Advanced Functional and Structural Thin Films and Coatings: On-Demand Oral Presentations
Sponsored by: TMS: Thin Films and Interfaces Committee
Program Organizers: Ramana Chintalapalle, University of Texas at El Paso; Adele Carrado, University of Strasbourg; Gerald Ferblantier, University of Strasbourg - IUT LP / ICube Laboratory - CNRS; Karine Mougin, Cnrs, Is2m; Heinz Palkowski, Clausthal University of Technology; Nuggehalli Ravindra, New Jersey Institute of Technology
Monday 8:00 AM
March 14, 2022
Room: Advanced Materials
Location: On-Demand Room
Silicone Breast Implants: Grafting of a Bioactive Polymer to Improve the Bio-integration: Mylan Lam1; Vincent Humblot2; Romain Vayron3; Véronique Migonney1; Celine Falentin-Daudre1; 1Universite Sorbonne Paris Nord; 2Université Bourgogne Franche-Comté; 3Université de Valenciennes
Silicone breast implant (BI) issues have raised many concerns these past years. Part of the top 10 most implantable biomedical devices, BIs are widely used for aesthetic and reconstructive surgeries. However, as with any devices, BIs are subjected to healthcare-associated infections as the development of capsular contractures mostly or, more rarely, the apparition of large cell anaplasic lymphoma, a cancer-related to breast prosthesis. The grafting of bioactive polymers has been actively demonstrated to improve surfaces’ bio-integration by conferring them an antibacterial property and improving biocompatibility. In the scientific literature, numerous strategies are reported to overcome bacterial biofilms and improve the surface’s biocompatibility by surface modifications. Our team has recently achieved a simple way to graft the poly(styrene sodium sulfonate) directly on silicone breast implants outer shell only using UV irradiation with a grafting “from” strategy. Characterization methods as SEM, XPS, AFM, ATR-FTIR, colorimetric assay, and WCA confirmed the grafting.
Doping of Biomimetic Calcium-deficient Hydroxyapatite Deposited on Activated Carbon Fiber Cloth to Improve Bone Regeneration: Florian Olivier1; Nathalie Rochet2; Sylvie Bonnamy1; 1ICMN/CNRS; 2iBV/ INSERM
In previous study we shown that sono-electrodeposition process can be optimized to coat activated carbon fiber cloth (ACC) with carbonated calcium-deficient hydroxyapatite (CDA). In the present study, this process is used to dope CDA coatings in performing calcium substitution with cations such as strontium, manganese and gallium. Cations-substituted CDA coatings were synthetized and quantitatively controlled up to 10 at.%. In this range, the presence of substitution does not modify the microtexture and slightly modified the crystallographic structure. Especially for the strontium-substituted CDA, the biocompatibility of the materials was tested using primary human osteoblasts. It revealed a positive and dose-dependent effect of strontium addition on osteoblast activity and proliferation. In vivo experiments were performed in a model of rat femoral defect to investigate bone regeneration. Results revealed the high biocompatibility of Sr-substituted CDA/ACC biomaterials and highlighted their efficacy to accelerate the bone defect reconstruction by simple apposition on the wounded zone.
Materials for Antireflective Coatings in Photovoltaics - An Overview: Vishal Mehta1; NM Ravindra2; Andrew Cochran1; Cory Conkel1; 1Ohio Northern University; 2New Jersey Institute of Technology
Optical properties of dielectrics play a critical role in various applications including the design and manufacture of optical components & devices such as detectors, filters, imagers, lenses, optical coatings, photonic crystals, sensors and waveguides, and solar cells. Reflectance due to varying thicknesses of different dielectrics such as Aluminum Oxide (Al2O3), Silicon Dioxide (SiO2), Indium Tin Oxide (ITO), Magnesium Fluoride (MgF2) and Silicon Nitride (Si3N4) have been simulated and compared in the range of visible to near infrared by mathematical modelling using MATLAB simulations. The results of the evolution of spectral properties, as a function of dielectric material thickness, on silicon substrates will be presented.
Grafting Phosphonic Acid Polymers onto Titanium Implant by UV Irradiation: Caroline Pereira1; Véronique Migonney1; Céline Falentin-Daudré1; 1LBPS/CSPBAT, UMR CNRS 7244, Institut Galilée, Université Sorbonne Paris Nord
Titanium (Ti) and its alloys are considerably used as biomaterials for hard tissue replacements. These materials have excellent physical and chemical properties such as good corrosion resistance, acceptable biocompatibility, and mechanical properties close to human bone. However, unmodified Ti-based materials bind to the host tissue poorly. Different techniques have been proposed to enhance bone growth around the implant. One interesting method is grafting bioactive polymers. Previous studies carried out in our laboratory have shown that polymers such as poly (sodium styrene sulfonate) (polyNaSS), poly (methacrylic acid) (polyMA) can favor osteoblast cell adhesion and differentiation. In this context, we propose to chemically modify Ti with a phosphonic acid-based polymer, poly (vinyl benzyl phosphonic acid) (polyVBP). This study assessed poly(VBP) grafting's effect on Ti surfaces and its bioactivity. Ti grafted samples showed significantly better response with osteoblast cells, related to enhanced interaction between cells and the surface due to phosphonate groups' presence.
Fifty Shades of TiN: How Deposition Conditions Influence the Growth Morphology and Thereby Hardness and Especially Fracture Toughness: Paul Mayrhofer1; Rainer Hahn1; Alexander Kirnbauer1; 1TU Wien
Almost fifty different TiN coatings were prepared by reactive and unreactive magnetron sputtering, as well as by reactive cathodic arc evaporation. In addition to vary between these three individual deposition techniques, we also individually varied the substrate temperature, partial pressures, substrates (e.g., single-phase MgO, to allow for epitaxial growth or not), as well as bias potential. The fracture toughness of these individually prepared TiN coatings was evaluated from micromechanical bending tests (inside a FEGSEM) of free-standing cantilevers. The individual deposition techniques and conditions result in either pronounced columnar or rather dense growth morphologies, with open or compact column and grain boundary regions. Due to these variations in growth morphology the hardness (obtained by nanoindentation with the Oliver–Pharr method) of TiN varied between 15.9 and 39.7 GPa and their fracture toughness between 0.6 and 2.9 MPa√m.
In-situ Mapping of Local Orientation and Strain in a Fully Operable Infrared Sensor Using Dark Field X-ray Microscopy: Can Yildirim1; Philippe Ballet2; Patrice Gergaud2; Francois Boulard2; Tao Zhou3; Raphael Pesci4; Tobias Schulli2; Nicolas Baier2; Thanh Nguyen2; Brellier Delphine2; 1European Synchrotron Radiation Facility; 2CEA; 3ANL; 4ENSAM
Hybridized focal plane array HgCdTe (MCT) sensors are the workhorse of high performance infrared detectors covering a broad range of applications from space investigation to gas monitoring. Here we dark-field X-ray microscopy (DFXM) to map the structural variations of a fully operable MCT sensor at temperatures down to 80 K. We report, for the first time, on the nanoscale structural evolution over a large population of photodiodes at operating temperatures with high spatial and angular resolution. Our results show that lattice distortion and strain in the MCT epilayer increases at lower temperatures. The FWHM values of the rocking curves reach up to 0.02° at 80 K, three times higher than the room temperature value. The thermal cycle results show that the thermal effects are almost completely reversible and the measure strain is in the elastic regime. We discuss the origin of the temperature-generated structural modifications using complimentary finite element modelling.
Study on Surface Cracking and Interfacial Delamination of Metallic Coatings Using a Tension Test: Deepesh Yadav1; Sanjay Sampath1; B N Jaya1; 1Indian Institute of Technology Bombay
Surface cracking and interfacial delamination of metallic coatings, deposited by high-velocity oxy-fuel technique, have been investigated under tension test. Local strain distribution has been determined in the coating and substrate by digital image correlation for increasing applied global strain and, results reveal that coating and substrate show same strain until the elastic limit of the substrate is reached. As the substrate is plastically deformed interface delamination takes place in the metallic Ni and Ni-5Al coatings while both surface cracking and delamination take place in the NiCrAlY coating. Results also show no plastic deformation occurs in these metallic coatings throughout the test. Numerical simulations have been used to determine stress distribution in the coating, substrate and at the interface, to quantify the fracture strength of the coating and interfacial shear strength, based on the failure mode experimentally observed.
Surface Chemistry and Subsurface Microstructure of Al 2024-T3 Laser-interference Structured: Adrian Sabau1; Harry Meyer1; Donovan Leonard1; 1Oak Ridge National Laboratory
For adhesive joining and coating applications, non-chemical surface preparation techniques are needed to reduce the environmental impact and associated costs with chemical surface preparation. In this study, the laser-interference technique was employed in a continuous scanning mode to functionalize the surface of Al 2024-T3 for enhanced coating adhesion and corrosion protection. The laser-interference power profile was created by splitting the beam and guiding both beams on the same spot, creating a line-interference pattern on the treated surface. XPS was used to assess the “cleaning” of the surface and the extent of oxide layer regrowth. SEM was used to characterize the sub-surface microstructure modifications, e.g., the heat-affected zone and precipitate dissolution. Aside from demonstrated periodic micron-scale topology, numerous clusters of nano-scale spherical particles were found to be present within ~250 nm below the surface. Also, several bands seem evident in the lower part of the precipitate dissolution area.
Stress Evolution and Recovery in High-entropy Metal Sublattice Diborides: Alexander Kirnbauer1; Peter Polcik2; Paul Mayrhofer3; 1TU Wien; 2Plansee Composite Materials GmbH; 3TU Wien, Thin Film Materials Science Division
A high entropy metal sublattice diboride (HESB) consisting of (Hf,Ta,V,W,Zr) has been synthesised by DC magnetron sputtering at different substrate temperatures. The stress evolution of the different coatings as well as recovery processes have been investigated by curvature measurements using a K-MOS thermal scan wafer curvature. The results show that all the coatings exhibit compressive residual stresses after deposition with a decreasing tendency for coatings deposited at higher substrate temperatures. Evaluating the thermal expansion coefficient shows a lower value for the HESB than for the used sapphire substrates leading to a decrease of compressive stresses when heating the samples. To investigate ongoing recovery processes the samples were held at a target temperature of 900 °C for 2 hours and subsequently investigated by XRD, nanoindentation, and detailed transmission electron microscopy.
Large Scale Growth of Diamond on Surface-terminated Silicon-incorporated Diamond-like Carbon Thin Films: Parand Riley1; Pratik Joshi1; Roger Narayan1; Jagdish Narayan1; 1North Carolina State University
Continuous diamond growth over large areas with reduced thermal stress is fundamental to benefit from the unique properties of diamond. We report a method to modify the surface of silicon-incorporated diamond-like carbon (Si-DLC) thin-film to enhance the nucleation and growth of diamond. In this method, the surfaces of Si-DLC films are plasma treated by fluorine and oxygen species using a reactive ion etching process, to produce fluorine-terminated Si-DLC (F Si-DLC) and Oxygen-terminated Si-DLC (O Si-DLC) films. The analyses represented that the sp2/sp3 carbon bond ratio on the surface of F Si-DLC and O Si-DLC has diminished from 20.28% in Si-DLC to 4.41% and 8.96%, respectively. Moreover, new sp3 hybridized bonds formed on the surface of F Si-DLC and O Si-DLC films. Analyses results proved that in comparison with Si-DLC, the nucleation density and growth of diamond on F Si-DLC and O Si-DLC films have enhanced significantly, and the stress reduced.
Application of Mg/Al2O3 and Mg/SiO2 Nanolaminates for Uniform and Controlled Corrosion of Biodegradable Implants: Pratap Deshmukh1; Sudheer Neralla1; Jagannathan Sankar1; Sergey Yarmolenko1; 1North Carolina A&T State University
Degradable thin films are found to be effective for controlling corrosion of biodegradable implant materials. We have shown that uniform corrosion of magnesium alloy substrates can be achieved by depositing slow-degrading water-permeable Mg/MeOx nanolaminates. In this study, model Mg/Al2O3 and Mg/SiO2 nanolaminates, with bilayer thickness varying from 20 to 100 nm, were deposited on glass substrates using magnetron sputtering techniques at room temperature. These coatings degrade through formation and growth of pores in magnesium layers resulted in reaction of Mg with water penetrating through defects in oxide layers. Applicability of these nanolaminates for controlling degradation was studied by immersion of the samples in different concentrations of saline and measuring pore growth rate at 37°C using optical microscopy. Effect of oxide layer thickness, saline flow rate and sputtering deposition parameters on pore density and corrosion rate was investigated. It was found that nanolaminate degradation time is proportional to number of bilayers.
Effect of Oxygen Partial Pressure and Pulse Frequency on the Structure and Properties of Tungsten Incorporated Ga2O3 Films made by Pulsed Laser Deposition: Francelia Sanchez1; Debabrata Das2; C.V. Ramana2; 1University of Texas at El Paso; 2UTEP
Gallium oxide (Ga2O3), which is an ultra-wide band gap material, has potential for integration into the next-generation electronic and optoelectronic devices. High physical and chemical stability also makes intrinsic and doped Ga2O3 interesting for many technological applications. In this work, the effect of oxygen partial pressure (pO2) and pulsed-laser frequency (fp) on the structure, morphology, and optical properties of tungsten (W) incorporated Ga2O3 (Ga2-2xWxO3, GWO) films made by pulsed laser deposition (PLD) investigated. The GWO films were deposited onto Si(100) at 700°C by varying pO2 and fp in the range of 50 to 200 mTorr and 3 to 5 Hz, respectively. X-ray diffraction, atomic force microscopy, UV-visible spectrophotometry, and spectroscopic ellipsometry were employed to understand the structure-property correlation. The results indicate that the grain size and crystallinity increase with oxygen partial pressure while the inverse correlation exists with the frequency. These changes also influence the optical properties of GWO films.
Improvement of Hydrophilicity and Wetting Behavior on Patterned PLA Substrates by AP Plasma Treatment and APTES Grafting: Mai Uyên1; Po-Yu Chen1; 1National Tsing Hua University
Polylactic acid (PLA) substrates with tunable wettability and unidirectional wetting behavior were fabricated by combining 3D printing and surface modification. The atmospheric pressure plasma (APP) was used to modify the PLA surface, followed by grafting with (3-aminopropyl)triethoxysilane (APTES) in hydrolysis solution to achieve hydrophilicity with measured contact angle of ~45°. Atomic force microscopy (AFM) was applied to characterize morphology after different treatments. The success of hydrolyzed APTES grafting onto surface was confirmed by X-ray photoelectron spectroscopy (XPS), which showed increases in C1s, O1s and N1s peaks of the grafted sample compared to untreated and plasma treated sample. The effective hydrophilicity was certified by investigating the long-term durability in contact angles on the treated PLA samples after 20 days. Furthermore, arrowhead-structured arrays were designed and fabricated by 3D printing followed by AP plasma modification and grafting, which further exhibited unidirectional liquid transportation and can be applied in various fields.
Non-reactively Sputtered Ultra-high Temperature Nb-C Coatings: Ahmed Bahr1; Rainer Hahn1; Oliver Hudak1; Tomasz wojcik1; Jürgen Ramm2; Szilard Kolozsvári3; Eleni Ntemou4; Eduardo Pitthan4; Daniel Primetzhofer4; Alexander Kirnbauer5; Helmut Riedl-Tragenreif1; 1Christian Doppler Laboratory for Surface Engineering of high-performance Components, TU Wien; 2Oerlikon Balzers, Oerlikon Surface Solutions AG; 3Plansee Composite Materials GmbH; 4Department of Physics and Astronomy, Uppsala University; 5Institute of Materials Science and Technology, TU Wien
Physical vapor deposited transition metal carbide (TMC) based thin films are known to form nanocomposite microstructures comprised of nanocrystalline metal carbide grains embedded into an amorphous C matrix. The structural and thermomechanical properties of NbC films are strongly influenced by the carbon content determined by the C/Me ratio and the morphology. Here, we employed high power pulsed magnetron sputtering to deposit extremely hard NbC thin films and investigated the influence of the deposition parameters on the microstructure, thermo-mechanical properties, fracture behavior, as well as corrosion and oxidation resistance. Through distinct control of the peak power density, we can control the stoichiometry, as well as crystallinity of the films, that leading to a wide range of thermo-mechanical properties. The extremely high phase stability of NbC coatings (up to 1600 °C) stands in contrast to the limited oxidation resistance at around 600 °C (a well-known effect for coating materials based on TMC).