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2018


Grain-boundary diffusion coefficient in alpha-Al2O3 from spark plasma sintering tests: Evidence of collective motion of charge disconnections


Tamura, Y; Zapata-Solvas, E; Moshtaghioun, BM; Gomez-Garcia, D; Dominguez-Rodriguez, A
Ceramics International, 44 (2018) 19044-19048

ABSTRACT

The sintering of fine-grained a-alumina by spark plasma sintering (SPS) was performed to study grain growth under SPS conditions. Grain growth is found to be extensive at relative densities above 95%. A grain growth versus dwell time analysis during SPS allows for the determination of the grain-boundary diffusion coefficient. This study shows that the remarkable enhancement of grain-boundary diffusion derived from a previous analysis could be a consequence of the presence of the recently discovered "disconnections" at the grain boundaries of alpha-alumina. Their presence, together with their electric charge and the external electric field at the boundaries, are the key ingredients for a violation of the typical grain growth kinetic law. When they are introduced appropriately, an updated value of the grain-boundary diffusion coefficient is achieved. A comparison with other values reported previously in the literature through other techniques and a critical analysis are also carried out.


Octubre, 2018 | DOI: 10.1016/j.ceramint.2018.07.073

High-temperature oxidation of CrAlYN coatings: Implications of the presence of Y and type of steel


Rojas, TC; Dominguez-Meister, S; Brizuela, M; Sanchez-Lopez, JC
Surface & Coatings Technology, 354 (2018) 203-2013

ABSTRACT

Nanolayered CrAIN and CrAIYN/CrAIN (average contents of Al approximate to 25 at.% and Y approximate to 1.6 at. %) coatings are deposited on M2 and 316 steel substrates and heated to 1000 degrees C in air for 2 h to study their oxidation mechanism, the thermal stability and the reactive element (RE) effect of yttrium. CrAIN on M2 develops a Cr2O3/Al2O3 passivation layer that preserves in high degree the fcc-CrAIN structure however iron ions leave the substrate and travel to the surface along the column boundaries. The CrAIYN/CrAIN coatings deposited on steels are not stable at 1000 degrees C, and the initial fcc-CrAIN phase is partially transformed to hcp-Al(O)N and Cr-Fe phases (M2) and Cr2N and Al2O3 (316). The addition of Y changes the predominant scale growth direction. Inward oxygen diffusion becomes dominant but a reduction of the oxide scale thickness as compared to CrAIN is not observed. The advanced microstructural analysis made by transmission electron microscopy combined with electron energy loss spectroscopy determined that yttrium migrates mainly to the oxide scale (forming mixed oxides with substrate elements - V and Mo, either as dispersed particles or segregated at the grain boundaries) in M2, and to the oxide interface and column boundaries (forming Al-Y oxides and YN, respectively) in 316 steel. The benefits of addition of Y in improving the oxidation resistance are discussed comparatively with literature data. The RE effect of yttrium is thus observed to be dependent on the substrate, film architecture and composition.


Octubre, 2018 | DOI: 10.1016/j.surfcoat.2018.09.020

Photocatalytic H2 production from glycerol aqueous solutions over fluorinated Pt-TiO2 with high {001} facet exposure


V. Vaiano; M.A. Lara; G. Iervolino; M. Matarangolo; J.A. Navío; M.C. Hidalgo
Journal of Photochemistry and Photobiology A-Chemistry, 365 (2018) 52-59

ABSTRACT

An optimized fluorinated TiO2 catalyst with high {001} facet exposure loaded with platinum (TiO2-PtFAC) was tested in the photocatalytic hydrogen production from glycerol solution under UV light irradiation. The samples were synthesized by direct hydrothermal treatment starting from two different types of precursors that are titanium tetraisopropoxide (I) or titanium butoxide (B), while platinisation was performed by photodeposition method. The obtained catalysts were characterised by different techniques (XRD, FESEM, TEM, BET, UV–vis DRS, XRF and XPS) and the results evidenced that anatase is the only crystalline phase present in all TiO2 samples. The morphology of the samples was seen as rectangular platelets particles where Pt particles were was observed all over the surface. The presence of Pt and F in the platinised samples was also confirmed by XRF and XPS analysis. The photocatalytic results have shown that the presence of Pt on TiO2{001}facet surface remarkably enhanced the hydrogen production from aqueous solution at 5 wt % of glycerol. Comparing the results obtained from the photocatalysts prepared by the two different precursors, it was found that the best performances in terms of H2 production was achieved with TiO2-PtFAC(I) (about 13 mmol L−1 after 4 h of irradiation time), while the H2 production was lower for TiO2-PtFAC(B) (about 9 mmol L−1 after 4 h of irradiation time). The effect of the operating conditions using TiO2-PtFAC(I) evidenced that the highest H2 production was obtained with a photocatalyst dosage equal to 1.5 g L−1, initial glycerol concentration at 5 wt% and a pH value equal to 7. Finally, a photocatalytic test was also performed on glycerol solution prepared with a real water matrix. Despite the presence of ions scavengers (chlorides and carbonates) in solution, TiO2-PtFAC(I) was able to reach a photocatalytic H2production of about 6 mmol L−1 after 4 h of UV light irradiation.


Octubre, 2018 | DOI: 10.1016/j.jphotochem.2018.07.032

Biomass fly ash and aluminium industry slags-based geopolymers


Perez-Villarejo, L; Bonet-Martinez, E; Eliche-Quesada, D; Sanchez-Soto, PJ; Rincon-Lopez, JM; Castro-Galiano, E
Materials Letters, 229 (2018) 6-12

ABSTRACT

Geopolymers are a new class of non-Portland cements produced using an alumino-silicate material and an activating solution, which is mainly composed of sodium or potassium and waterglass to be subsequently cured at relatively low temperatures. Those can be formulated by adding natural minerals, waste and/or industrial by-products. The study investigates the microstructural properties of geopolymers synthesized from metakaolin (MK) and the admixture of fly ash (FBA) and aluminium industry slags (AIS) at different ages of curing. Five different geopolymer compositions were prepared and characterized by XRD, ATR-FTIR and SEM/EDS. The study revealed that geopolymeric gels are identified, which show mainly glassy microstructures, in agreement with the X-ray amorphous diffraction patterns, broad FTIR features and confirmed by SEM/EDS, with promising results prior to an industrial scale.


Octubre, 2018 | DOI: 10.1016/j.matlet.2018.06.100

Manufacture of sustainable clay ceramic composite with composition SiO2-Al2O3-CaO-K2O materials valuing biomass ash from olive pomace


Bonet-Martinez, E; Perez-Villarejo, L; Eliche-Quesada, D; Sanchez-Soto, PJ; Carrasco-Hurtado, B; Castro-Galiano, E
Materials Letters, 229 (2018) 21-25

ABSTRACT

Fly ash is a biomass combustion by-product produced by dragging ash from the base of the furnace. Disposing of ash is a growing economic and environmental burden. Based on physical and chemical properties, fly ash could be used in the manufacture of construction materials. This paper investigates the influence of biomass fly ash from olive pomace as additive to manufacture of clay ceramic composite materials. Fired clay brick at 950 degrees C were prepared containing between 0 and 25 wt% fly ash. Final products are studied by water absorption, bulk density, loss of ignition, linear shrinkage, compressive strength and physisorption N-2. The results reveal that the porosity of the materials increases with the level of fly ash replacement (10% up to 25 wt%) resulting in to increased water absorption and decreased compressive strength. Fired clay brick developed in this study can be used for construction materials based on criteria of the current regulations. 


Octubre, 2018 | DOI: 10.1016/j.matlet.2018.06.105

Study of the thermal decomposition of historical metal threads


Perez-Rodriguez, JL; Perez-Maqueda, R; Franquelo, ML; Duran, A
Journal of Thermal Analysis and Calorimetry, 134 (2018) 15-22

ABSTRACT

In this work, it is reported that thermal analysis techniques such as differential thermal analysis and thermogravimetric analysis are very useful for evaluating metals threads and fibres used in the manufacture of historical artifacts. Thermal analysis has been used to characterize the silk, cotton and linen employed as supports and the copper, silver and aluminium as the metallic components in the studied threads. Other organic compounds, mainly added for the conservation of the threads, have also been characterized.


Octubre, 2018 | DOI: 10.1007/s10973-017-6924-x

A direct in situ observation of water-enhanced proton conductivity of Eu-doped ZrO2: Effect on WGS reaction


Garcia-Moncada, N; Bobadilla, LF; Poyato, R; Lopez-Cartes, C; Romero-Sarria, F; Centeno, MA; Odriozola, JA
Applied Catalysis B-Environmental, 231 (2018) 343-356

ABSTRACT

Eu-doped ZrO2 solid solutions have been synthesized in order to prepare proton conductors as water-enhancer additives for the WGS reaction. Elemental characterization has been carried out revealing homogeneous dopant distribution resulting in fluorite-type solid solutions for Eu2O3 contents up to similar to 9 mol.%. Representative samples of the Eu-doped ZrO2 series have been analysed by Impedance Spectroscopy (IS) in inert, oxygen and wet conditions. The solid solution with 5 mol.% of Eu2O3 has presented the highest conductivity values for all tested conditions indicating an optimal amount of dopant. Moreover, the presence of vapour pressure results in an increment of the conductivity at temperatures lower than 300 degrees C, meanwhile at higher temperatures the conductivity is the same than that in inert conditions. To elucidate these results, in situ DRIFTS studies were carried out. These experiments evidenced the existence of water dissociation at oxygen vacancies (band at 3724 cm(-1)) as well as the presence of physisorbed water at temperatures up to similar to 300 degrees C where the band at 5248 cm(-1) characteristic of these species disappeared. These results points to a layer model where the physisorbed water interacts with surface hydroxyls generated by dissociated water that improves the proton conductivity through Grotthuss' mechanism in the RT-300 degrees C temperature range. These samples were successfully tested in WGS reaction as additive to a typical Pt-based catalyst. The presence of the mixed oxide reveals an increase of the catalyst' activity assisted by the proton conductor, since improves the water activation step.


Septiembre, 2018 | DOI: 10.1016/j.apcatb.2018.03.001

Pt/CePO4 catalysts for the WGS reaction: influence of the water-supplier role of the support on the catalytic performance


Navarro-Jaen, S; Centeno, MA; Laguna, OH; Odriozola, JA
Journal of Materials Chemistry A, 6 (2018) 17001-17010

ABSTRACT

For Pt catalysts which have demonstrated great activity for the WGS reaction, the activation of water is described as the rate-limiting step. Such limitation could be overcome through the design of supports able to supply water. In this study, the hexagonal and monoclinic phases of CePO4 have been evaluated as supports for Pt WGS catalysts. The hexagonal structure presents channels containing water, absent in the monoclinic structure. The presence of these channels in the hexagonal phase increases the interaction with the water molecules, leading to an enhancement of the WGS catalytic performance. DRIFTS results showed that dissociation of water does not occur on these supports, while calculated apparent activation energies present values similar to those reported in the literature for the dissociation of water in Pt (111). These results suggest that cerium phosphates act as water suppliers, increasing the number of available species to be dissociated on the Pt surface.


Septiembre, 2018 | DOI: 10.1039/c8ta04603d

A comprehensive and in-depth analysis of the synthesis of advanced adsorbent materials


Osuna, FJ; Cota, A; Pavon, E; Alba, MD
Journal of Cleaner Production, 194 (2018) 665-672

ABSTRACT

Na-Mica-4, a synthetic fluorophlogopite, is an attractive adsorbent. However, the synthesis at large scale demands an economically prized, feasible scalable and sustainable synthesis method, which requires a deep knowledge of the influence of each synthesis step. A set of Na-Mica-4 were synthesized by methods that had one synthesis parameter as variable. The purity, crystallinity and heteroatoms distribution were analysed thorough X-ray diffraction and nuclear magnetic resonance. The results shed a light on the main factors for the design of the final product and indicated that an environmental friendship synthesis could be possible. 


Septiembre, 2018 | DOI: 10.1016/j.jclepro.2018.05.179

Performance improvement in olive stone's combustion from a previous carbonization transformation


Gomez-Martin, A; Chacartegui, R; Ramirez-Rico, J; Martinez-Fernandez, J
Fuel, 228 (2018) 254-262

ABSTRACT

Under the framework of circular economy, agricultural wastes are an interesting carbon-based feedstock for thermal energy and power generation. Their use could extend the availability of biomass-based fuel and, at the same time, would reduce negative environmental effects. However, depending on the residues' characteristics, their direct combustion in boilers presents some challenges which could be overcome with a carbonization pretreatment. In this paper, the main mechanisms of thermochemical transformation of an abundant agricultural waste, olive stone, into biochar products via slow carbonization are analyzed, with emphasis on the effect of peak carbonization temperature. Thermogravimetric and differential scanning calorimetry analysis are used to evaluate the performance of the resulting biochars compared to raw olive stone in combustion processes and to assess the correlation between the peak carbonization temperature and compositional and fuel properties. Results show that with a prior treatment up to an optimum temperature of 800 degrees C the energy density is increased up to three times compared to the raw material. These findings suggest that carbonization of olive stones reduces the barriers to their direct use in current biomass boiler technology.


Septiembre, 2018 | DOI: 10.1016/j.fuel.2018.04.127

Nanostructural Analysis of Porous Oblique Angle Deposited (OAD) Multilayer Systems by Grazing-Incidence Small-Angle X-Ray Scattering


Oliva-Ramirez, M; Lopez-Santos, C; Yubero, F; Gonzalez-Elipe, AR
Advanced Optical Materials, 5 (2018) 1800530

ABSTRACT

This work reports a thorough characterization analysis of various porous thin film multilayers by means of grazing-incidence small-angle X-ray scattering (GISAXS). Alternated TiO2/SiO2 nanocolumnar layers deposited at oblique angles are fabricated in slanted, chiral, and zig-zag configurations by rotating azimuthally the substrate from one layer to the next. Multilayer systems formed by the stacking of 3 and 15 alternant thin films of these two oxides are morphologically characterized by scanning electron microscopy (SEM) and structurally by GISAXS. This technique has provided a means to determine various vertical and lateral correlation lengths and to assess the anisotropic electron density distribution along the structural elements existing in the multilayers. This information can be systematically used to account for the actual arrangement of nanostructural elements in multilayer systems.


Septiembre, 2018 | DOI: 10.1002/admi.201800530

Sensing and biosensing with screen printed electrodes modified with nanostructured nickel oxide thin films prepared by magnetron sputtering at oblique angles


Salazar, P; Garcia-Garcia, FJ; Gonzalez-Elipe, AR
Electrochemistry Communications, 94 (2018) 5-8

ABSTRACT

This work reports about the sensing and biosensing applications of a novel screen printed electrode (SPE) modified by nanostructured nickel oxide thin films obtained by reactive magnetron sputtering under an oblique angle configuration. Using these films as electrodes we demonstrate their ability to detect hydrogen peroxide under neutral pH conditions. Furthermore, as a proof-of-concept, NiO-modified SPEs have been developed and their cholesterol biosensing properties determined by cyclic voltammetry and chronoamperometry.


Septiembre, 2018 | DOI: 10.1016/j.elecom.2018.07.020

ZnO and Pt-ZnO photocatalysts: Characterization and photocatalytic activity assessing by means of three substrates


Jaramillo, C; Navio, J.A.; Hidalgo, M.C.; Macías, M.
Catalysis Today, 313 (2018) 12-19

ABSTRACT

ZnO nanoparticles have been previously synthesized by a facile precipitation procedure by mixing aqueous solutions of Zn(II) acetate and dissolved Na2CO3 at pH ca. 7.0 without the addition of a template. The as-prepared ZnO material was anealed at 400 °C in air for 2 h. The Pt-ZnO catalysts (0.5 or 1.0 Pt wt.%) were obtained by photochemical deposition method on the surface of the prepared ZnO sample, using hexachloroplatinic acid (H2PtCl6). It has been shown that Zn2+ is lost from the photocatalyst to the medium and a replacement of the cationic vacancies of Zn2+ by Pt4+ cations occurs during the platinization process of the ZnO samples, regardless of whether the platinum metal photodeposition process. The as-prepared catalysts were characterized by XRD, BET, FE-SEM, TEM, XPS and diffuse reflectance spectroscopy (DRS). Three different probe molecules were used to evaluate the photocatalytic properties under UV-illumination: Methyl Orange and Rhodamine B were chosen as dye substrates and Phenol as a transparent substrate. High conversion values (ca. 100%) and a total organic carbon (TOC) removal of 90–96%, were obtained over these photocatalysts after 160 min of UV illumination. In general, it was observed that the presence of Pt on ZnO affects the lattice parameters and the crystallite size. Although ZnO can completely degrade RhB, MO and Phenol totally in ca. 60 min, the process is more efficient for Pt–ZnO photocatalysts.


Septiembre, 2018 | DOI: 10.1016/j.cattod.2017.12.009

Improving the activity of gold nanoparticles for the water-gas shift reaction using TiO2-Y2O3: an example of catalyst design


Plata, JJ; Romero-Sarria, F; Suarez, JA; Marquez, AM; Laguna, OH; Odriozola, JA; Sanz, JF
Physical Chemistry Chemical Physics, 20 (2018) 22076-22083

ABSTRACT

In the last ten years, there has been an acceleration in the pace at which new catalysts for the water-gas shift reaction are designed and synthesized. Pt-based catalysts remain the best solution when only activity is considered. However, cost, operation temperature, and deactivation phenomena are important variables when these catalysts are scaled in industry. Here, a new catalyst, Au/TiO2-Y2O3, is presented as an alternative to the less selective Pt/oxide systems. Experimental and theoretical techniques are combined to design, synthesize, characterize and analyze the performance of this system. The mixed oxide demonstrates a synergistic effect, improving the activity of the catalyst not only at large-to-medium temperatures but also at low temperatures. This effect is related to the homogeneous dispersion of the vacancies that act both as nucleation centers for smaller and more active gold nanoparticles and as dissociation sites for water molecules. The calculated reaction path points to carboxyl formation as the rate-limiting step with an activation energy of 6.9 kcal mol(-1), which is in quantitative agreement with experimental measurements and, to the best of our knowledge, it is the lowest activation energy reported for the water-gas shift reaction. This discovery demonstrates the importance of combining experimental and theoretical techniques to model and understand catalytic processes and opens the door to new improvements to reduce the operating temperature and the deactivation of the catalyst.


Septiembre, 2018 | DOI: 10.1039/c8cp03706j

Graphene or carbon nanofiber-reinforced zirconia composites: Are they really worthwhile for structural applications?


Cano-Crespo, R; Moshtaghioun, BM; Gomez-Garcia, D; Moreno, R; Dominguez-Rodriguez, A
Journal of the European Ceramic Society, 38 (2018) 3994-4002

ABSTRACT

The use of allotropic phases of carbon (i.e. nanotubes, graphene or carbon nanofibers) as second phases to design ceramic composites is a hot topic at present. Researchers try to provide a remarkable improvement of the parent ceramic assuming that some of the outstanding mechanical properties of these phases migrate to the resultant composite. This reasonable idea has been questioned severely in the case of nanotubes addition but there is not any analysis for the other two phases cited previously. To elucidate this question, zirconia was selected as a model ceramic. This paper reports the mechanical properties of zirconia composites reinforced either with graphene or carbon nanofibers, with special emphasis on the high-temperature plasticity.


Septiembre, 2018 | DOI: 10.1016/j.jeurceramsoc.2018.04.045

Nanostructured vanadium carbonitride prepared by combustion synthesis during mechanical milling


Jalaly, M; Gotor, FJ; Sayagues, MJ
Journal of Alloys and Compounds, 763 (2018) 18-24

ABSTRACT

Vanadium carbonitride (VCN) nanoparticles were synthesized by a mechanically induced magnesiothermic combustion in a Mg/V2O5/C3H6N6 system. Initial materials ignited after a short milling time of 6 min. Various characterizations such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), high-resolution transmission electron microscopy (HRTEM) and elemental mapping confirmed that the product of the combustion was a mixed carbonitride. In this process, magnesium reduces vanadium oxide to generate elemental V and a great amount of heat. Melamine decomposes due to the temperature rise, and its decomposed species form the carbonitride compound. The chemical composition of the synthesized product was estimated to be VC0.26N0.36.


Septiembre, 2018 | DOI: 10.1016/j.jallcom.2018.05.352

Mechanosynthesis of Sr1-xLaxTiO3 anodes for SOFCs: Structure and electrical conductivity


Sayagues, MJ; Gotor, J; Pueyo, M; Poyato, R; Garcia-Garcia, FJ
Journal of Alloys and Compounds, 763 (2018) 679-686

ABSTRACT

Sr1-xLaxTiO3 (SLT; 0 <= x <= 0.5) powder samples were synthesised at room temperature by a mechanochemical method from SrO, La2O3 and TiO2 mixtures in 90 min. The obtained SLT samples as potential anode materials in solid oxide fuel cells (SOFCs) were investigated. The microstructure, electrical conductivity and chemical compatibility with yttria-stabilised zirconia (YSZ) were studied. The powder samples had a nanometric character after milling. After a subsequently heating at 900 degrees C, the particle size slightly increased, but still remained nanometric. At this high temperature, a good chemical compatibility with YSZ was found. The x = 0.2 sample gave the best electrical conductivity values, i.e. 0.23 W cm(-2). These features make such as-obtained samples good candidates to be used as anodes in SOFCs.


Septiembre, 2018 | DOI: 10.1016/j.jallcom.2018.05.243

Combined kinetic analysis of multistep processes of thermal decomposition of polydimethylsiloxane silicone


Garcia-Garrido, C; Perez-Maqueda, LA; Criado, JM; Sanchez-Jimenez, PE
Polymer, 153 (2018) 558-564

ABSTRACT

In this work, we studied the thermal decomposition of a widely employed silicone elastomer, polydimethylsiloxane, in an inert atmosphere. This silicone elastomer has several applications due to its high thermal stability such as MEMS (microelectromechanical systems) precursors, microfluidic components, adhesives, lubricants, and precursors for non-porous ceramics. Therefore, a reliable description of the thermal decomposition kinetics is important to prevent or control the decomposition in such applications. While the decomposition has been amply reported as a complex process, most kinetic studies published on this system use simplified methods that avoid the fact that the entire process cannot be described by a single kinetic triplet. Here, we have studied the decomposition process by first separating the overall reaction into its three constituent steps which were subsequently analysed independently. The deconvolution was carried out using Fraser-Suzuki function that is capable of fitting an asymmetric peak fitting function. The resulting kinetic parameters proved to be able to reconstruct the original experimental curves but are also capable of producing accurate predictions of curves recorded at heating schedules different from those employed to record the experimental data used in the kinetic analysis. Finally, it was found that the rate limiting step of all stages is the diffusion of the gases released during the polymer decomposition through the transforming polymeric matrix.


Septiembre, 2018 | DOI: 10.1016/j.polymer.2018.08.045

Absorption enhancement in methylammonium lead iodide perovskite solar cells with embedded arrays of dielectric particles


Jimenez-Solano, A; Carretero-Palacios, S; Miguez, H
Optics Express, 26 (2018) A865-A878

ABSTRACT

In the field of hybrid organic-inorganic perovskite based photovoltaics, there is a growing interest in the exploration of novel and smarter ways to improve the cells light harvesting efficiency at targeted wavelength ranges within the minimum volume possible, as well as in the development of colored and/or semitransparent devices that could pave the way both to their architectonic integration and to their use in the flowering field of tandem solar cells. The work herein presented targets these different goals by means of the theoretical optimization of the optical design of standard opaque and semitransparent perovskite solar cells. In order to do so, we focus on the effect of harmless, compatible and commercially available dielectric inclusions within the absorbing material, methylammonium lead iodide (MAPI). Following a gradual and systematic process of analysis, we are capable of identifying the appearance of collective and hybrid (both localized and ex tended) photonic resonances which allow to significantly improve light harvesting and thus the overall efficiency of the standard device by above 10% with respect to the reference value while keeping the semiconductor film thickness to a minimum. We believe our results will be particularly relevant in the promising field of perovskite solar cell based tandem photovoltaic devices, which has posed new challenges to the solar energy community in order to maximize the performance of semitransparent cells, but also for applications focusing on architectonic integration. 


Septiembre, 2018 | DOI: 10.1364/OE.26.00A865

Adhesion enhancement of DLC hard coatings by HiPIMS metal ion etching pretreatment


Santiago, JA; Fernandez-Martinez, I; Wennberg, A; Molina-Aldareguia, JM; Castillo-Rodriguez, M; Rojas, TC; Sanchez-Lopez, JC; Gonzalez, MU; Garcia-Martin, JM; Li, H; Bellido-Gonzalez, V; Monclus, MA; Gonzalez-Arrabal, R
Surface & Coatings Technology, 349 (2018) 787-796

ABSTRACT

Poor adhesion is a recurrent problem for the wider use of diamond-like carbon (DLC) coatings in industrial applications. In this work, we investigate the effectiveness of high-power impulse magnetron sputtering (HiPIMS) metal ion etching to improve the adhesion of DLC coatings on high speed steel substrates. The influence of HiPIMS pretreatment parameters, the metal ion selection for the process and the addition of bonding layers on the adhesion properties were studied. Daimler-Benz and nanoscratch test methods were used to evaluate the adhesion. The elemental composition, morphology and microstructure of the samples were evaluated by EELS, SEM, AFM and HRTEM. In general, samples pretreated with HiPIMS metal ion etching withstand larger critical loads than those pretreated by conventional Ar + glow discharge and bonding layers. The pretreatment is proven to be very effective at removing surface contaminants and providing a gradual interface. The selection of Cr over Ti contributes to a significant improvement on the adhesion due to the reduction of the oxygen level at the interface thus ensuring an optimal coating-substrate contact and a more compliant structure, which prevents the delamination failure.


Septiembre, 2018 | DOI: 10.1016/j.surfcoat.2018.04.090

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