Search results for: sputtering

Authors: Somayeh Azizi, Mohammad Hossein Ehsani, Amir Zareidoost

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In this research, a technique has been developed to reduce the corrosion rate of magnesium (Mg) metal by creating Zr-Nb thin film coatings. In this regard, thin-film coatings of niobium (Nb) zirconium (Zr) double alloy are applied on pure Mg specimens under different processes conditions, such as the change of the substrate temperature, substrate bias, and coating thickness using the magnetron sputtering method. Then, deposited coatings are analyzed in terms of surface features via field-emission scanning electron microscopy (FE-SEM), thin-layer X-ray diffraction (GI-XRD), energy-dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), and corrosion tests. Also, nano-scratch tests were carried out to investigate the adhesion of the thin film. The results showed that the (Zr-Nb) thin films could control the degradation rate of Mg in the simulated body fluid (SBF). The nano-scratch studies depicted that the (Zr-Nb) thin films have a proper adhesion with the Mg substrate. Therefore, this technique could be used to enhance the corrosion resistance of bare Mg and could result in improving the performance of the biodegradable Mg implant for orthopedic applications.

Keywords: (Zr-Nb) thin film, magnetron sputtering, biodegradable Mg, degradation rate

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Authors: Omar M. Elmabrouk

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The cutting tool, in the high-speed machining process, is consistently dealing with high localized stress at the tool tip, tip temperature exceeds 800°C and the chip slides along the rake face. These conditions are affecting the tool wear, the cutting tool performances, the quality of the produced parts and the tool life. Therefore, a thin film coating on the cutting tool should be considered to improve the tool surface properties while maintaining its bulks properties. One of the general coating processes in applying thin film for hard coating purpose is PVD magnetron sputtering. In this paper, the prediction of the effects of PVD magnetron sputtering coating process parameters, sputter power in the range of (4.81-7.19 kW), bias voltage in the range of (50.00-300.00 Volts) and substrate temperature in the range of (281.08-600.00 °C), were studied using artificial neural network (ANN). The results were compared with previously published results using RSM model. It was found that the ANN is more accurate in prediction of tool hardness, and hence, it will not only improve the tool life of the tool but also significantly enhances the efficiency of the machining processes.

Keywords: artificial neural network, hardness, prediction, titanium aluminium nitrate coating

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Authors: Ke-Jing Lee, Cheng-Jung Lee, Yu-Chi Chang, Li-Wen Wang, Yeong-Her Wang

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To avoid the cross-talk issue of only resistive random access memory (RRAM) cell, one transistor and one resistor (1T1R) architecture with a TiO₂-based RRAM cell connected with solution barium zirconate nickelate (BZN) organic thin film transistor (OTFT) device is successfully demonstrated. The OTFT were fabricated on a glass substrate. Aluminum (Al) as the gate electrode was deposited via a radio-frequency (RF) magnetron sputtering system. The barium acetate, zirconium n-propoxide, and nickel II acetylacetone were synthesized by using the sol-gel method. After the BZN solution was completely prepared using the sol-gel process, it was spin-coated onto the Al/glass substrate as the gate dielectric. The BZN layer was baked at 100 °C for 10 minutes under ambient air conditions. The pentacene thin film was thermally evaporated on the BZN layer at a deposition rate of 0.08 to 0.15 nm/s. Finally, gold (Au) electrode was deposited using an RF magnetron sputtering system and defined through shadow masks as both the source and drain. The channel length and width of the transistors were 150 and 1500 μm, respectively. As for the manufacture of 1T1R configuration, the RRAM device was fabricated directly on drain electrodes of TFT device. A simple metal/insulator/metal structure, which consisting of Al/TiO₂/Au structures, was fabricated. First, Au was deposited to be a bottom electrode of RRAM device by RF magnetron sputtering system. Then, the TiO₂ layer was deposited on Au electrode by sputtering. Finally, Al was deposited as the top electrode. The electrical performance of the BZN OTFT was studied, showing superior transfer characteristics with the low threshold voltage of −1.1 V, good saturation mobility of 5 cm²/V s, and low subthreshold swing of 400 mV/decade. The integration of the BZN OTFT and TiO₂ RRAM devices was finally completed to form 1T1R configuration with low power consumption of 1.3 μW, the low operation current of 0.5 μA, and reliable data retention. Based on the I-V characteristics, the different polarities of bipolar switching are found to be determined by the compliance current with the different distribution of the internal oxygen vacancies used in the RRAM and 1T1R devices. Also, this phenomenon can be well explained by the proposed mechanism model. It is promising to make the 1T1R possible for practical applications of low-power active matrix flat-panel displays.

Keywords: one transistor and one resistor (1T1R), organic thin-film transistor (OTFT), resistive random access memory (RRAM), sol-gel

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Authors: Issam Lakdhar, Akram Alhussein, Juan Creus

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With the huge increase in world energy consumption, researchers are working to find other alternative sources of energy instead of fossil fuel one causing many environmental problems as the production of greenhouse effect gases. Hydrogen is considered a green energy source, which its combustion does not cause environmental pollution. The transport and the storage of the gas molecules or the other products containing this smallest chemical element in metallic structures (pipelines, tanks) are crucial issues. The dissolve and the permeation of hydrogen into the metal lattice lead to the formation of hydride phases and the embrittlement of structures. To protect the metallic structures, a surface treatment could be a good solution. Among the different techniques, magnetron sputtering is used to elaborate micrometric coatings capable of slowing down or stop hydrogen permeation. In the plasma environment, the deposition parameters of new thin-film metallic glasses Al-Ti-W were optimized and controlled in order to obtain, hydrogen barrier. Many characterizations were carried out (SEM, XRD and Nano-indentation…) to control the composition and understand the influence of film microstructure and chemical composition on the hydrogen permeation through the coatings. The coating performance was evaluated under two hydrogen production methods: chemical and electrochemical (cathodic protection) techniques. The hydrogen quantity absorbed was experimentally determined using the Thermal-Desorption Spectroscopy method (TDS)). An ideal ATW thin film was developed and showed excellent behavior against the diffusion of hydrogen.

Keywords: thin films, hydrogen, PVD, plasma technology, electrochemical properties

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Authors: Ahmad I. Ayesh

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This work reports on the fabrication of tin nanoclusters by sputtering and inert-gas condensation inside an ultra-high vacuum compatible system. This technique allows to fine tune the size and yield of nanoclusters by controlling the nanocluster source parameters. The produced nanoclusters are deposited on SiO2/Si substrate with pre-formed electrical electrodes to produce a nanocluster device. Those devices can be potentially used for gas sensor applications.

Keywords: tin, nanoclusters, inert-gas condensation, nanotechnology

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Authors: Zue-Chin Chang

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RF magnetron sputtering is used on the ceramic targets, each of which contains zinc oxide (ZnO), zinc oxide doped with aluminum (AZO) and zinc oxide doped with gallium (GZO). The XRD analysis showed a preferred orientation along the (002) plane for ZnO, AZO, and GZO films. The AZO film had the best electrical properties; it had the lowest resistivity of 6.6 × 10-4 cm, the best sheet resistance of 2.2 × 10-1 Ω/square, and the highest carrier concentration of 4.3 × 1020 cm-3, as compared to the ZnO and GZO films.

Keywords: aging, films, microstructure, photoelectric property

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Authors: Henry Navarro, Martin Sirena, Nestor Haberkorn

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We report the electrical transport through voltage-current curves (I-V) in tunnels junction GdBa₂Cu₃O₇-d/ insulator/ GdBa₂Cu₃O₇-d, and Nb/insulator/ GdBa₂Cu₃O₇-d is analyzed using a conducting atomic force microscope (CAFM) at room temperature. The measurements were obtained on tunnel junctions with different areas (900 μm², 400 μm² and 100 μm²). Trilayers with GdBa₂Cu₃O₇-d (GBCO) as the bottom electrode, SrTiO₃ (STO) or BaTiO₃ (BTO) as the insulator barrier (thicknesses between 1.6 nm and 4 nm), and GBCO or Nb as the top electrode were grown by DC sputtering on (100) SrTiO₃ substrates. For STO and BTO barriers, asymmetric IV curves at positive and negative polarization can be obtained using electrodes with different work function. The main difference is that the BTO is a ferroelectric material, while in the STO the ferroelectricity can be produced by stress or deformation at the interfaces. In addition, hysteretic IV curves are obtained for BTO barriers, which can be ascribed to a combined effect of the FE reversal switching polarization and an oxygen vacancy migration. For GBCO/ BTO/ GBCO heterostructures, the IV curves correspond to that expected for asymmetric interfaces, which indicates that the disorder affects differently the properties at the bottom and top interfaces. Our results show the role of the interface disorder on the electrical transport of conducting/ insulator/ conduction heterostructures, which is relevant for different applications, going from resistive switching memories (at room temperature) to Josephson junctions (at low temperatures). The superconducting transition of the GBCO electrode was characterized by electrical transport using the 4-prong configuration with low density of topological defects and with Tc over liquid N₂ can be obtained for thicknesses of 16 nm, our results demonstrate that GBCO films with an average root-mean-square (RMS) smaller than 1 nm and areas (up 100 um²) free of 3-D topological defects can be obtained.

Keywords: thin film, sputtering, conductive atomic force microscopy, tunnel junctions

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Authors: Lina F. Ballesteros, Hafsae Lamsaf, Miguel A. Cerqueira, Lorenzo M. Pastrana, Sandra Carvalho, Jose A. Teixeira, S. Calderon V.

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The use of bio-based packaging materials containing metallic and bimetallic nanostructures is relatively modern technology. In this sense, the food packaging industry has been investigating biological and renewable resources that can replace petroleum-based materials to reduce the environmental impact and, at the same time, including new functionalities using nanotechnology. Therefore, the main objective of the present work consisted of developing bio-based poly-lactic acid (PLA) films with Zinc (Zn) and Zinc-Iron (Zn-Fe) nanostructures deposited by magnetron sputtering. The structural, antimicrobial, and optical properties of the films were evaluated when exposed at 60% and 96% relative humidity (RH). The morphology and elemental analysis of the samples were determined by scanning (transmission) electron microscopy (SEM and STEM), and inductively coupled plasma optical emission spectroscopy (ICP-OES). The structure of the PLA was monitored before and after deposition by Fourier transform infrared spectroscopy (FTIR) analysis, and the antimicrobial and color assays were performed by using the zone of inhibition (ZOI) test and a Minolta colorimeter, respectively. Finally, the films were correlated in terms of the deposit conditions, Zn or Zn-Fe concentrations, and thickness. The results revealed PLA films with different morphologies, compositions, and thicknesses of Zn or Zn-Fe nanostructures. The samples showed a significant antibacterial and antifungal activity against E. coli, P. aeruginosa, P. fluorescens, S. aureus, and A. niger, and considerable changes of color and opacity at 96% RH, especially for the thinner nanostructures (150-250 nm). On the other hand, when the Fe fraction was increased, the lightness of samples increased, as well as their antimicrobial activity when compared to the films with pure Zn. Hence, these findings are relevant to the food packaging field since intelligent and active films with multiple properties can be developed.

Keywords: biopolymers, functional properties, magnetron sputtering, Zn and Zn-Fe nanostructures

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Authors: Sharon Waichman, Shahaf Froim, Ido Zukerman, Shmuel Barzilai, Shmual Hayun, Avi Raveh

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Boron carbide is a ceramic material with superior properties such as high chemical and thermal stability, high hardness and high wear resistance. Moreover, it has a big cross section for neutron absorption and therefore can be employed in nuclear based applications. However, an efficient attachment of boron carbide to a metal such as aluminum can be very challenging, mainly because of the formation of aluminum-carbon bonds that are unstable in humid environment, the affinity of oxygen to the metal and the different thermal expansion coefficients of the two materials that may cause internal stresses and a subsequent failure of the bond. Here, we aimed to achieving a strong and a durable attachment between the boron carbide coating and the aluminum substrate. For this purpose, we applied Ti as a thin intermediate layer that provides a gradual change in the thermal expansion coefficients of the configured layers. This layer is continuous and therefore prevents the formation of aluminum-carbon bonds. Boron carbide coatings with a thickness of 1-5 µm were deposited on the aluminum substrate by pulse-DC magnetron sputtering. Prior to the deposition of the boron carbide layer, the surface was pretreated by energetic ion plasma followed by deposition of the Ti intermediate adhesive layer in a continuous process. The properties of the Ti intermediate layer were adjusted by the bias applied to the substrate. The boron carbide/aluminum bond was evaluated by various methods and complementary techniques, such as SEM/EDS, XRD, XPS, FTIR spectroscopy and Glow Discharge Spectroscopy (GDS), in order to explore the structure, composition and the properties of the layers and to study the adherence mechanism of the boron carbide/aluminum contact. Based on the interfacial bond characteristics, we propose a desirable solution for improved adhesion of boron carbide to aluminum using a highly efficient intermediate adhesive layer.

Keywords: adhesion, boron carbide coatings, ceramic/metal bond, intermediate layer, pulsed-DC magnetron sputtering

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Authors: Mario Alejandro Grisales, M. Daniela Chimá, Gilberto Bejarano Gaitán

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High entropy alloys (HEA) and nitride (HEN) are currently very attractive to the automotive, aerospace, metalworking and materials forming manufacturing industry, among others, for exhibiting higher mechanical properties, wear resistance, and thermal stability than binary and ternary alloys. In this work medium-entropy coatings of TiTaZrNb and the nitrides of (TiTaZrNb)Nx were synthesized on to AISI 420 and M2 steel samples by the direct current magnetron sputtering technique. The influence of the bias voltage supplied to the substrate on the microstructure, chemical- and phase composition of the matrix coating was evaluated, and the effect of nitrogen flow on the microstructural, mechanical and tribological properties of the corresponding nitrides was studied. A change in the crystalline structure from BCC for TiTaZrNb coatings to FCC for (TiTaZrNb)Nx was observed, that is associated with the incorporation of nitrogen into the matrix and the consequent formation of a solid solution of (TiTaZrNb)Nx. An increase in hardness and residual stresses was observed with increasing bias voltage for TiTaZrNb, reaching 12.8 GPa for the coating deposited with a bias of -130V. In the case of (TiTaZrNb)Nx nitride, a greater hardness of 23 GPa is achieved for the coating deposited with a N2 flow of 12 sccm, which slightly drops to 21.7 GPa for that deposited with N2 flow of 15 sccm. The slight reduction in hardness could be associated with the precipitation of the TiN and ZrN phases that are formed at higher nitrogen flows. The specific wear rate of the deposited coatings ranged between 0.5xexp13 and 0.6xexp13 N/m2. The steel substrate exhibited an average hardness of 2.0 GPa and a specific wear rate of 203.2exp13 N/m2. Both the hardness and the specific wear rate of the synthesized nitride coatings were higher than that of the steel substrate, showing a protective effect of the steel against wear.

Keywords: medium entropy coatings, hard coatings, magnetron sputtering, tribology, wear resistance

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Authors: Yi Hu, Chun-Chi Lin, Shau-En Yeh, Shin Lee

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In this study, p–n heterojunctions with La0.5Sr0.5CoO3 (LSCO) and W-doped VO2 thin films were fabricated by the radio frequency (r.f.) magnetron sputtering technique and sol-gel process, respectively. The thickness of VO2 and LSCO thin films are about 40 nm and 400 nm, respectively. Good crystalline match between LSCO and VO2 films was observed from the SEM. The built-in voltages for the junction are about 1.1 V and 2.3 V for the sample in the metallic and insulating state, respectively. The sample can undergo the current induced MIT during applying field when the sample was heated at 40 and 50ºC. This is in agreement with the value obtained from the difference in the work functions of LSCO and VO2. The band structure of the heterojunction was proposed based on the results of analysis.

Keywords: hetrojection, Mott transition, switching , VO2

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Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

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Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

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Authors: Marie Kudrnová, Jana Rejková

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The samples of supplied INCONEL 601, 617, 625, and HASTELLOY C-22 alloys and experimental nickel alloy MoNiCr were examined by XPS (X-ray photoelectron spectroscopy) before and after exposure. The experiment was performed in a mixture of LiCl-KCl salt (58.2-41.8 wt. %). The exposure conditions were 440°C, pressure 0.2 MPa, 500 hours in an inert argon atmosphere. The XPS analysis shows that a thin oxide layer composed of metal oxides such as NiO, Cr₂O₃, and Nb₂O₅ was formed. After sputtering the exposed surface with Ar ions, metals were also detected in the elemental state, indicating a very thin protective oxide layer with a thickness in units of up to tens of nanometers.

Keywords: XPS, MSR, nickel alloy, metal oxides

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Authors: Vivek Garg, Brajendra S. Sengar, Gaurav Siddharth, Nisheka Anadkat, Amitesh Kumar, Shailendra Kumar, Shaibal Mukherjee

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CuInGaSe (CIGSe) is the dominant thin film solar cell technology. The band alignment of Buffer/CIGSe interface is one of the most crucial parameters for solar cell performance. In this article, the valence band offset (VBOff) and conduction band offset (CBOff) values of Cu(In0.70Ga0.30)Se/ 1 at.% Ga: Mg0.25Zn0.75O (GMZO) heterojunction, grown by dual ion beam sputtering system (DIBS), are calculated to understand the carrier transport mechanism at the heterojunction for the realization of all sputtered buffer-less solar cells. To determine the valence band offset (VBOff), ∆E_V at GMZO/CIGSe heterojunction interface, the standard method based on core-level photoemission is utilized. The value of ∆E_V can be evaluated by considering common core-level peaks. In our study, the values of (Valence band onset)VBOn, obtained by linear extrapolation method for GMZO and CIGSe films are calculated to be 2.86 and 0.76 eV. In the UPS spectra peak positions of Se 3d is observed in UPS spectra at 54.82 and 54.7 eV for CIGSe film and GMZO/CIGSe interface respectively, while the peak position of Mg 2p is observed at 50.09 and 50.12 eV for GMZO and GMZO/CIGSe interface respectively. The optical band gap of CIGSe and GMZO are obtained from absorption spectra procured from spectroscopic ellipsometry are 1.26 and 3.84 eV respectively. The calculated average values of ∆E_v and ∆E_C are estimated to be 2.37 and 0.21 eV, respectively, at room temperature. The calculated positive conduction band offset termed as a spike at the absorber junction is the required criterion for the high-efficiency solar cells for the efficient charge extraction from the junction. So we can conclude that the above study confirms GMZO thin films grown by the dual ion beam sputtering system are the suitable candidate for the CIGSe thin films based ultra-thin buffer-less solar cells. We investigated the band-offset properties at the GMZO/CIGSe heterojunction to verify the suitability of the GMZO for the realization of the buffer-less solar cells. The calculated average values of ∆E_V and ∆E_C are estimated to be 2.37 and 0.21 eV, respectively, at room temperature. The calculated positive conduction band offset termed as a spike at the absorber junction is the required criterion for the high-efficiency solar cells for the efficient charge extraction from the junction. So we can conclude that the above study confirms GMZO thin films grown by the dual ion beam sputtering system are the suitable candidate for the CIGSe thin films based ultra-thin buffer-less solar cells. Acknowledgment: We are thankful to DIBS, EDX, and XRD facility equipped at Sophisticated Instrument Centre (SIC) at IIT Indore. The authors B.S.S and A.K acknowledge CSIR and V.G acknowledge UGC, India for their fellowships. B.S.S is thankful to DST and IUSSTF for BASE Internship Award. Prof. Shaibal Mukherjee is thankful to DST and IUSSTF for BASE Fellowship and MEITY YFRF award. This work is partially supported by DAE BRNS, DST CERI, and DST-RFBR Project under India-Russia Programme of Cooperation in Science and Technology. We are thankful to Mukul Gupta for SIMS facility equipped at UGC-DAE Indore.

Keywords: CIGSe, DIBS, GMZO, solar cells, UPS

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Authors: Brahim Aissa

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Transparent conductive oxides (TCOs) used as front electrodes in solar cells must feature simultaneously high electrical conductivity, low contact resistance with the adjacent layers, and an appropriate refractive index for maximal light in-coupling into the device. However, these properties may conflict with each other, motivating thereby the search for TCOs with high performance. Additionally, due to the presence of temperature sensitive layers in many solar cell designs (for example, in thin-film silicon and silicon heterojunction (SHJ)), low-temperature deposition processes are more suitable. Several deposition techniques have been already explored to fabricate high-mobility TCOs at low temperatures, including sputter deposition, chemical vapor deposition, and atomic layer deposition. Among this variety of methods, to the best of our knowledge, magnetron sputtering deposition is the most established technique, despite the fact that it can lead to damage of underlying layers. The Sn doped In₂O₃ (ITO) is the most commonly used transparent electrode-contact in SHJ technology. In this work, we studied the properties of ITO thin films grown by RF sputtering. Using different oxygen fraction in the argon/oxygen plasma, we prepared ITO films deposited on glass substrates, on one hand, and on a-Si (p and n-types):H/intrinsic a-Si/glass substrates, on the other hand. Hall Effect measurements were systematically conducted together with total-transmittance (TT) and total-reflectance (TR) spectrometry. The electrical properties were drastically affected whereas the TT and TR were found to be slightly impacted by the oxygen variation. Furthermore, the time of flight-secondary ion mass spectrometry (TOF-SIMS) technique was used to determine the distribution of various species throughout the thickness of the ITO and at various interfaces. The depth profiling of indium, oxygen, tin, silicon, phosphorous, boron and hydrogen was investigated throughout the various thicknesses and interfaces, and obtained results are discussed accordingly. Finally, the extreme conditions were selected to fabricate rear emitter SHJ devices, and the photovoltaic performance was evaluated; the lower oxygen flow ratio was found to yield the best performance attributed to lower series resistance.

Keywords: solar cell, silicon heterojunction, oxygen content, optoelectronic properties

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Authors: Dhiflaoui Hafedh, Khlifi Kaouther, Ben Cheikh Larbi Ahmed

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Monolayer and multilayer coatings of CrN and AlCrN deposited on 100Cr6 (AISI 52100) substrate by PVD magnetron sputtering system. The micro structures of the coatings were characterized using atomic force microscopy (AFM). The AFM analysis revealed the presence of domes and craters which are uniformly distributed over all surfaces of the various layers. Nano indentation measurement of CrN coating showed maximum hardness (H) and modulus (E) of 14 GPa and 240 GPa, respectively. The measured H and E values of AlCrN coatings were found to be 30 GPa and 382 GPa, respectively. The improved hardness in both the coatings was attributed mainly to a reduction in crystallite size and decrease in surface roughness. The incorporation of Al into the CrN coatings has improved both hardness and Young’s modulus.

Keywords: CrN, AlCrN coatings, hardness, nanoindentation

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Authors: Mohammad Farooq Wani

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Tribological characterization of ZrN coatings deposited on titanium modified austenitic stainless steel (alloy D-9) substrates has been investigated. The coatings were deposited in the deposition temperature range 300–873 K, using the pulsed magnetron sputtering technique. Scratch adhesion tests were carried out using Rc indenter under various conditions of load. Detailed tribological studies were conducted to understand the friction and wear behaviour of these coatings. For all tribological studies steel and ceramic balls were used as counter face material. 3D-Surface profiles of all wear tracks was carried out using 3D universal profiler.

Keywords: ZrN, Surafce coating, thin film, tribology, friction and wear

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Authors: Mantas Sriubas, Kristina Bockute, Darius Virbukas, Giedrius Laukaitis

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In this work, the doped TiO2 (dopants – Ca, Mg) was investigated. The comparison between the physical vapour deposition methods as electron beam vapour deposition and magnetron sputtering was performed and the structural and electrical properties of the formed thin films were investigated. Thin films were deposited on different type of substrates: SiO2, Alloy 600 (Fe-Ni-Cr) and Al2O3 substrates. The structural properties were investigated using Ambios XP-200 profilometer, scanning electron microscope (SEM) Hitachi S-3400N, X-ray energy-dispersive spectroscope (EDS) Quad 5040 (Bruker AXS Microanalysis GmbH), X-ray diffractometer (XRD) D8 Discover (Bruker AXS GmbH) with glancing angles focusing geometry in a 20 – 70° range using the Cu Kα1 λ = 0.1540562 nm radiation). The impedance spectroscopy measurements were performed using Probostat® (NorECs AS) measurement cell in the frequency range from 10-1-106 Hz under reducing and oxidizing conditions in temperature range of 200 °C to 1200 °C. The investigation of the e-beam deposited Ca and Mg doped-TiO2 thin films shows that the thin films are dense without any visible pores and cavities and the thin films grow in zone T according Barna-Adamik SZM. Substrate temperature was kept 600 °C during the deposition and Ts/Tm ≈ 0.32 (substrate temperature (Ts) and coating material melting temperature (Tm)). The surface diffusion is high however, the grain boundary migration is strongly limited at this temperature. This means that structure is inhomogeneous and the columnar structure is mostly visible in the upper part of the films. According to XRD, the increasing of the Ca dopants’ concentration increases the crystallinity of the formed thin films and the crystallites size increase linearly and Ca dopants act as prohibitors. Thin films are comprised of anatase TiO2 phase with an exception of 2 % Ca doped TiO2, where a small peak of Ca arise. In the case of Mg doped-TiO2 the intensities of the XRD peaks decreases with increasing Mg molar concentration. It means that there are less diffraction planes of the particular orientation in thin films with higher impurities concentration. Thus, the crystallinity decreases with increasing Mg concentration and Mg dopants act as inhibitors. The impedance measurements show that the dopants changed the conductivity of the formed thin films. The conductivity varies from 10-3 S/cm to 10-4 S/cm at 800 °C under wet reducing conditions. The microstructure of the magnetron sputtered thin TiO2 films is different comparing to the thin films deposited using e-beam deposition therefore influencing other structural and electrical properties.

Keywords: electrical properties, electron beam deposition, magnetron sputtering, microstructure, titanium dioxide

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Authors: Sara Khamseh, Elahe Sharifi

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321 alloy steel is austenitic stainless steel with high oxidation resistance and is commonly used to fabricate heat exchangers and steam generators. However, the low hardness and weak tribological performance can cause dangerous failures during industrial operations. The well-designed protective coatings on 321 alloy steel surfaces with high hardness and good tribological performance can guarantee their safe applications. The surface protection of metal substrates using protective coatings showed high efficiency in prevailing these problems. Carbon-based multicomponent coatings, such as metal-added amorphous carbon coatings, are crucially necessary because of their remarkable mechanical and tribological performances. In the current study, (Nb: Si: a-C) multicomponent coatings (a-C: amorphous carbon) were coated on 321 alloys using a balanced magnetron (BM) sputtering system at room temperature. The effects of the Si/Nb ratio on microstructure, mechanical and tribological characteristics of (Nb: Si: a-C) composite coatings were investigated. The XRD and Raman analysis results showed that the coatings formed a composite structure of cubic diamond (C-D), NbC, and graphite-like carbon (GLC). The NbC phase's abundance decreased when the C-D phase's affluence increased with an increasing Si/Nb ratio. The coatings' indentation hardness and plasticity index (H³/E² ratio) increased with an increasing Si/Nb ratio. The better mechanical properties of the coatings with higher Si content can be attributed to the higher cubic diamond (C-D) content. The cubic diamond (C-D) is a challenging phase and can positively affect the mechanical performance of the coatings. It is well documented that in hard protective coatings, Si encourages amorphization. In addition, THE studies showed that Nb and Mo can act as a catalyst for nucleation and growth of hard cubic (C-D) and hexagonal (H-D) diamond phases in a-C coatings. In the current study, it seems that fully arranged nanocomposite coatings contain hard C-D and NbC phases that embedded in the amorphous carbon (GLC) phase is formed. This unique structure decreased grain boundary density and defects and resulted in high hardness and H³/E² ratio. Moreover, the COF and wear rate of the coatings decreased with increasing Si/Nb ratio. This can be attributed to the good mechanical properties of the coatings and the formation of graphite-like carbon (GLC) structure with lamellae arrangement in the coatings. The complex and self-lubricant coatings are successfully formed on the surface of 321 alloys. The results of the present study clarified that Si addition to (Nb: a-C) coatings improve the mechanical and tribological performance of the coatings on 321 alloy.

Keywords: COF, mechanical properties, microstructure, (Nb: Si: a-C) coatings, Wear rate

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Authors: Kuan Yu Lin, Shih Chih Chen

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This study focuses on the Al/HfO₂/Si/Al structure to explore the electrical properties of the structure. This experiment uses a radio frequency magnetron sputtering system to deposit high dielectric materials on p-type silicon substrates of 1~10 Ω-cm (100). Consider the hafnium dioxide film as a dielectric layer. Post-deposition annealing at 750°C in nitrogen atmosphere. Electron beam evaporation of metallic aluminum is then used to complete the top/bottom electrodes. The metal is post-annealed at 450°C for 20 minutes in a nitrogen environment to complete the MOS component. Its dielectric constant, equivalent oxide layer thickness, oxide layer defects, and leakage current mechanism are discussed. At PDA 750°C-5s, the maximum k value was found to be 21.2, and the EOT was 3.68nm.

Keywords: high-k gate dielectrics, HfO₂, post deposition annealing, RF magnetic

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Authors: S. M. Hamidi, M. Zamani

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Magneto-plasmonic (MP) structures have turned into essential tools for the amplification of magneto-optical (MO) responses via the combination of MO activity and surface Plasmon resonance (SPR). Both the plasmonic and the MO properties of the resulting MP structure become interrelated because the SPR of the metallic medium. This interconnection can be modified the wave vector of surface plasmon polariton (SPP) in MP multilayer [1] or enhanced the MO activity [2- 3] and also modified the sensor responses [4]. There are several types of MP structures which are studied to enhance MO response in miniaturized configuration. In this paper, we propose a new MP structure based on the nano-metal grating and we investigate the MO and optical properties of this new structure. Our new MP structure fabricate by DC magnetron sputtering method and our home made MO experimental setup use for characterization of the structure.

Keywords: Magneto-plasmonic structures, magneto-optical effect, nano-garting

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Authors: K. Kefif, Y. Bouizem, A. Belfedal, D. J. Sib, K. Zellama, l. Chahed

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Hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared by radio frequency magnetron sputtering at relatively low growth temperatures (Ts=100 °C). The films grown on glass substrate in order to use the new generation of substrates sensitive to elevated temperatures. Raman spectroscopy was applied to investigate the effect of the argon gas diluted in hydrogen, on the structural properties and the evolution of the micro structure in the films. Raman peak position, intensity and line width were used to characterize the quality and the percentage of the crystallites in the films. The results of this investigation suggest the existence of a threshold dilution around a gas mixture of argon (40%) and hydrogen (60%) for which the crystallization occurs, even at low deposition temperatures. The difference between the amorphous and the crystallized structures is well confirmed by spectroscopic ellipsometry (SE) technique.

Keywords: Silicon, Thin films, Structural properties, Raman spectroscopy, Ellipsometry

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Authors: Haesook Kim, Ha Na Ra, Mansu Kim, Hyun Gi Kim, Sung Soo Kim

Abstract:

Epoxy-ZrP (α-zirconium phosphate) nanocomposites were coated on inorganic barrier layer such as sputtering and atomic layer deposition (ALD) to improve the barrier properties and protect the layer. ZrP nanoplatelets were synthesized using a reflux method and exfoliated in the polymer matrix. The barrier properties of coating layer were characterized by measuring water vapor transmission rate (WVTR). The WVTR dramatically decreased after epoxy-ZrP nanocomposite coating, while maintaining the optical properties. It was also investigated the effect of epoxy-ZrP coating on inorganic layer after bending and reliability test. The optimal structure composed of inorganic and epoxy-ZrP nanocomposite layers was used in organic light emitting diodes (OLED) encapsulation.

Keywords: α-zirconium phosphate, barrier properties, epoxy nanocomposites, OLED encapsulation

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Authors: K. Kaouther, D. Hafedh, A. Ben Cheikh Larbi

Abstract:

Various structures and compositions thin films were deposited on 100C6 (AISI 52100) steel substrate by PVD magnetron sputtering system. The morphological proprieties were evaluated using an atomic force microscopy (AFM). Vickers microindentation tests were performed with a Shimadzu HMV-2000 hardness testing machine. Hardness measurement was carried out using Jonsson and Hogmark model. The results show that the coatings topography was dominated by domes and craters. Mechanical behavior and failure modes under microindentation were depending of coatings structure and composition. TiAlN multilayer showed exception in the microindentation resistance compared to TiN single layer and TiAlN/TiAlN nanolayer. Piled structure provides an increase of failure resistance and a decrease in cracks propagation.

Keywords: PVD thin films, multilayer, microindentation, cracking, damage mechanisms

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Authors: Min-Hao Wang, Shih-Chih Chen

Abstract:

Recently, the merits such as simple structure, low power consumption, and compatibility with complementary metal oxide semiconductor (CMOS) process give an advantage of resistive random access memory (RRAM) as a promising candidate for the next generation memory， hafnium dioxide (HfO2) has been widely studied as an oxide layer material, but the use of copper (Cu) as both top and bottom electrodes has rarely been studied. In this study, radio frequency sputtering was used to deposit the intermediate layer HfO₂, and electron beam evaporation was used. For the upper and lower electrodes (cu), using different AR: O ratios, we found that the control of the metal filament will make the filament widely distributed, causing the current to rise to the limit current during Reset. However, if the flow ratio is controlled well, the ON/OFF ratio can reach 104, and the set voltage is controlled below 3v.

Keywords: RRAM, metal filament, HfO₂, Cu electrode

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Authors: G. Rosaz, V. Semblanet, S. Calatroni, A. Sublet, M. Taborelli

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We report in this paper the design and qualification of a cylindrical unbalanced magnetron source. The dedicated magnetic assemblies were simulated using a finite element model. A hall-effect magnetic probe was then used to characterize those assemblies and compared to the theoretical magnetic profiles. These show a good agreement between the expected and actual values. The qualification of the different magnetic assemblies was then performed by measuring the ion flux density reaching the surface of the sample to be coated using a commercial retarding field energy analyzer. The strongest unbalanced configuration shows an increase from 0.016 A.cm^-2 to 0.074 A.cm^-2 of the ion flux density reaching the sample surface compared to the standard balanced configuration for a pressure 5.10^-3 mbar and a plasma source power of 300 W.

Keywords: ion energy distribution function, magnetron sputtering, niobium, unbalanced, SRF cavities, thin film

Procedia PDF Downloads 219

Authors: Peter Kus, Anna Ostroverkh, Yurii Yakovlev, Yevheniia Lobko, Roman Fiala, Ivan Khalakhan, Vladimir Matolin

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Hydrogen economy is a concept of low-emission society which harvests most of its energy from renewable sources (e.g., wind and solar) and in case of overproduction, electrochemically turns the excess amount into hydrogen, which serves as an energy carrier. Proton exchange membrane water electrolyzers (PEMWE) are the backbone of this concept. By fast-response electricity to hydrogen conversion, the PEMWEs will not only stabilize the electrical grid but also provide high-purity hydrogen for variety of fuel cell powered devices, ranging from consumer electronics to vehicles. Wider commercialization of PEMWE technology is however hindered by high prices of noble metals which are necessary for catalyzing the redox reactions within the cell. Namely, platinum for hydrogen evolution reaction (HER), running on cathode, and iridium for oxygen evolution reaction (OER) on anode. Possible way of how to lower the loading of Pt and Ir is by using conductive high-surface nanostructures as catalyst supports in conjunction with thin-film catalyst deposition. The presented study discusses unconventional technique of membrane electron assembly (MEA) preparation. Noble metal catalysts (Pt and Ir) were magnetron sputtered in very low loadings onto the surface of porous sublayers (located on gas diffusion layer or directly on membrane), forming so to say localized three-phase boundary. Ultrasonically sprayed corrosion resistant TiC-based sublayer was used as a support material on anode, whereas magnetron sputtered nanostructured etched nitrogenated carbon (CNx) served the same role on cathode. By using this configuration, we were able to significantly decrease the amount of noble metals (to thickness of just tens of nanometers), while keeping the performance comparable to that of average state-of-the-art catalysts. Complex characterization of prepared supported catalysts includes in-cell performance and durability tests, electrochemical impedance spectroscopy (EIS) as well as scanning electron microscopy (SEM) imaging and X-ray photoelectron spectroscopy (XPS) analysis. Our research proves that magnetron sputtering is a suitable method for thin-film deposition of electrocatalysts. Tested set-up of thin-film supported anode and cathode catalysts with combined loading of just 120 ug.cm⁻² yields remarkable values of specific current. Described approach of thin-film low-loading catalyst deposition might be relevant when noble metal reduction is the topmost priority.

Keywords: hydrogen economy, low-loading catalyst, magnetron sputtering, proton exchange membrane water electrolyzer

Procedia PDF Downloads 137

Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

Abstract:

Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: crystallinity, glow discharge, nitriding, sputtering

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Authors: Motonori Tamura

Abstract:

The hydrogen barrier properties of the coatings of diamond-like carbon (DLC) were evaluated. Using plasma chemical vapor deposition and sputtering, DLC coatings were deposited on Type 316L stainless steels. The hydrogen permeation rate was reduced to 1/1000 or lower by the DLC coatings. The DLC coatings with high hydrogen content had high hydrogen barrier function. For hydrogen diffusion in coatings, the movement of atoms through hydrogen trap sites such as pores in coatings, and crystal defects such as dislocations, is important. The DLC coatings are amorphous, and there are both sp3 and sp2 bonds, and excess hydrogen could be found in the interstitial space and the hydrogen trap sites. In the DLC coatings with high hydrogen content, these hydrogen trap sites are likely already filled with hydrogen atoms, and the movement of new hydrogen atoms could be limited.

Keywords: hydrogen permeation, stainless steels, diamond-like carbon, hydrogen trap sites

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Authors: Marie Kudrnova, Jana Petru

Abstract:

This study is part of the international research - Materials for Molten Salt Reactors (MSR) and addresses the part of the project dealing with the corrosion behavior of candidate construction materials. Inconel 625 was characterized by x-ray photoelectron spectroscopy (XPS) before and after high–temperature experiment in molten salt. The experiment was performed in a horizontal tube furnace molten salt reactor, at 450 °C in argon, at atmospheric pressure, for 150 hours. Industrially produced HITEC salt was used (NaNO3, KNO3, NaNO2). The XPS study was carried out using the ESCAProbe P apparatus (Omicron Nanotechnology Ltd.) equipped with a monochromatic Al Kα (1486.6 eV) X-ray source. The surface layer on alloy 625 after exposure contains only Na, C, O, and Ni (as NiOx) and Nb (as NbOx BE 206.8 eV). Ni was detected in the metallic state (Ni0 – Ni 2p BE-852.7 eV, NiOx - Ni 2p BE-854.7 eV) after a short Ar sputtering because the oxide layer on the surface was very thin. Nickel oxides can form a protective layer in the molten salt, but only future long-term exposures can determine the suitability of Inconel 625 for MSR.

Keywords: Inconel 625, molten salt, oxide layer, XPS

Procedia PDF Downloads 116