Browsing by Author "Cavaleiro, Albano"
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- Can ZrAlN thin films be used as thermistor sensors for temperature assessment?Publication . Martins, Bruno; Patacas, Carlos; Cavaleiro, Albano; Faia, Pedro; Bondarchuk, Oleksandr; Fernandes, FilipeThe electrical characteristics and conduction mechanisms of ZrAlN thin films for their potential use as thermistor sensors were assessed. Various compositions of Zr1-xAlxN were synthesized by sputtering and studied up to 200 °C to understand their sensitivity and applicability. Among the compositions studied, the ones with x = 0.34 and x = 0.46 showed the highest sensitivities, reaching values close to 3000 K. However, the thermo-resistive properties exhibited by these compositions limited their utilization above 100 °C. Zr1-xAlxN film compositions with x higher than 0.46 showed amorphous structures and were found to be insulative. Composition with x = 0.26, within the cubic phase, showed the most promising electrical properties regarding temperature sensing in the studied range. XPS analysis of this composition confirmed the presence of Zr-N and Al-N bonds, with a Zr3+ oxidation state, which suggests the availability of a free electron contributing to the electrical conduction. Impedance measurements performed at different temperatures for this composition revealed the dominant role of the grain boundaries in the conduction mechanism, based upon electron hopping between grains, overcoming the energy barrier imposed by the grain boundaries. ZrAlN thin films demonstrate negative temperature coefficient (NTC) thermistor behavior, expanding their applications beyond protective coatings to temperature monitoring.
- Deciphering the mechanical strengthening mechanism: Soft metal doping in ceramic matrices: A case study of TiN-Ag filmsPublication . Luan, Jing; Kong, Fanlin; Xu, Junhua; Fernandes, Filipe; Evaristo, Manuel; Dong, Songtao; Cavaleiro, Albano; Ju, Hongbo; Fernandes, FilipeSoft metals have been widely added into ceramic-based films for fully meeting the demanding requirements of green tribological applications. However, the resulting considerable increase of the mechanical strength by adding a soft metal below 5 at.%, which reversed the rule-of-mixture, was still not fully revealed. In this paper, a case study of TiN-Ag films was carried out to investigate the strengthening mechanism induced by adding soft metal in TiN-Ag composite/multilayered films deposited by magnetron sputtering. The results showed that dual-phases of fcc-TiN and fcc-Ag co-existed in the composite films with the Ag particles embedded in the matrix. In some areas of the Ag particles, with a size below 4 nm, epitaxial growth with the TiN template was detected, which obliged the lattice to be distorted and shrunken. Consequently, both hardness and elastic modulus were enhanced from 21 and 236 GPa, for the reference TiN film, to 26 and 323 GPa for the TiN-Ag composite film with 2.4 at.% Ag. The possibility of having the epitaxial growth of Ag within TiN were also confirmed by designing a TiN/Ag multilayered film with an Ag layer thickness of ∼3 nm.
- Design and magnetron sputtering of nanomultilayered W2N/Ag-SiNx films: Microstructural insights and optimized self-lubricant properties from room temperature to 500 ◦CPublication . Luan, Jing; Kong, Fanlin; Evaristo, Manuel; Fernandes, Filipe; Zhou, Yazhou; Cavaleiro, Albano; Ju, Hongbo; Fernandes, FilipeNovel multilayered films were engineered by integrating W2N and Ag-SiNx layers in a multilayer structure to obtain improved hardness and tribological properties. The films were fabricated by alternating magnetron sputtering, depositing 40 nm layers of W2N with varying thickness of Ag-SiNx layers varying in thickness from 4 to 20 nm. The effect of the increase thickness of the Ag-SiNx layers in the films microstructure and tribological properties were accessed. Tribological experiments were conducted at room temperature (RT), 500 °C, and RT-500 °C cycling conditions. The results revealed the production of a multilayered structure comprising single fcc-W2N layers interspersed with dual-phase layers consisting of fcc-Ag and amorphous SiNx phases. Tribological results indicated an improvement in the tribological performance with increase thickness of the Ag-SiNx layer up to 12 nm. The tribo-synergistic/combined action of both W2N and Ag-SiNx layers, along with the presence of layered lubricant tribo-phases of WO3 and Ag2WO4, showcased the pivot role in reducing friction and enhancing wear resistance. The optimized multilayered film, featuring a 12 nm Ag-SiNx layer, demonstrated exceptional tribological properties under temperature-cycling from RT to 500 °C.
- Effect of Annealing Heat Treatment on the Composition, Morphology, Structure and Mechanical Properties of the W-S-N CoatingsPublication . Yaqub, Talha Bin; Al-Rjoub, Abbas; Khalid, Hafiza Ayesha; Yaqoob, Khurram; Fernandes, Filipe; Cavaleiro, AlbanoAlloyed-transition metal dichalcogenide (TMD) coatings have been under investigation as multi-environment lubricants for the past few decades. These coatings display very low coefficient of friction properties at elevated temperatures. Studies on the annealing of these low-friction coatings are missing in the literature. For the first time, in this study, the annealing of the W-S-N dry lubricant coatings was carried out to study its effects on the composition, morphology, crystal structure and hardness of the coatings. The W-S-N coatings were deposited by direct current (DC) reactive magnetron sputtering. The analysis was carried out for as-deposited, 200 °C and 400 °C annealed coatings. The as-deposited coatings have N content in the range of 0–25.5 at. %. The coatings are compact and the densification increased with the increase in N-alloying. All the coatings are crystalline except the highest N-alloyed coating which is X-ray amorphous. A maximum hardness of 8.0 GPa was measured for the coating alloyed with 23 at. % N. Annealing did not affect the composition and morphology of the coatings, while some variations were observed in their crystal structure and hardness. The maximum hardness increased from 8 GPa to 9.2 GPa after 400 °C annealing of the 23 at. % N-alloyed coating.
- Electrical properties and thermistor behavior of TiAlN thin films deposited by combinatorial sputteringPublication . Martins, Bruno; Patacas, Carlos; Cavaleiro, Albano; Faia, Pedro; Bondarchuk, Oleksandr; Fernandes, FilipeA combinatorial deposition was performed by direct current magnetron sputtering (DCMS) to develop Ti1-xAlxN thin films with different Ti/Al ratios and investigate the electrical response to temperature. The crystal structure as a function of the x was studied by X-ray diffraction, and sheet resistance response was measured up to 200 ◦C. From x = 0.16 to x = 0.56, the film shows an fcc phase with Al in solid solution in the TiN matrix, whilst, from x ≥ 0.69, a mixture of hcp (AlN) and fcc phases is observed. A negative temperature coefficient (NTC) thermistor behavior was found from x = 0.21 onwards, and a maximum sensitivity β of 1600 K was observed for x = 0.56 and 0.69. One fcc sample (x = 0.46) was selected to analyze the chemical states by X-ray photoelectron spectroscopy and the impedance behavior with the temperature by electrical impedance spectroscopy. The crystal structure, bond states and impedance analysis were compared with an AlN thin film. It is concluded that the conduction mechanism for x = 0.46 is based upon electron hopping, and the effect of the grain boundary is more relevant than the grain at low temperatures. We demonstrate that it is possible to use TiAlN as an NTC-thermistor with different crystal structures and chemical compositions.
- Expanding the applications of the wear-resistant titanium aluminum nitride thin-film to include temperature sensingPublication . Martins, Bruno; Patacas, Carlos; Cavaleiro, Albano; Faia, Pedro; Zorro, Fátima; Carbo-Argibay, Enrique; FGerreira, Paulo J.; Fernandes, Filipe; Fernandes, FilipeThis study investigates an approach to temperature sensing by integrating Titanium Aluminum Nitride (TiAlN), originally engineered for wear and corrosion applications, as a temperature sensor within a multilayered thin film system. A nitride multilayer system was developed by physical vapor deposition (PVD) using a single four-target magnetron sputtering chamber; intermediate vacuum interruption steps were employed for masking procedures. The multilayer architecture design aimed to provide the sensor layer with mechanical protection and electrical shielding. Structural and electrical characterization of the TiAlN single layer revealed semiconductor behavior and stable electrical resistance up to 750 °C, with minimal signal stabilization requirements. Despite the higher Al content, the TiAlN temperature sensor exhibited a cubic crystal structure characterized by diffuse nanolayers, resulting from a two-fold rotational deposition and target configuration. A detailed examination of the multilayer system cross-section containing the TiAlN sensor was conducted using scanning transmission electron microscopy (STEM). The analysis revealed its columnar morphology with the presence of typical PVD growth defects, including voids and droplets. While the presence of these defects may impact the electrical characteristics of the sensor, the selected experimental conditions effectively maintained the structural integrity of the multilayer system despite the vacuum interruptions caused by masking procedures. Validation experiments confirmed the functionality of the multilayer system for temperature measurements up to 400 °C. The signal acquisition system addressed room temperature resistance variations and low sensitivity (thermistor coefficient ∼100 K), resulting in a measured error of approximately 6%. This study demonstrates promising results of TiAlN as a temperature sensor within a multilayered system, expanding its range of potential applications.
- Exploring tribological characteristics of ZrN-MoSN composite films fabricated via RF magnetron sputtering: Insights from microstructure and performance analysisPublication . Luan, Jing; Lu, Hongying; Xu, Junhua; Fernandes, Filipe; Fernandes, Filipe; Evaristo, Manuel; Ma, Bingyang; Xie, Fuxiang; Cavaleiro, Albano; Ju, HongboAchieving the stringent demands of sustainable tribological industrial applications poses a significant challenge, particular in optimizing the self-lubricant performance of nitride-based films. This paper tackled this challenge by designing and depositing a series of ZrN-MoSN composite films with varying (Mo + S)/Zr ratios, employing RF magnetron sputtering, aimed to enhance the tribological properties through utilizing the high loading capacity of the ZrN matrix and the exceptional self-lubricating attributes of Mo-S-N additives. After conducting thorough investigations on the microstructure, and tribological properties, the results revealed that the dense columnar structured ZrN-MoSN composite films displayed a polycrystalline composition comprising fcc-ZrN and hcp-MoS2 phases, intertwined with amorphous phases of Mo(SN)x and MoS2(N2). (Mo + S)/Zr ratios below 1.08 exhibited a minor impact on the room temperature (RT) tribological properties, while higher ratios led to degradation on RT average friction coefficient (COF) and wear rate (WR). However, the synergistic effect of ZrN matrix and the tribo-phases of layered MoO3 and hard ZrO2 contributed to the significant enhanced 500 °C tribological properties, particularly with an optimized (Mo + S)/Zr ratio of 0.43.
- Influence of the alloying elements on the tribological performance of DLC coatings in different sliding conditionsPublication . Evaristo, Manuel; Fernandes, Filipe; Cavaleiro, AlbanoReduction of friction and wear at the sliding surfaces are the main concern in several applications. From an extensive list of low friction hard coatings, DLC type is one of the most studied and develop for achieving low wear and friction. The addition of an alloying element is extensively used, since it can change significantly the coatings performance. Therefore, in this research the tribological behaviour of DLC coatings alloyed with different elements was evaluated, since no works comparing the tribological properties of DLC films with approximately the same alloying elements concentration are reported in the literature. The coatings were deposited by physical vapor deposition and alloyed with: tungsten (W), silver (Ag), silicon (Si), silicon and oxygen (SiO), with concentrations of metallic elements between 10 and 15 at. % and a pure DLC coating was also deposited for comparison purposes. The coatings hardness varied between 23 GPa for the pure DLC and 11 GPa for the alloyed with Si and O. The tribological behaviour of the coatings was evaluated by pin-on-disk against 10 mm 100Cr6 steel balls, at room temperature (RT) and 100 ◦C. The best wear resistance was achieved with the pure DLC and DLC-W for RT tests. At RT the lowest friction was obtained with the DLCSi and DLCSiO coatings. Despite of the low COF values, those coatings displayed the highest specific wear rate values among all the films. This is attributed to the presence of hard SiC particles stick at the ball counterpart which promotes severe abrasion of the coatings surface. The increase of the temperature to 100 ◦C increases significantly the friction coefficient for the DLC and DLC-W coatings, whilst, for DLC-Ag, DLC-Si and DLC-SiO coatings a slight decrease is noticed. At this temperature DLCAg coating is the more performing due to the formation of a tick tribolayer rich in Ag adhered at the counterpart surface. With this work it was concluded that friction and wear are not directly related, and the third bodies formed on the sliding surfaces have major influence on the tribological performance of the system.
- Insights into the oxidation resistance mechanism and tribological behaviors of multilayered TiSiN/CrVxN hard coatingsPublication . Ju, Hongbo; Athmani, Moussa; Luan, Jing; AL-Rjoub, Abbas; Cavaleiro, Albano; Yaqub, Talha Bin; Chala, Abdelouahad; Ferreira, Fabio; Fernandes, FilipeIn the last decades, vanadium alloyed coatings have been introduced as potential candidates for self-lubrication due to their perfect tribological properties. In this work, the influence of V incorporation on the wear performance and oxidation resistance of TiSiN/CrN film coatings deposited by direct current (DC) reactive magnetron sputtering is investigated. The results show that vanadium incorporation significantly decreases the oxidation resistance of the coatings. In general, two layers are formed during the oxidation process: i) Ti(V)O2 on top, followed by a protective layer, which is subdivided into two layers, Cr2O3 and Si–O. ii) The diffusion of V controls the oxidation of V-containing coatings. The addition of vanadium improves the wear resistance of coatings, and the wear rate decreases with increasing V content in the coatings; however, the friction coefficient is independent of the chemical composition of the coatings. The wear of the V-containing coatings is driven by polishing wear.
- Nano-multilayered ZrN‒Ag/Mo‒S‒N film design for stable anti-frictional performance at a wide range of temperaturesPublication . Ju, Hongbo; Luan, Jing; Xu, Junhua; Cavaleiro, Albano; Evaristo, Manuel; Fernandes, Filipe; Fernandes, FilipeA multilayer film, composed by ZrN-Ag (20 nm) and Mo-S-N (10 nm) layers, combining the intrinsic lubricant characteristics of each layer was deposited using DC magnetron sputtering system, to promote lubrication in a wide-range of temperatures. The results showed that the ZrN-Ag/Mo-S-N multilayer film exhibited a sharp interface between the different layers. A face-centered cubic (fcc) dual-phases of ZrN and Ag co-existed in the ZrN-Ag layers, whilst the Mo-S-N layers displayed a mixture of hexagonal close-packed MoS2 (hcp-MoS2) nano-particles and an amorphous phase. The multilayer film exhibited excellent room temperature (RT) triblogical behavior, as compared to the individual monolayer film, due to the combination of a relative high hardness with the low friction properties of both layers. The reorientation of MoS2 parallel to the sliding direction also contributed to the enhanced anti-frictional performance at RT. At 400 °C, the reorientation of MoS2 as well as the formation of MoO3 phase were responsible for the lubrication, whilst the hard t-ZrO2 phase promoted abrasion and, consequently, led to increasing wear rate. At 600 °C, the Ag2MoO4 double-metal oxide was the responsible for the low friction and wear-resistance; furthermore, the observed transformation from t-ZrO2 to m-ZrO2, could also have contributed to the better tribological performance.