposit interface is limited. The interface region, the adjoining area of substrate and deposit, is characterized by the presence of the fusion zone (FZ) and heat-affected zone (HAZ), experiencing rapid thermal gyrations resulting in thermal-induced transformations. Inconel 718 was utilized as work material for both the substrate and deposit. Three blocks of Inconel 718 material were deposited by Direct Energy Deposition (DED) using three different laser powers, 550W, 750W and 950W, respectively. A coupled thermo-mechanical transient approach was utilized to correlate temperature history to the evolution of microstructure. The thermal history of the deposition process was monitored with the thermocouples installed inside the substrate material. The interface region of the blocks was analyzed with Optical Microscopy (OM) and Scanning Electron Microscopy (SEM), including the electron back-scattered diffraction (EBSD) technique. Laser power was found to influence the dissolution of intermetallic precipitated phases in the substrate and grain growth in the interface region. Microstructure and thermal history data were utilized to draw conclusive comparisons between the investigated process parameters.

Keywords: additive manufacturing, direct energy deposition, electron back-scattered diffraction, finite element analysis, inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region

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Authors: Camilla G. Goncalves, Benedito Christ, Walter Miyakawa, Antonio J. Abdalla

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This work aims to investigate the properties and microstructure of diamond-like carbon film deposited by pulsed laser deposition by ablation of a graphite target in a vacuum chamber on a steel substrate. The equipment was mounted to provide one laser beam. The target of high purity graphite and the steel substrate were polished. The mechanical and tribological properties of the film were characterized using Raman spectroscopy, nanoindentation test, scratch test, roughness profile, tribometer, optical microscopy and SEM images. It was concluded that the pulsed laser deposition (PLD) technique associated with the low-pressure chamber and a graphite target provides a good fraction of sp3 bonding, that the process variable as surface polishing and laser parameter have great influence in tribological properties and in adherence tests performance. The optical microscopy images are efficient to identify the metallurgical bond.

Keywords: characterization, DLC, mechanical properties, pulsed laser deposition

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Authors: Anubhav Kumar Dwivedi, Arshad Khan, S. N. Tripathi, Manish Joshi, Gaurav Mishra, Dinesh Nath, Naveen Tiwari, B. K. Sapra

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In a nuclear reactor accident scenario, a large number of fission products may release to the piping system of the primary heat transport. The released fission products, mostly in the form of the aerosol, get deposited on the inner surface of the piping system mainly due to gravitational settling and thermophoretic deposition. The removal processes in the complex piping system are controlled to a large extent by the thermal-hydraulic conditions like temperature, pressure, and flow rates. These parameters generally vary with time and therefore must be carefully monitored to predict the aerosol behavior in the piping system. The removal process of aerosol depends on the size of particles that determines how many particles get deposit or travel across the bends and reach to the other end of the piping system. The released aerosol gets deposited onto the inner surface of the piping system by various mechanisms like gravitational settling, Brownian diffusion, thermophoretic deposition, and by other deposition mechanisms. To quantify the correct estimate of deposition, the identification and understanding of the aforementioned deposition mechanisms are of great importance. These mechanisms are significantly affected by different flow and thermodynamic conditions. Thermophoresis also plays a significant role in particle deposition. In the present study, a series of experiments were performed in the piping system of the National Aerosol Test Facility (NATF), BARC using metal aerosols (zinc) in dry environments to study the spatial distribution of particles mass and number concentration, and their depletion due to various removal mechanisms in the piping system. The experiments were performed at two different carrier gas flow rates. The commercial CFD software FLUENT is used to determine the distribution of temperature, velocity, pressure, and turbulence quantities in the piping system. In addition to the in-built models for turbulence, heat transfer and flow in the commercial CFD code (FLUENT), a new sub-model PBM (population balance model) is used to describe the coagulation process and to compute the number concentration along with the size distribution at different sections of the piping. In the sub-model coagulation kernels are incorporated through user-defined function (UDF). The experimental results are compared with the CFD modeled results. It is found that most of the Zn particles (more than 35 %) deposit near the inlet of the plenum chamber and a low deposition is obtained in piping sections. The MMAD decreases along the length of the test assembly, which shows that large particles get deposited or removed in the course of flow, and only fine particles travel to the end of the piping system. The effect of a bend is also observed, and it is found that the relative loss in mass concentration at bends is more in case of a high flow rate. The simulation results show that the thermophoresis and depositional effects are more dominating for the small and larger sizes as compared to the intermediate particles size. Both SEM and XRD analysis of the collected samples show the samples are highly agglomerated non-spherical and composed mainly of ZnO. The coupled model framed in this work could be used as an important tool for predicting size distribution and concentration of some other aerosol released during a reactor accident scenario.

Keywords: aerosol, CFD, deposition, coagulation

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Authors: Ana Paula Mousinho, Ronaldo D. Mansano, Nelson Ordonez

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Carbon nanotubes are one of the main elements in nanotechnologies; their applications are in microelectronics, nano-electronics devices (photonics, spintronic), chemical sensors, structural material and currently in clean energy devices (supercapacitors and fuel cells). The use of magnetic particle decorated carbon nanotubes increases the applications in magnetic devices, magnetic memory, and magnetic oriented drug delivery. In this work, single-walled carbon nanotubes (CNTs) forest decorated with chromium were deposited at room temperature by high-density plasma chemical vapor deposition (HDPCVD) system. The CNTs forest was obtained using pure methane plasmas and chromium, as precursor material (seed) and for decorating the CNTs. Magnetron sputtering deposited the chromium on silicon wafers before the CNTs' growth. Scanning electron microscopy, atomic force microscopy, micro-Raman spectroscopy, and X-ray diffraction characterized the single-walled CNTs forest decorated with chromium. In general, the CNTs' spectra show a unique emission band, but due to the presence of the chromium, the spectra obtained in this work showed many bands that are related to the CNTs with different diameters. The CNTs obtained by the HDPCVD system are highly aligned and showed metallic features, and they can be used as photonic material, due to the unique structural and electrical properties. The results of this work proved the possibility of obtaining the controlled deposition of aligned single-walled CNTs forest films decorated with chromium by high-density plasma chemical vapor deposition system.

Keywords: CNTs forest, high density plasma deposition, high-aligned CNTs, nanomaterials

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Authors: Somnath Mahato, Minarul Islam Sarkar, Luis Guillermo Gerling, Joaquim Puigdollers, Asit Kumar Kar

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Nanostructured Zinc Oxide (ZnO) thin films have been successfully deposited on indium tin oxide (ITO) coated glass substrates by a simple two electrode electrodeposition process at constant potential. The preparative parameters such as deposition time, deposition potential, concentration of solution, bath temperature and pH value of electrolyte have been optimized for deposition of uniform ZnO thin films. X-ray diffraction studies reveal that the prepared ZnO thin films have a high preferential oriented c-axis orientation with compact hexagonal (wurtzite) structure. Surface morphological studies show that the ZnO films are smooth, continuous, uniform without cracks or holes and compact with nanorod-like structure on the top of the surface. Optical properties reveal that films exhibit higher absorbance in the violet region of the optical spectrum; it gradually decreased in the visible range with increases in wavelength and became least at the beginning of NIR region. The photoluminescence spectra shows that the observed peaks are attributed to the various structural defects in the nanostructured ZnO crystal. The microstructural and optical properties suggest that the electrodeposited ZnO thin films are suitable for application in photosensitive devices such as photovoltaic solar cells photoelectrochemical cells and light emitting diodes etc.

Keywords: electrodeposition, microstructure, optical properties, ZnO thin films

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Authors: M. Khalid Alamgir, Javed Ahsan Bhatti, M. Zafarullah Khan

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Thin film of amorphous carbon (DLC) was deposited on 316 steel using Nd: YAG laser having energy 300mJ. Pure graphite was used as a target. The vacuum in the deposition chamber was generated in the range of 10-6 mbar by turbo molecular pump. Ratio of sp3 to sp2 content shows amorphous nature of the film. This was confirmed by Raman spectra having two peaks around 1300 cm-1 i.e. D-band to 1700 cm-1 i.e. G-band. If sp3 bonding ratio is high, the films behave like diamond-like whereas, with high sp2, films are graphite-like. The ratio of sp3 and sp2 contents in the film depends upon the deposition method, hydrogen contents and system parameters. The structural study of the film was carried out by XRD. The hardness of the films as measured by Vickers hardness tester and was found to be 28 GPa. The EDX result shows the presence of carbon contents on the surface in high rate and optical microscopy result shows the smoothness of the film on substrate. The film possesses good adhesion and can be used to coat surgical instruments.

Keywords: DLC, thin film, Raman spectroscopy, XRD, EDX

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Authors: A. Ozel

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The ductile to brittle transition temperature is a very important criterion that is used for selection of materials in some applications, especially in low-temperature conditions. For that reason, in this study transition temperature of as-cast and austempered unalloyed ductile iron in the temperature interval from -60 to +100 degrees C have been investigated. The microstructures of samples were examined by light microscope. The impact energy values obtained from the experiments were found to depend on the austempering time and temperature.

Keywords: Austempered Ductile Iron (ADI), Charpy test, microstructure, transition temperature

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Authors: Manjit Singha, Sandeep Singh Sandhu, A. S. Shahi

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Stellite 6 is cobalt based superalloy used for protective coatings. It is used to improve the wear performance of stainless steel engineering components subjected to harsh environmental conditions. This paper reports the high temperature wear analysis of satellite 6 cladded on AISI 304 L substrate using SMAW process. Bead on plate experiment was carried out by varying current and electrode manipulation techniques to optimize the dilution and hardness. 80 Amp current and weaving technique was found to be the optimum set of parameters for overlaying which were further used for multipass multilayer cladding on two plates of AISI 304 L substrate. On the first plate, seven layers seven passes of stellite 6 was overlaid which was used in as cladded form and the second plate was overlaid with five layers five passes of satellite 6 with further TIG remelting. The wear performance was examined for normal temperature environmental condition and harsh temperature environmental condition. The satellite 6 coating with TIG remelting was found to be better in both the conditions even with lesser metal deposition due to its finer grain structure.

Keywords: surfacing, stellite 6, dilution, overlay, SMAW, high-temperature frictional wear, micro-structure, micro-hardness

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Authors: Yusuf S. Dambatta, Ahmed A. D. Sarhan

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Fused deposition modelling (FDM) is one of the most prominent rapid prototyping (RP) technologies which is being used to efficiently fabricate CAD 3D geometric models. However, the process is coupled with many drawbacks, of which the surface quality of the manufactured RP parts is among. Hence, studies relating to improving the surface roughness have been a key issue in the field of RP research. In this work, a technique of modelling the surface roughness in FDM is presented. Using experimentally measured surface roughness response of the FDM parts, an ANFIS prediction model was developed to obtain the surface roughness in the FDM parts using the main critical process parameters that affects the surface quality. The ANFIS model was validated and compared with experimental test results.

Keywords: surface roughness, fused deposition modelling (FDM), adaptive neuro fuzzy inference system (ANFIS), orientation

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Authors: Abdelrahman Zkria, Tsuyoshi Yoshitake

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Diamond is one of the most interesting semiconducting carbon materials owing to its unique physical and chemical properties, yet its application in electronic devices is limited due to the difficulty of realizing n-type conduction by nitrogen doping. In contrast Ultrananocrystalline diamond with diamond grains of about 3–5 nm in diameter have attracted much attention for device-oriented applications because they may enable the realization of n-type doping with nitrogen. In this study, nitrogen-doped Ultra-Nanocrystalline diamond films were prepared by coaxial arc plasma deposition (CAPD) method, the nitrogen content was estimated by X-ray photoemission spectroscopy (XPS). The electrical conductivity increased with increasing nitrogen contents. Heterojunction diodes with p-type Si were fabricated and evaluated based on current–voltage (I–V) and capacitance–voltage (C–V) characteristics measured in dark at room temperature.

Keywords: heterojunction diodes, hopping conduction mechanism, nitrogen-doping, ultra-nanocrystalline diamond

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Authors: Zydrunas Kavaliauskas, Aleksandras Iljinas, Liutauras Marcinauskas, Mindaugas Milieska, Vitas Valincius

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The magnetron sputtering deposition method is often used to obtain thin film coatings. The main advantage of magnetron vaporization compared to other deposition methods is the high rate erosion of the cathode material (e.g., copper, aluminum, etc.) and the ability to operate under low-pressure conditions. The structure of the formed coatings depends on the working parameters of the magnetron deposition system, which is why it is possible to influence the properties of the growing film, such as morphology, crystal orientation, and dimensions, stresses, adhesion, etc. The properties of these coatings depend on the distance between the substrate and the magnetron surface, the vacuum depth, the gas used, etc. Using this deposition technology, substrates are most often placed near the anode. The magnetic trap of the magnetrons for localization of electrons in the cathode region is formed using a permanent magnet system that is on the side of the cathode. The scientific literature suggests that, after insertion of a small amount of copper into graphite, the electronic conductivity of graphite increase. The aim of this work is to create thin (up to 300 nm) layers on a graphite surface using a magnetron evaporation method, to investigate the formation peculiarities and microstructure of thin films, as well as the mechanism of copper diffusion into graphite inner layers at different thermal treatment temperatures. The electron scanning microscope was used to investigate the microrelief of the coating surface. The chemical composition is determined using the EDS method, which shows that, with an increase of the thermal treatment of the copper-carbon layer from 200 °C to 400 °C, the copper content is reduced from 8 to 4 % in atomic mass units. This is because the EDS method captures only the amount of copper on the graphite surface, while the temperature of the heat treatment increases part of the copper because of the diffusion processes penetrates into the inner layers of the graphite. The XRD method shows that the crystalline copper structure is not affected by thermal treatment.

Keywords: carbon, coatings, copper, magnetron sputtering

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Authors: Chil-Chyuan Kuo, Chen-Hsuan Tsai

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This study presents a cost-effective approach for rapid fabricating modeling platforms utilized in fused deposition modeling system. A small-batch production of modeling platforms about 20 pieces can be obtained economically through silicone rubber mold using vacuum casting without applying the plastic injection molding. The air venting systems is crucial for fabricating modeling platform using vacuum casting. Modeling platforms fabricated can be used for building rapid prototyping model after sandblasting. This study offers industrial value because it has both time-effectiveness and cost-effectiveness.

Keywords: vacuum casting, fused deposition modeling, modeling platform, sandblasting, surface roughness

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Authors: Prajna Paramita Mohapatra, Pamu Dobbidi

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Lithium ferrite (LiFe5O8) has potential applications as a component of microwave magnetic devices such as circulators and monolithic integrated circuits. For efficient device applications, spinel ferrites in the form of thin films are highly required. It is necessary to improve their magnetic and dielectric behavior by optimizing the processing parameters during deposition. The lithium ferrite thin films are deposited on Pt/Si substrate using the pulsed laser deposition technique (PLD). As controlling the film thickness is the easiest parameter to tailor the strain, we deposited the thin films having different film thicknesses (160 nm, 200 nm, 240 nm) at oxygen partial pressure of 0.001 mbar. The formation of single phase with spinel structure (space group - P4132) is confirmed by the XRD pattern and the Rietveld analysis. The optical bandgap is decreased with the increase in thickness. FESEM confirmed the formation of uniform grains having well separated grain boundaries. Further, the film growth and the roughness are analyzed by AFM. The root-mean-square (RMS) surface roughness is decreased from 13.52 nm (160 nm) to 9.34 nm (240 nm). The room temperature magnetization is measured with a maximum field of 10 kOe. The saturation magnetization is enhanced monotonically with an increase in thickness. The magnetic resonance linewidth is obtained in the range of 450 – 780 Oe. The dielectric response is measured in the frequency range of 104 – 106 Hz and in the temperature range of 303 – 473 K. With an increase in frequency, the dielectric constant and the loss tangent of all the samples decreased continuously, which is a typical behavior of conventional dielectric material. The real part of the dielectric constant and the dielectric loss is increased with an increase in thickness. The contribution of grain and grain boundaries is also analyzed by employing the equivalent circuit model. The highest dielectric constant is obtained for the film having a thickness of 240 nm at 104 Hz. The obtained results demonstrate that desired response can be obtained by tailoring the film thickness for the microwave magnetic devices.

Keywords: PLD, optical response, thin films, magnetic response, dielectric response

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Authors: Edison A. Bonifaz

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In this work, a numerical procedure is proposed to design dense multi-material structures using the Directed Energy Deposition (DED) process. A thermo-mechanical finite element model to predict thermal cycles and residual stresses is presented. A numerical layer build-up procedure coupled with a moving heat flux was constructed to minimize strains and residual stresses that result in the multi-layer deposition of an AISI 316 austenitic steel on an AISI 304 austenitic steel substrate. To simulate the DED process, the automated interface of the ABAQUS AM module was used to define element activation and heat input event data as a function of time and position. Of this manner, the construction of ABAQUS user-defined subroutines was not necessary. Thermal cycles and thermally induced stresses created during the multi-layer deposition metal AM pool crystallization were predicted and validated. Results were analyzed in three independent metal layers of three different experiments. The one-way heat and material deposition toolpath used in the analysis was created with a MatLab path script. An optimal combination of feedstock and heat input printing parameters suitable for fabricating multi-material dense structures in the directed energy deposition metal AM process was established. At constant power, it can be concluded that the lower the heat input, the lower the peak temperatures and residual stresses. It means that from a design point of view, the one-way heat and material deposition processing toolpath with the higher welding speed should be selected.

Keywords: event series, thermal cycles, residual stresses, multi-pass welding, abaqus am modeler

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Authors: Nouf Alharbi

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The electrospray deposition technique became an important method that enables fragile, nonvolatile molecules to be deposited in situ in high vacuum environments. Furthermore, it is considered one of the ways to close the gap between basic surface science and molecular engineering, which represents a gradual change in the range of scientist research. Also, this paper talked about one of the most important techniques that have been developed and aimed for helping to further develop and characterize the electrospray by providing data collected using an image charge detection instrument. Image charge detection mass spectrometry (CDMS) is used to measure speed and charge distributions of the molecular ions. As well as, some data has been included using SIMION simulation to simulate the energies and masses of the molecular ions through the system in order to refine the mass-selection process.

Keywords: charge, deposition, electrospray, image, ions, molecules, SIMION

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Authors: Asmat Nawaz, Ali Koray Erdinc, Burak Gultekin, Muhammad Tayyib, Ceylan Zafer, Kaiying Wang, M. Nadeem Akram

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In this study, a sequential deposition process is used for the fabrication of PEDOT: PSS based inverted planar perovskite solar cell. A small amount of additive deionized water (DI-H₂O) was added into PbI₂ + Dimethyl formamide (DMF) precursor solution in order to increase the solubility of PbI₂ in DMF, and finally to manipulate the surface morphology of the perovskite films. A morphology transition from needle like structure to hexagonal plates, and then needle-like again has been observed as the DI-H2O was added continuously (0.0 wt% to 3.0wt%). The latter one leads to full surface coverage of the perovskite, which is essential for high performance solar cell.

Keywords: charge carrier diffusion lengths, Methylamonium lead iodide, precursor composition, perovskite solar cell, sequential deposition

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Authors: Najmul Hasan, Shiping Li, Chunli Liu

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The synergy effect of surface modifications using the acid treatment and noble metal (Au) deposition on the efficiency of SnFe2O4 (SFO) nano-octahedron photocatalyst has been investigated. Inorganic acids (H2SO4 and HNO3) were employed to compare the effects of different acids. It has been found that after corrosion treatment using H2SO4 and deposition of Au nanoparticles, SnFe2O4 nano-octahedron (Au-S-SFO) showed significantly enhanced photocatalytic activity under simulated light irradiation. Au-S-SFO was characterized by XRD, XPS, EDS, FTIR, Uv-vis-DRS, SEM, PL, and EIS analysis. The mechanism for CO2 reduction was investigated by scavenger tests. The stability of Au-S-SFO was confirmed by continuously repeated tests followed by XRD analysis. The surface corrosion treatment of SFO octahedron with H2SO4 could produce hydroxyl group (-OH) and sulfonic acid group (-SO3H) as reaction sites. These active sites not only enhanced the Au nanoparticles deposition to the acid treated SFO surface but also acted as the Brønsted acid sites that enhance the water adsorption and provide protons for CTC degradation and CO2 reduction. These effects improved the carrier separation and transfer efficiency. In addition, the photocatalytic efficiency was further enhanced by the surface plasmon resonance (SPR) effect of Au nanoparticles deposited on the surface of acid-treated SFO. As a result of the synergy of both acid treatment and SPR effect from the Au NPs, Au-S-SFO exhibited the highest CO2 reduction activity with 2.81, 1.92, and 2.69 times higher evolution rates for CO, CH4, and H2, respectively than that of pure SFO.

Keywords: surface modification, CO2 reduction, Au deposition, Gas-liquid interfacial plasma

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Authors: Renu Kumari, Jyotsna Dutta Majumdar

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In the present study, composite coating consisting of hydroxyapatite (HA) + 50 wt% TiO2 has been developed on Ti-6Al-4V substrate by plasma spray deposition technique. Followed by plasma spray deposition, detailed surface roughness and microstructural characterization were carried out by using optical profilometer and scanning electron microscopy (SEM), respectively. The composition and phase analysis were carried out by energy-dispersive X-ray spectroscopy analysis, and X-ray diffraction (XRD) technique, respectively. The bio-activity behavior of the uncoated and coated samples was also compared by dipping test in Hank’s solution. The average surface roughness of the coating was 10 µm (as compared to 0.5 µm of as-received Ti-6Al-4V substrate) with the presence of porosities. The microstructure of the coating was found to be continuous with the presence of solidified splats. A detailed XRD analysis shows phase transformation of TiO2 from anatase to rutile, decomposition of hydroxyapatite, and formation of CaTiO3 phase. Standard dipping test confirmed a faster kinetics of deposition of calcium phosphate in the coated HA+50% wt.% TiO2 surface as compared to the as-received substrate.

Keywords: titanium, plasma spraying, microstructure, bio-activity, TiO2, hydroxyapatite

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Authors: Hsyi-En Cheng, Ying-Yi Liou

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Metal-oxide semiconductor (MOS) gas sensors are widely used in the gas-detection market due to their high sensitivity, fast response, and simple device structures. However, the high working temperature of MOS gas sensors makes them difficult to integrate with the appliance or consumer goods. One-dimensional (1-D) nanostructures are considered to have the potential to lower their working temperature due to their large surface-to-volume ratio, confined electrical conduction channels, and small feature sizes. Unfortunately, the difficulty of fabricating 1-D nanostructure electrodes has hindered the development of low-temperature MOS gas sensors. In this work, we proposed a method to fabricate nanotube-arrays, and the SnO₂ nanotube-array sensors with different wall thickness were successfully prepared and examined. The fabrication of SnO₂ nanotube arrays incorporates the techniques of barrier-free anodic aluminum oxide (AAO) template and atomic layer deposition (ALD) of SnO₂. First, 1.0 µm Al film was deposited on ITO glass substrate by electron beam evaporation and then anodically oxidized by five wt% phosphoric acid solution at 5°C under a constant voltage of 100 V to form porous aluminum oxide. As the Al film was fully oxidized, a 15 min over anodization and a 30 min post chemical dissolution were used to remove the barrier oxide at the bottom end of pores to generate a barrier-free AAO template. The ALD using reactants of TiCl4 and H₂O was followed to grow a thin layer of SnO₂ on the template to form SnO₂ nanotube arrays. After removing the surface layer of SnO₂ by H₂ plasma and dissolving the template by 5 wt% phosphoric acid solution at 50°C, upright standing SnO₂ nanotube arrays on ITO glass were produced. Finally, Ag top electrode with line width of 5 μm was printed on the nanotube arrays to form SnO₂ nanotube-array sensor. Two SnO₂ nanotube-arrays with wall thickness of 30 and 60 nm were produced in this experiment for the evaluation of gas sensing ability. The flat SnO₂ films with thickness of 30 and 60 nm were also examined for comparison. The results show that the properties of ALD SnO₂ films were related to the deposition temperature. The films grown at 350°C had a low electrical resistivity of 3.6×10-3 Ω-cm and were, therefore, used for the nanotube-array sensors. The carrier concentration and mobility of the SnO₂ films were characterized by Ecopia HMS-3000 Hall-effect measurement system and were 1.1×1020 cm-3 and 16 cm3/V-s, respectively. The electrical resistance of SnO₂ film and nanotube-array sensors in air and in a 5% H₂-95% N₂ mixture gas was monitored by Pico text M3510A 6 1/2 Digits Multimeter. It was found that, at 200 °C, the 30-nm-wall SnO₂ nanotube-array sensor performs the highest responsivity to 5% H₂, followed by the 30-nm SnO₂ film sensor, the 60-nm SnO₂ film sensor, and the 60-nm-wall SnO₂ nanotube-array sensor. However, at temperatures below 100°C, all the samples were insensitive to the 5% H₂ gas. Further investigation on the sensors with thinner SnO₂ is necessary for improving the sensing ability at temperatures below 100 °C.

Keywords: atomic layer deposition, nanotube arrays, gas sensor, tin dioxide

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Authors: Maria Pintea, Nigel Mason

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Induced chemistry is one of the newest pathways in the nanotechnology field with applications in the focused electron beam induced processes for deposition of nm scale structures. Si(OPr)₄ and Ti(OEt)₄ are two of the precursors that have not been so extensively researched, though highly sought for semiconductor and medical applications fields, the two compounds make good candidates for FEBIP and are the subject of velocity slice map imaging analysis for deposition purposes, offering information on kinetic energies, fragmentation channels, and angular distributions. The velocity slice map imaging technique is a method used for the characterization of molecular dynamics of the molecule and the fragmentation channels as a result of induced chemistry. To support the gas-phase analysis, Meso-Bio-Nano simulations of irradiation dynamics studies are employed with final results on Fe(CO)₅ deposited on various substrates. The software is capable of running large scale simulations for complex biomolecular, nano- and mesoscopic systems with applications to thermos-mechanical DNA damage, complex materials, gases, nanoparticles for cancer research and deposition applications for nanotechnology, using a large library of classical potentials, many-body force fields, molecular force fields involved in the classical molecular dynamics.

Keywords: focused electron beam induced deposition, FEBID, induced chemistry, molecular dynamics, velocity map slice imaging

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Authors: Pouyan Motamedi, Ken Bosnick, Ken Cadien, James Hogan

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Growth of conformal ultrathin metal films has attracted a considerable amount of attention recently. Plasma-enhanced atomic layer deposition (PEALD) is a method capable of growing conformal thin films at low temperatures, with an exemplary control over thickness. The authors have recently reported on growth of metastable epitaxial nickel thin films via PEALD, along with a comprehensive characterization of the films and a study on the relationship between the growth parameters and the film characteristics. The goal of the current study is to use the mentioned films as a case study to investigate the temperature-activated phase transformation and agglomeration in ultrathin metallic films. For this purpose, metastable hexagonal nickel thin films were annealed using a controlled heating/cooling apparatus. The transformations in the crystal structure were observed via in-situ synchrotron x-ray diffraction. The samples were annealed to various temperatures in the range of 400-1100° C. The onset and progression of particle formation were studied in-situ via laser measurements. In addition, a four-point probe measurement tool was used to record the changes in the resistivity of the films, which is affected by phase transformation, as well as roughening and agglomeration. Thin films annealed at various temperature steps were then studied via atomic force microscopy, scanning electron microscopy and high-resolution transmission electron microscopy, in order to get a better understanding of the correlated mechanisms, through which phase transformation and particle formation occur. The results indicate that the onset of hcp-to-bcc transformation is at 400°C, while particle formations commences at 590° C. If the annealed films are quenched after transformation, but prior to agglomeration, they show a noticeable drop in resistivity. This can be attributed to the fact that the hcp films are grown epitaxially, and are under severe tensile strain, and annealing leads to relaxation of the mismatch strain. In general, the results shed light on the nature of structural transformation in nickel thin films, as well as metallic thin films, in general.

Keywords: atomic layer deposition, metastable, nickel, phase transformation, thin film

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Authors: Hatem Diaf, Patrice Melinon, Antonio Pereira, Bernard Moine, Nicholas Blanchard, Florent Bourquard, Florence Garrelie, Christophe Donnet

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Glassy carbon exhibits excellent biological compatibility with live tissues meaning it has high potential for applications in life science. Moreover, glassy carbon has interesting properties including 'high temperature resistance', hardness, low density, low electrical resistance, low friction, and low thermal resistance. The structure of glassy carbon has long been a subject of debate. It is now admitted that glassy carbon is 100% sp2. This term is a little bit confusing as long sp2 hybridization defined from quantum chemistry is related to both properties: threefold configuration and pi bonding (parallel pz orbitals). Using plasma laser deposition of carbon clusters combined with pulsed nano/femto laser annealing, we are able to synthesize thin films of glassy carbon of good quality (probed by G band/ D disorder band ratio in Raman spectroscopy) without thermal post annealing. A careful inspecting of Raman signal, plasmon losses and structure performed by HRTEM (High Resolution Transmission Electron Microscopy) reveals that both properties (threefold and pi orbitals) cannot coexist together. The structure of the films is compared to models including schwarzites based from negatively curved surfaces at the opposite of onions or fullerene-like structures with positively curved surfaces. This study shows that a huge collection of porous carbon named vitreous carbon with different structures can coexist.

Keywords: glassy carbon, cluster deposition, coating, electronic structure

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Authors: Rukshana Pervin

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We report a detailed study on the transport properties of a 40 nm thick granular aluminum film. As measured by temperature-dependent resistance R(T), a resistance peak is observed before the transition to superconductivity, which indicates that the diffusion channel is subjected to weak localization and electron-electron interaction, and the superconductor channel is subjected to SC fluctuations (SCFs). The zero-magnetic field transport measurement demonstrated that Electron-Electron Interaction (EEI), weak localization, and SCFs are closely related in this granular aluminum film. The characteristic temperature at which SCFs emerge on the sample is determined by measuring the R(T) during cooling. The SCF of the film is studied in terms of the direct contribution of the Aslamazov-Larkin's fluctuation Cooper pair density and the indirect contribution of the Maki-Thomson's quasiparticle pair density. In this sample, the rise in R(T) above the SCF characteristic temperature indicates the WL and/or EEI. Comparative analyses are conducted on how the EEI and WL contribute to the upturn in R(T).

Keywords: fluctuation superconductivity, weak localization, thermal deposition, electron-electron interaction

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Authors: Asmat Nawaz, Ceylan Zafer, Ali K. Erdinc, Kaiying Wang, M. Nadeem Akram

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Hybrid halide Perovskites with the general formula ABX₃, where X = Cl, Br or I, are considered as an ideal candidates for the preparation of photovoltaic devices. The most commonly and successfully used hybrid halide perovskite for photovoltaic applications is CH₃NH₃PbI₃ and its analogue prepared from lead chloride, commonly symbolized as CH₃NH₃PbI₃_ₓClₓ. Some researcher groups are using lead free (Sn replaces Pb) and mixed halide perovskites for the fabrication of the devices. Both mesoporous and planar structures have been developed. By Comparing mesoporous structure in which the perovskite materials infiltrate into mesoporous metal oxide scaffold, the planar architecture is much simpler and easy for device fabrication. In a typical perovskite solar cell, a perovskite absorber layer is sandwiched between the hole and electron transport. Upon the irradiation, carriers are created in the absorber layer that can travel through hole and electron transport layers and the interface in between. We fabricated inverted planar heterojunction structure ITO/PEDOT/ Perovskite/PCBM/Al, based solar cell via two-step spin coating method. This is also called Sequential deposition method. A small amount of cheap additive H₂O was added into PbI₂/DMF to make a homogeneous solution. We prepared four different solution such as (W/O H₂O, 1% H₂O, 2% H₂O, 3% H₂O). After preparing, the whole night stirring at 60℃ is essential for the homogenous precursor solutions. We observed that the solution with 1% H₂O was much more homogenous at room temperature as compared to others. The solution with 3% H₂O was precipitated at once at room temperature. The four different films of PbI₂ were formed on PEDOT substrates by spin coating and after that immediately (before drying the PbI₂) the substrates were immersed in the methyl ammonium iodide solution (prepared in isopropanol) for the completion of the desired perovskite film. After getting desired films, rinse the substrates with isopropanol to remove the excess amount of methyl ammonium iodide and finally dried it on hot plate only for 1-2 minutes. In this study, we added H₂O in the PbI₂/DMF precursor solution. The concept of additive is widely used in the bulk- heterojunction solar cells to manipulate the surface morphology, leading to the enhancement of the photovoltaic performance. There are two most important parameters for the selection of additives. (a) Higher boiling point w.r.t host material (b) good interaction with the precursor materials. We observed that the morphology of the films was improved and we achieved a denser, uniform with less cavities and almost full surface coverage films but only using precursor solution having 1% H₂O. Therefore, we fabricated the complete perovskite solar cell by sequential deposition technique with precursor solution having 1% H₂O. We concluded that with the addition of additives in the precursor solutions one can easily be manipulate the morphology of the perovskite film. In the sequential deposition method, thickness of perovskite film is in µm and the charge diffusion length of PbI₂ is in nm. Therefore, by controlling the thickness using other deposition methods for the fabrication of solar cells, we can achieve the better efficiency.

Keywords: methylammonium lead iodide, perovskite solar cell, precursor composition, sequential deposition

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Authors: Nazanin Sheibanian, Raffaella Sesana, Sedat Ozbilen

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In recent years, high-entropy alloys (HEAs) have attracted considerable attention due to their unique properties and potential applications. In this study, novel HEA coatings were prepared on Mg substrates using mechanically alloyed HEA powder feedstocks based on Al_(0.1-0.5)CoCrCuFeNi and MnCoCrCuFeNi multi-material systems. The coatings were deposited by the Cold Spray (CS) process using three different temperatures of the process gas (N2) (650°C, 750°C, and 850°C) to examine the effect of gas temperature on coating properties. In this study, Infrared Thermography (non-destructive) was examined as a possible quality control technique for HEA coatings applied to magnesium substrates. Active Thermography was employed to characterize coating properties using the thermal response of the coating. Various HEA chemical compositions and deposition temperatures have been investigated. As a part of this study, a comprehensive macro and microstructural analysis of Cold Spray (CS) HEA coatings has been conducted using macrophotography, optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM+EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microhardness tests, roughness measurements, and porosity assessments. These analyses provided insight into phase identification, microstructure characterization, deposition, particle deformation behavior, bonding mechanisms, and identifying a possible relationship between physical properties and thermal responses. Based on the figures and tables, it is evident that the Maximum Relative Radiance (∆RMax) of each sample differs depending on both the chemical composition of HEA and the temperature at which Cold Spray is applied.

Keywords: active thermography, coating, cold spray, high- entropy alloy, material characterization

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Authors: Antoine Lauvray, Fabien Poulhaon, Pierre Michaud, Pierre Joyot, Emmanuel Duc

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Additive Friction Stir Manufacturing (AFSM) is a new industrial process that follows the emergence of friction-based processes. The AFSM process is a solid-state additive process using the energy produced by the friction at the interface between a rotating non-consumable tool and a substrate. Friction depends on various parameters like axial force, rotation speed or friction coefficient. The feeder material is a metallic rod that flows through a hole in the tool. Unlike in Friction Stir Welding (FSW) where abundant literature exists and addresses many aspects going from process implementation to characterization and modeling, there are still few research works focusing on AFSM. Therefore, there is still a lack of understanding of the physical phenomena taking place during the process. This research work aims at a better AFSM process understanding and implementation, thanks to numerical simulation and experimental validation performed on a prototype effector. Such an approach is considered a promising way for studying the influence of the process parameters and to finally identify a process window that seems relevant. The deposition of material through the AFSM process takes place in several phases. In chronological order these phases are the docking phase, the dwell time phase, the deposition phase, and the removal phase. The present work focuses on the dwell time phase that enables the temperature rise of the system composed of the tool, the filler material, and the substrate and due to pure friction. Analytic modeling of heat generation based on friction considers as main parameters the rotational speed and the contact pressure. Another parameter considered influential is the friction coefficient assumed to be variable due to the self-lubrication of the system with the rise in temperature or the materials in contact roughness smoothing over time. This study proposes, through numerical modeling followed by experimental validation, to question the influence of the various input parameters on the dwell time phase. Rotation speed, temperature, spindle torque, and axial force are the main monitored parameters during experimentations and serve as reference data for the calibration of the numerical model. This research shows that the geometry of the tool as well as fluctuations of the input parameters like axial force and rotational speed are very influential on the temperature reached and/or the time required to reach the targeted temperature. The main outcome is the prediction of a process window which is a key result for a more efficient process implementation.

Keywords: numerical model, additive manufacturing, friction, process

Procedia PDF Downloads 114