Triode Magnetron Sputtering Research Articles

Tribological and Corrosion Behavior of AISI 1045 Coated with AISI 316 Film Produced By Triode Magnetron Sputtering

Tribological and Corrosion Behavior of AISI 1045 Coated with AISI 316 Film Produced By Triode Magnetron Sputtering

Rutile TiO2 thin films growth on glass substrates with generation of high entropy interface

TiO2 thin films obtained through Reactive Magnetron Sputtering (RMS) have been extensively studied in the last decades for several applications as photocatalyst and self-cleaning coats. However, reactive deposition through MS onto large area substrates can be troublesome due to inhomogeneous films thickness and poor adhesion between film and substrate. This paper investigates the deposition of TiO2 thin films on glass substrates through a two steps method, namely: 1- deposition of nanometer thickness Ti metallic films on glass substrate, through triode magnetron sputtering; 2- oxidation of the Ti film through thermal treatment in atmospheric air, to obtain stoichiometric TiO2 layers. The film oxidation was performed concomitantly to the glass thermal treatment carried out at 650 °C. Analysis through XPS depth profile indicates the formation of a chemically graded high entropy interlayer due to the interdiffusion of atoms from substrate to film and vice-versa, during the thermal treatment. The high entropy interface layer contributes to reduces the mismatch between the film and the substrate lattice, resulting in an improvement of film adhesion. The badgap analysis through Tauc method show two energy values, namely 3.2 eV and 2.9 eV, which can be attributed to TiO2-rutile layer and the high entropy zone at interface, composed by [Ca-Na-Si-Ti]Ox oxides. The wettability results show that the contact angle may be as low as 10° between a deionized water drop and the rutile-TiO2 surface, after activation with UV light irradiation, which is characteristic of super-hydrophilic surface.

Duplex treatment on AISI D2 tool steel: plasma nitriding and reactive deposition of TiN and TiAlN films via magnetron sputtering

In this work, titanium nitride (TiN) and titanium aluminum nitride (TiAIN) films have been obtained via triode magnetron sputtering. The films were deposited using a direct current source on plasma nitrided AISI D2 tool steel (duplex treatment), non-nitrided steel, and silicon. The nitrided layer was characterized by scanning electron microscopy (SEM), Vickers microhardness, and X-ray diffraction (XRD). The films were characterized by SEM and XRD. The mechanical properties of the coatings were determined using the instrumented indentation technique (IIT) and the adhesion of the film to the substrate was qualitatively evaluated using the Rockwell C test. Both films presented no significant variation in hardness (H) and elastic modulus (E). However, compared to the films obtained in non-nitrided steel, the duplex treatment improvided the film-substrate adhesion. The improvement in adhesion can be attributed to the preliminary plasma nitriding treatment and the compressive loads acting on the nitrided surface.

Influence of substrate stiffness and of PVD parameters on the microstructure and tension fracture characteristics of TiN thin films

Titanium nitride is widely used as wear resistant coating thin films in industrial parts. Mechanically they correspond to nanometric 2D ceramic systems which are bound to a much thicker metallic substrate. Under uniaxial tension these films respond by forming a periodic array of cracks. The separation between the cracks is primarily defined by the strength and stiffness of the film. Secondary factors, as the elastic properties of the substrate, or the microstructure and/or induction of residual stresses during processing may also have and effect. In the present work PVD TiN films were deposited by triode magnetron sputtering in Brass and Aluminum substrates. The deposition characteristics of the films were varied by changing the bias potential and the nitrogen supply during deposition (constant or variable). Tension fractures were observed in situ using a traveling microscope and under nanoindentation/scratching tests. Energy Filtered TEM was used to access the nitrogen levels across film thickness. The results were correlated with the film residual stress levels obtained in the different deposition conditions.

The effect of annealing on the structural, optical and electrical properties of Titanium Nitride (TiN) thin films prepared by DC magnetron sputtering with supported discharge

Nano-crystalline Titanium Nitride (TiN) thin films were deposited on glass substrates by reactive DC magnetron sputtering in the presence of a supported discharge (dc triode magnetron sputtering). A hot thermionic filament which was negatively biased is kept between the target and substrate, and was used to sustain the discharge at much lower pressures. The TiN films deposited at room temperature (RT) were annealed at different temperatures of 373, 473 and 573 K in a high vacuum for 1 h. The films were characterized for their morphological, structural, micro-structural, optical and electrical properties. RT deposited titanium to nitrogen ratio was found to be 1:1 which has been confirmed by EDAX. XRD studies showed that the as-deposited TiN thin film were amorphous in nature and transformed to a nano-crystalline structure with increasing annealing temperatures. The crystallite growth of TiN thin films started around 373 K onwards, and it became a face-centered cubic structure with a preferred orientation along the (111) plane. The band gap of TiN thin films was found to increase from 2.7 to 3.2 eV with an increase in the annealing temperature. The photoluminescence spectrum of TiN thin films indicates a broadening of emission wavelength in the visible region with a maximum emission peak around 360 nm. The electrical resistivity of TiN thin films was found to drop significantly from 1800 to 400 µΩ cm with an increase in the annealing temperature. The AFM micrographs of annealed TiN thin films show uniform surface pattern associated with a large accumulation of fine grains. Through this work, it has been demonstrated that it is possible to achieve the required physical properties of TiN films at lower annealing temperatures by the supported discharge dc magnetron technique compared to other sputtering techniques.

Behavior of coated forming tools with TiAlN coatings grown by Triode Magnetron Sputtering

This research focusses on tribological analysis of Titanium Aluminum Nitride (TiAlN) coatings deposited by means of Triode Magnetron Sputtering, when used as a protective coating on forming tools. The analysis is carried out from the microstructural properties which directly influence the tribological behavior. It was observed that the predominant wear mechanisms on the surface are delamination and tribo-oxidation; an increase in the useful life of the tool was observed making hard coatings an excellent alternative in the metalworking industry.

Bias voltage influence on the mechanical and tribological properties of titaniumaluminum nitride coatings produced by triode magnetron sputtering

TixAl1-xN coatings were grown using the triode magnetron sputtering technique with various bias voltages between -40 V and -150 V. As the bias voltage increased, an increase in the Al atomic percentage was observed, presenting a competition with Ti and producing structural changes. Moreover, the grain size and roughness were also strongly influenced by the bias voltage. It was observed that coatings with concentrations of approximately 25% Al and 75% Ti exhibited an optimum mixture of mechanical and tribological properties. The average coefÞcient of friction was low for the TiAlN coating that was grown at -40 V. Additionally, the critical load was obtained by measuring the adhesion using the scratch test.

Structural and Morphological Properties of Titanium Aluminum Nitride Coatings Produced by Triode Magnetron Sputtering

Tix Al1−xN coatings were grown using the triode magnetron sputtering technique varying the bias voltage between -40 V and -150V. The influence of bias voltage on structural and morphological properties was analyzed by means of energy dispersive spectroscopy, x-ray diffraction and atomic force microscopy techniques. As the bias voltage increased, an increase inthe Al atomic percentage was observed competing with Ti and producing structural changes. At low Al concentrations, the film presented a FCC crystalline structure; nevertheless, as Al was increased, the structure pre-sented a mix of FCC and HCP phases. On the other hand, an increase inbias voltage produced a decrease films thickness due to an increase in colli-sions. Moreover, the grain size and roughness were also strongly influencedby bias voltage.

Structural and Mechanical Characterization of Duplex Multilayer Coatings Deposited onto H13 Tool Steel

Quenched and tempered H13 tool steel was plasma nitrided and Physical Vapour Deposition (PVD) coated in a hybrid reactor aiming to obtain a TiN/TiC multilayer coating deposited on a plasma nitrided substrate, with a more gentle transition of elastic-plastic properties between the outermost layer of the coating and the substrate. Duplex treatment (plasma nitriding and PVD coating) was carried out in a hybrid reactor. Plasma nitriding preceded the DC triode magnetron sputtering PVD process, conducted inside the same chamber, using CH 4 and N 2 as reactive gases. Multilayer TiN/TiC coatings deposited on a nitrided H13 substrate were obtained. The multilayer coating was composed by a first Ti interlayer to grant adhesion, followed by a second 18.4 at% C TiC layer with a cF8 NaCl type unit cell, then a 41.9 at% N TiN layer and finally an outermost 32.3 at% C TiC layer with the same cF8 NaCl type unit cell. The multilayer coating showed a gentle transition of elastic-plastic properties assessed by the H/E * and the H 3 /E *2 ratios and the elastic recovery as a function of the distance from the surface of the specimen. The adhesion of the multilayered coating to the substrate was greater in the case of the duplex coated specimen as compared to the non duplex treated H13 steel.

Epitaxial Ni3FeN thin films: A candidate for spintronic devices and magnetic sensors

A new type of epitaxial ferromagnetic nitride (Ni3 Fe N = permalloy nitride = “PyN”) compound films were grown on Al2O3(112¯0) substrates using reactive triode magnetron sputtering. The results of electron back-scattering diffraction and x-ray diffraction techniques indicate a high quality epitaxial crystalline structure with growth normal of (100). Magnetization measurements of epitaxial PyN films revealed several unique results. (1) A textbook square hysteresis loop that suggest existence of single magnetic domain in these films. (2) A coercive field is tunable from a few mOe up to a few Oe by changing the film thickness. (3) A magnetization that switches (rotate) over a very small field range of δHC ≤ 0.05 Oe, independent of the film thickness. This small δH indicates a very large resistive sensitivity (δR/δH) of the epitaxial PyN. (4) The epitaxial PyN thermal cycling through several cycles between “2 and 800 K” (−271 °C to +527 °C) shows much less degradation only about 2–5% compared to 40% degradation of a simple Py film. Four-probe transport measurements give an anisotropic magnetoresistance of ≈6%, sufficiently higher than other known ferromagnetic materials. These interesting properties are ideal for a variety of spintronic devices and magnetic sensors.

Modeling reactive sputter deposition of titanium nitride in a triode magnetron sputtering system

In this paper, the so-called Berg's model was successfully employed in order to model the reactive sputter deposition of titanium nitride (TiN) by a triode magnetron sputtering (TMS) system. Such system consists of a grounded grid introduced between the target and the substrate. The grid acts as the anode, and the glow discharge is formed between the target and grid. The qualitative model was compared to experimental data. In addition, results from a conventional MS system were also compared to the ones from the modified TMS system. It was possible to observe that (a) the width of the hysteresis region is narrower for TMS for all modeled conditions; (b) the hysteresis width increases as a function of grid-to-target distance.

Effect of oxygen concentration and system geometry on the current–voltage relations during reactive sputter deposition of titanium dioxide thin films

Current–voltage relations at different magnetron sputtering systems and gas mixtures were studied during reactive sputter deposition of titanium dioxide thin films. The main goal of this work was to investigate the influence of reactive gas mixture (Ar + O 2) and system geometry on the electrical characteristics of the discharge. The geometries utilized were the conventional magnetron sputtering, hollow cathode magnetron sputtering and triode magnetron sputtering. A change in the system geometry leads to a change in the electric field distribution, which alters the working range of the discharge voltage and magnetron efficiency. It is noticed that the discharge voltage at constant current can be reduced when the geometry is altered from conventional magnetron to hollow cathode magnetron or triode magnetron, at the same time the magnetron efficiency is increased when hollow cathode magnetron or triode magnetron are used instead of conventional magnetron sputtering.

TiAlN coatings deposited by triode magnetron sputtering varying the bias voltage

TiAlN films were deposited on AISI O1 tool steel using a triode magnetron sputtering system. The bias voltage effect on the composition, thickness, crystallography, microstructure, hardness and adhesion strength was investigated. The coatings thickness and elemental composition analyses were carried out using scanning electron microscopy (SEM) together with energy dispersive X-ray (EDS). The re-sputtering effect due to the high-energy ions bombardment on the film surface influenced the coatings thickness. The films crystallography was investigated using X-ray diffraction characterization. The X-ray diffraction (XRD) data show that TiAlN coatings were crystallized in the cubic NaCl B1 structure, with orientations in the {1 1 1}, {2 0 0} {2 2 0} and {3 1 1} crystallographic planes. The surface morphology (roughness and grain size) of TiAlN coatings was investigated by atomic force microscopy (AFM). By increasing the substrate bias voltage from −40 to −150 V, hardness decreased from 32 GPa to 19 GPa. Scratch tester was used for measuring the critical loads and for measuring the adhesion.

Radar absorbing materials based on titanium thin film obtained by sputtering technique

Titanium thin films with nanometer thicknesses were deposited on polyethylene terephthalate (PET) substrate using the triode magnetron sputtering technique. It was observed that the titanium thin film-polymeric substrate set attenuates the energy of the incident electromagnetic wave in the frequency range of 8 to 12 GHz. This result allows to consider this set as a radar absorbing material, which may be employed in automobile, telecommunication, aerospace, medical, and electroelectronic areas. Results of the reflectivity show that the attenuation depends on the thin film thickness, as a determining factor. Thin films with 25 to 100 nm thickness values show attenuation of the electromagnetic wave energy from around 20 to 50%. Analyses by Rutherford backscattering spectrometry provided information about the thickness of the thin films studied. Hall effect analyses contributed to better understand the influence of the thin film thickness on the electron mobility and consequently on absorption properties.

Control of the substrate temperature using a triode magnetron sputtering system

The bombardment of ions and electrons at the substrate has been studied by varying the magnetic field distribution and the grid-target distance in a triode magnetron sputtering system. The substrate temperature was correlated with the substrate current density and with the type of species bombarding the substrate. The results indicate a possibility to modify and control the bombardment at the substrate surface from predominantly electronic to predominantly ionic, which increases the substrate temperature from 383 K to 473 K, respectively.

Influence of electromagnetic confinement on the characteristics of a triode magnetron sputtering system

Three different configurations of magnetic traps were set up by changing the number of central magnets in a Triode Magnetron Sputtering system, where the anode consists of a grid positioned at a distance from an aluminum target on the cathode. The grid and the wall chamber are grounded and the plasma is formed in the space between the target and the grid. The current–voltage ( I– V) characteristics of argon discharges were obtained, for each magnetic configuration and for various grid–target distances. It is noticed that the magnetron efficiency strongly depends on the inter-electrode distance and magnetic trap configuration. The configuration with the highest unbalance coefficient has I– V curves that differ substantially from the usual relation observed in conventional magnetron discharges. In this case the usual I– V fitting curves of magnetron mode of operation are not appropriate to describe the electrical characteristics of the discharge.

Structural characterization of Fe–C coatings prepared by reactive triode-magnetron sputtering

Fe1–xCx coatings were synthesized by triode magnetron sputtering of an iron target in a methane/argon atmosphere with a large range of composition (x = 0.3 to 0.6 ± 0.06). Film surfaces were characterized by grazing incidence x-ray diffraction, scanning and transmission electron microscopies, and electron energy loss spectroscopy, to study effects of the variation of the methane gas flow rate on their structural properties. The coatings were constituted of the ε-Fe3C carbide (x = 0.3 and 0.36), in which carbon atoms are in octahedral sites, and of nanocomposite structure constituted of disordered and crystalline carbide nanograins embedded in a carbon matrix made of an amorphous and poorly crystallized graphenelike material (x = 0.55 and 0.60). In situ annealing of the nanocomposite Fe0.45C0.55 coating led to the formation of carbides θ-Fe3C and Fe7C3 (with carbon atoms in prismatic sites) and C-rich cubic carbide possibly related to the τ2-Fe2C7 compound.

Residual stresses in titanium nitride thin films obtained with step variation of substrate bias voltage during deposition

In this work, a series of depositions of titanium nitride (TiN) films on M2 and D2 steel substrates were conducted in a Triode Magnetron Sputtering chamber. The temperature; gas flow and pressure were kept constant during each run. The substrate bias was either decreased or increased in a sequence of steps. Residual stress measurements were later conducted through the grazing X-ray diffraction method. Different incident angles were used in order to change the penetration depth and to obtain values of residual stress at different film depths. A model described by Dolle was adapted as an attempt to calculate the values of residual stress at each incident angle as a function of the value from each individual layer. Stress results indicated that the decrease in bias voltage during the deposition has produced compressive residual stress gradients through the film thickness. On the other hand, much less pronounced gradients were found in one of the films deposited with increasing bias voltage.

Energy dissipation in depth-sensing indentation as a characteristic of the nanoscratch behavior of coatings

Wear behavior of coatings has usually been described in terms of mechanical properties such as hardness ( H) and effective elastic modulus ( E*). Alternatively, an energy approach appears as a promising analysis taking into account the influence of those properties. In a nanoindentation test, the dissipated energy depends not only on the hardness and elastic modulus, but also on the elastic recovery ( W e ). This work aims to establish a relation between plastic deformation energy ( E p ) during depth-sensing indentation method and the grooving resistance of coatings in nanoscratch tests. An energy dissipation coefficient ( K d ) was defined, calculated as the ratio of the plastic to the total deformation energy ( E p / E t ), which represents the energy dissipation of materials. Reactive depositions using titanium as the target and nitrogen and methane as reactive gases were obtained by triode magnetron sputtering, in order to assess wear and nanoindentation data. A topographical, chemical and microstructural characterization has been conducted using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), wave dispersion spectroscopy (WDS), scanning electron (SEM) and atomic force microscopy (AFM) techniques. Nanoscratch results showed that the groove depth was well correlated to the energy dissipation coefficient of the coatings. On the other hand, a reduction in the coefficient was found when the elastic recovery was increased.

Deposition of CrN coatings by PVD methods for mechanical application

CrN is an excellent wear and corrosion resistant material. There is much interest in the research community to develop CrN thin films for coating tools for metal and wood machining operations. The present study aims to develop CrN coatings for wear applications. The films were deposited by triode sputtering, magnetron sputtering and ion beam assisted deposition (IBAD) methods. Structural, chemical and mechanical characterization of the films was performed. For a better understanding, films deposited by sputtering and IBAD methods are compared. Structure and properties (especially residual stress) of the films, and aspects of film growth processes and their effects on film properties are discussed.