Search Results (16)

A novel artificial intelligence-assisted evaluation of the X-ray diffraction (XRD) peak profiles was elaborated for the characterization of the nanocrystallite microstructure in a combinatorial Co-Cr-Fe-Ni compositionally complex alloy (CCA) film. The layer was produced by a multiple beam sputtering physical vapor deposition (PVD) technique on a Si single crystal substrate with the diameter of about 10 cm. This new processing technique is able to produce combinatorial CCA films where the elemental concentrations vary in a wide range on the disk surface. The most important benefit of the combinatorial sample is that it can be used for the study of the correlation between the chemical composition and the microstructure on a single specimen. The microstructure can be characterized quickly in many points on the disk surface using synchrotron XRD. However, the evaluation of the diffraction patterns for the crystallite size and the density of lattice defects (e.g., dislocations and twin faults) using X-ray line profile analysis (XLPA) is not possible in a reasonable amount of time due to the large number (hundreds) of XRD patterns. In the present study, a machine learning-based X-ray line profile analysis (ML-XLPA) was developed and tested on the combinatorial Co-Cr-Fe-Ni film. The new method is able to produce maps of the characteristic parameters of the nanostructure (crystallite size, defect densities) on the disk surface very quickly. Since the novel technique was developed and tested only for face-centered cubic (FCC) structures, additional work is required for the extension of its applicability to other materials. Nevertheless, to the knowledge of the authors, this is the first ML-XLPA evaluation method in the literature, which can pave the way for further development of this methodology. Full article

Boron as thin film material is of relevance for use in modern micro- and nano-fabrication technology. In this research boron thin films are realized by a number of physical and chemical deposition methods, including magnetron sputtering, electron-beam evaporation, plasma enhanced chemical vapor deposition (CVD), thermal/non-plasma CVD, remote plasma CVD and atmospheric pressure CVD. Various physical, mechanical and chemical characteristics of these boron thin films are investigated, i.e., deposition rate, uniformity, roughness, stress, composition, defectivity and chemical resistance. Boron films realized by plasma enhanced chemical vapor deposition (PECVD) are found to be inert for conventional wet chemical etchants and have the lowest amount of defects, which makes this the best candidate to be integrated into the micro-fabrication processes. By varying the deposition parameters in the PECVD process, the influences of plasma power, pressure and precursor inflow on the deposition rate and intrinsic stress are further explored. Utilization of PECVD boron films as hard mask for wet etching is demonstrated by means of patterning followed by selective structuring of the silicon substrate, which shows that PECVD boron thin films can be successfully applied for micro-fabrication. Full article

A combinatorial Co-Cr-Fe-Ni compositional complex alloy (CCA) thin film disk with a thickness of 1 µm and a diameter of 10 cm was processed by multiple-beam-sputtering physical vapor deposition (PVD) using four pure metal sources. The chemical composition of the four constituent elements varied between 4 and 64 at.% in the film, depending on the distance from the four PVD sources. The crystal structure, the crystallite size, the density of lattice defects (e.g., dislocations and twin faults) and the crystallographic texture were studied as a function of the chemical composition. It was found that in a wide range of elemental concentrations a face-centered cubic (fcc) structure with {111} crystallographic texture formed during PVD. Considering the equilibrium phase diagrams, it can be concluded that mostly the phase composition of the PVD layer is far from the equilibrium. Body-centered cubic (bcc) and hexagonal-close packed (hcp) structures formed only in the parts of the film close to Co-Fe and Co-Cr sources, respectively. A nanocrystalline microstructure with the grain size of 10–20 nm was developed in the whole layer, irrespective of the chemical composition. Transmission electron microscopy indicated a columnar growth of the film during PVD. The density of as-grown dislocations and twin faults was very high, as obtained by synchrotron X-ray diffraction peak profile analysis. The nanohardness and the elastic modulus were determined by indentation for the different chemical compositions on the combinatorial PVD film. This study is the continuation of a former research published recently in Nagy et al., Materials 14 (2021) 3357. In the previous work, only the fcc part of the sample was investigated. In the present paper, the study was extended to the bcc, hcp and multiphase regions. Full article

Diamond is one of the fascinating films appropriate for optoelectronic applications due to its wide bandgap (5.45 eV), high thermal conductivity (3320 W m⁻¹·K⁻¹), and strong chemical stability. In this report, we synthesized a type of diamond film called nanocrystalline diamond (NCD) by employing a physical vapor deposition method. The synthesis process was performed in different ratios of nitrogen and hydrogen mixed gas atmospheres to form nitrogen-doped (n-type) NCD films. A high-resolution scanning electron microscope confirmed the nature of the deposited films to contain diamond nanograins embedded into the amorphous carbon matrix. Sensitive spectroscopic investigations, including X-ray photoemission (XPS) and near-edge X-ray absorption fine structure (NEXAFS), were performed using a synchrotron beam. XPS spectra indicated that the nitrogen content in the film increased with the inflow ratio of nitrogen and hydrogen gas (I_N/H). NEXAFS spectra revealed that the σ*C–C peak weakened, accompanied by a π*C=N peak strengthened with nitrogen doping. This structural modification after nitrogen doping was found to generate unpaired electrons with the formation of C–N and C=N bonding in grain boundaries (GBs). The measured electrical conductivity increased with nitrogen content, which confirms the suggestion of structural investigations that nitrogen-doping generated free electrons at the GBs of the NCD films. Full article

The primary objective of this study was to investigate and compare the surface topography of hard coatings deposited by three different physical vapor deposition methods (PVD): low-voltage electron beam evaporation, unbalanced magnetron sputtering and cathodic arc evaporation. In these deposition systems, various ion etching techniques were applied for substrate cleaning. The paper summarizes our experience and the expertise gained during many years of development of PVD hard coatings for the protection of tools and machine components. Surface topography was investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), scanning transmission electron microscopy (STEM) and 3D stylus profilometry. Observed similarities and differences among samples deposited by various deposition methods are discussed and correlated with substrate material selection, substrate pretreatment and deposition conditions. Large variations in the surface topography were observed between selected deposition techniques, both after ion etching and deposition processes. The main features and implications of surface cleaning by ion etching are discussed and the physical phenomena involved in this process are reviewed. During a given deposition run as well as from one run to another, a large spatial variation of etching rates was observed due to the difference in substrate geometry and batching configurations. Variations related to the specific substrate rotation (i.e., temporal variations in the etching and deposition) were also observed. The etching efficiency can be explained by the influence of different process parameters, such as substrate-to-source orientation and distance, shadowing and electric field effects. The surface roughness of PVD coatings mainly originates from growth defects (droplets, nodular defects, pinholes, craters, etc.). We briefly describe the causes of their formation. Full article

A nanocrystalline Co-Cr-Ni-Fe compositional complex alloy (CCA) film with a thickness of about 1 micron was produced by a multiple-beam-sputtering physical vapor deposition (PVD) technique. The main advantage of this novel method is that it does not require alloy targets, but rather uses commercially pure metal sources. Another benefit of the application of this technique is that it produces compositional gradient samples on a disk surface with a wide range of elemental concentrations, enabling combinatorial analysis of CCA films. In this study, the variation of the phase composition, the microstructure (crystallite size and defect density), and the mechanical performance (hardness and elastic modulus) as a function of the chemical composition was studied in a combinatorial Co-Cr-Ni-Fe thin film sample that was produced on a surface of a disk with a diameter of about 10 cm. The spatial variation of the crystallite size and the density of lattice defects (e.g., dislocations and twin faults) were investigated by X-ray diffraction line profile analysis performed on the patterns taken by synchrotron radiation. The hardness and the elastic modulus were measured by the nanoindentation technique. It was found that a single-phase face-centered cubic (fcc) structure was formed for a wide range of chemical compositions. The microstructure was nanocrystalline with a crystallite size of 10–27 nm and contained a high lattice defect density. The hardness and the elastic modulus values measured for very different compositions were in the ranges of 8.4–11.8 and 182–239 GPa, respectively. Full article

Electron interaction with methane molecule and accurate determination of its elastic cross-section is a demanding task for both experimental and theoretical standpoints and relevant for our better understanding of the processes in Earth’s and Solar outer planet atmospheres, the greenhouse effect or in plasma physics applications like vapor deposition, complex plasma-wall interactions and edge plasma regions of Tokamak. Methane can serve as a test molecule for advancing novel electron-molecule collision theories. We present a combined experimental and theoretical study of the elastic electron differential cross-section from methane molecule, as well as integral and momentum transfer cross-sections in the intermediate energy range (50–300 eV). The experimental setup, based on a crossed beam technique, comprising of an electron gun, a single capillary gas needle and detection system with a channeltron is used in the measurements. The absolute values for cross-sections are obtained by relative-flow method, using argon as a reference. Theoretical results are acquired using two approximations: simple sum of individual atomic cross-sections and the other with molecular effect taken into the account. Full article

This article focuses on the properties of the BaCeO₃ thin films formed by electron-beam vapor deposition and investigates the formation of barium cerates on supports with different thermal expansion coefficients (Stainless Steel, Invar, Glass Sealing, and Inconel substrates) and the influence of the technological parameters on the properties of the formed thin films with an emphasis on the stability of the films. Morphology and phase composition and mechanical and electrical properties were investigated. It was found that the main factors influencing the phase composition and morphology of the films are the temperature of the support and the deposition rate. However, the mechanical properties of the films are mostly influenced by strains introduced to thin films by using different supports. Two interesting features of the electrical properties of the studied strained films were noticed: the film with the highest in-plane tensile strain showed the lowest activation energy of total conductivity, whereas the film with the lowest strain showed the highest value of total conductivity. Full article

Scandia alumina stabilized zirconia (ScAlSZ) thin films were deposited using e-beam evaporation, and the effects of deposition parameters on the structure and chemical composition were investigated. The analysis of thin films was carried out using Energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-Ray Diffraction Analysis (XRD) and Raman spectroscopy methods. It was found that the chemical composition of ScAlSZ thin films was different from the chemical composition of the initial powder. Moreover, the Al concentration in thin films depends on the deposition rate, resulting in a lower concentration using a higher deposition rate. XPS analysis revealed that ZrO_x, oxygen vacancies, high concentrations of Al₂O₃ and metallic Al exist in thin films and influence their structural properties. The crystallinity is higher when the concentration of Al is lower (higher deposition rate) and at higher substrate temperatures. Further, the amount of cubic phase is higher and the amount of tetragonal phase lower when using a higher deposition rate. Full article

Liquid-borne particles sampling and cantilever-based mass detection are widely applied in many industrial and scientific fields e.g., in the detection of physical, chemical, and biological particles, and disease diagnostics, etc. Microscopic analysis of particles-adsorbed cantilever-samples can provide a good basis for measurement comparison. However, when a particles-laden droplet on a solid surface is vaporized, a cluster-ring deposit is often yielded which makes particles counting difficult or impractical. Nevertheless, in this study, we present an approach, i.e., on-cantilever particles imprinting, which effectively defies such odds to sample and deposit countable single particles on a sensing surface. Initially, we designed and fabricated a triangular microcantilever sensor whose mass m₀, total beam-length L, and clamped-end beam-width w are equivalent to that of a rectangular/normal cantilever but with a higher resonant frequency (271 kHz), enhanced sensitivity (0.13 Hz/pg), and quality factor (~3000). To imprint particles on these cantilever sensors, various calibrated stainless steel dispensing tips were utilized to pioneer this study by dipping and retracting each tip from a small particle-laden droplet (resting on a hydrophobic n-type silicon substrate), followed by tip-sensor-contact (at a target point on the sensing area) to detach the solution (from the tip) and adsorb the particles, and ultimately determine the particles mass concentration. Upon imprinting/adsorbing the particles on the sensor, resonant frequency response measurements were made to determine the mass (or number of particles). A minimum detectable mass of ~0.05 pg was demonstrated. To further validate and compare such results, cantilever samples (containing adsorbed particles) were imaged by scanning electron microscopy (SEM) to determine the number of particles through counting (from which, the lowest count of about 11 magnetic polystyrene particles was obtained). The practicality of particle counting was essentially due to monolayer particle arrangement on the sensing surface. Moreover, in this work, the main measurement process influences are also explicitly examined. Full article

Metallic film-coated porous silicon (PSi) has been reported as a lucrative surface-enhanced Raman scattering (SERS) substrate. The solution-based fabrication process is facile and easy; however, it requires additional reducing agent and extra chemical treatment, as well as hinders the suitability as a reproducible SERS substrate due to irregular hot spot generation via irregular deposition of metallic nanocrystallites. To address this issue, we report a unique one-step electronic beam (e-beam) physical vapor deposition (PVD) method to fabricate a consistent layer of gold (Au) nanofilm on PSi. Moreover, to achieve the best output as a SERS substrate, PSi prepared by electrochemical etching was used as template to generate an Au layer of irregular surface, offering the surface roughness feature of the PSi–Au thin film. Furthermore, to investigate the etching role and Au film thickness, Au-nanocrystallites of varying thickness (5, 7, and 10 nm) showing discrete surface morphology were characterized and evaluated for SERS effect using Rhodamine 6G (R6G). The SERS signal of R6G adsorbed on PSi–Au thin film showed a marked enhancement, around three-fold enhancement factor (EF), than the Si–Au thin film. The optimal SERS output was obtained for PSi–Au substrate of 7 nm Au film thickness. This study thus indicates that the SERS enhancement relies on the Au film thickness and the roughness feature of the PSi–Au substrate. Full article

The plasma spray–physical vapor deposition (PS–PVD) process has received considerable attention due to its non-line of sight deposition ability, high deposition rates, and cost efficiency. Compared with electron beam–physical vapor deposition (EB–PVD), PS–PVD can also prepare thermal barrier coatings (TBCs) with columnar microstructures. In this paper, yttria-stabilized zirconia (YSZ) coatings were fabricated by PS–PVD. Results showed that the as-deposited coating presented a typical columnar structure and was mainly composed of metastable tetragonal (t′-ZrO₂) phase. With thermal exposure, the initial t′ phase of YSZ evolved gradually into monoclinic (m-ZrO₂) phase. Significant increase in hardness (H) and the Young’s modulus (E) of the coating was attributed to the sintering effect of the coating during the thermal exposure, dependent on exposure temperature and time. However, the values of H and E decreased in the coatings thermally treated at 1300–1500 °C for 24 h, which is mainly affected by the formation of m-ZrO₂ phase. Full article

In this work, scandia-doped zirconia (ScSZ) and scandia–alumina co-doped zirconia (ScSZAl) thin films were prepared by electron beam vapor deposition. X-ray diffraction (XRD) results indicated a presence of ZrO₂ cubic phase structure, yet Raman analysis revealed the existence of secondary tetragonal and rhombohedral phases. Thus, XRD measurements were supported by Raman spectroscopy in order to comprehensively analyze the structure of formed ScSZ and ScSZAl thin films. It was also found that Al dopant slows down the formation of the cubic phase. The impedance measurements affirmed the correlation of the amount of secondary phases with the conductivity results and nonlinear crystallite size dependence. Full article

Arrays of 1D-vertically arranged gallium nitride (GaN) nanorods (NRs) are fabricated on sapphire and connected to both bottom and freestanding top contacts. This shows a fully validated top-down method to obtain ordered arrays of high-surface-to-volume elements that can be electrically interrogated and used, e.g., for sensing applications. Specifically, these will be used as highly integrated heating elements for conductometric gas sensors in self-heating operation. Detailed fabrication and processing steps involving inductively coupled plasma reactive ion etching (ICP-RIE), KOH-etching, interspace filling, and electron-beam physical vapor deposition technologies are discussed, in which they can be well adjusted and combined to obtain vertical GaN NRs as thin as 300 nm in arbitrarily large and regular arrays (e.g., 1 × 1, 3 × 3, 9 × 10 elements). These developed devices are proposed as a novel sensor platform for temperature-activated measurements that can be produced at a large scale offering low-power, and very stable temperature control. Full article

The influence of a specific surface area of evaporating powder on the properties of thin Sm-doped cerium (SDC) oxide films has not yet been sufficiently investigated. Therefore, SDC films were deposited by e-beam evaporation using Sm_0.2Ce_0.8O_2-δ powders of 6.2 m²/g, 11.3 m²/g, and 201.3 m²/g specific surface area on SiO₂, and Al₂O₃ substrates. X-Ray Diffraction (XRD) analysis showed that SDC thin films deposited on 600 °C SiO₂ substrates changed their preferred orientation from (111) to (311), (200), and (220) when evaporating 6.2 m²/g and 11.3 m²/g powders and using 0.2 nm/s, 1.2 nm/s, and 1.6 nm/s deposition rates. However, thin films deposited by evaporating powder of 201.3 m²/g specific surface area do not change their preferred orientation. The crystallite size of the SDC thin films depends on the substrate temperature and specific surface area of the evaporating powder. It increases from 6.40 nm to 89.1 nm with increasing substrate temperature (50–600 °C). Moreover, crystallites formed by evaporating a powder of 201.3 m²/g specific surface area are 1.4 times larger than crystallites formed by evaporating a powder of 6.2 m²/g specific surface area. An impedance analysis revealed that the normalized resistance of “grains” is higher than the normalized resistance of grain boundaries. Moreover, a total conductivity depends on crystallite size. It changes from 4.4 × 10⁻⁷ S/cm to 1.1 × 10⁻² S/cm (600 °C) when the crystallite sizes vary from 6.40 nm to 89.10 nm. In addition, the optical band gap becomes wider with increasing crystallite size proving that the Ce³⁺ concentration decreases with an increasing crystallite size. Full article