Effect of substrate bias voltage on amorphous Si–C–N films produced by PVD techniques

SixCyNz thin films were deposited by reactive magnetron sputtering in glass and steel substrates. The films were grown in a rotation mode over a carbon and a silicon targets in a mixed Ar/N2 atmosphere. The substrates were held at a substrate temperature of 573 K. The argon flow was kept constant (100 sccm) and the nitrogen flow was 20 sccm or 25 sccm, in each one of the two series of produced films, resulting in a working pressure around 0.5 Pa. The substrate bias varied between grounded and -100 V. The films were analysed with respect to microstructure, state of chemical bonding and optical properties by X-Ray Diffraction (XRD), Raman Spectroscopy (RS), optical reflectance and transmittance. Raman spectroscopy was used as a probe of microstructural modifications induced by deposition conditions. The main features observed in RS spectra are the well-known D- and G-bands characteristic of amorphous carbon materials. The position, widths and intensity ratio of these bands are found to be dependent of the films deposition conditions. The refractive index, absorption coefficient, optical band gap and also the thickness were calculated from transmittance spectra obtained between 200 nm and 2500 nm.The residual stress of the coatings depends on deposition conditions and was calculated by measuring the substrate curvature before and after film deposition. The curvature of the samples was measured by laser triangulation in two series of two orthogonal directions. All coatings were in a state of compressive residual stress. The average hardness and Young’s modulus of the produced coatings is about 16 GPa and 170 GPa, respectively. The nano-hardness of the grounded produced samples presented values about 30% lower

Optical characterization of TiAlN/TiAlON/SiO2 absorber for solar selective applications

Characterization of a TiAlN/TiAlON/SiO2 tandem absorber is reported in this contribution. The first two layers were deposited by magnetron sputtering and the third layer was prepared by plasma enhanced chemical vapour deposition (PECVD). The optimization was performed by determining the optical constants of individual layers by first measuring spectral transmittance and reflectance of the individual layers. Subsequently the measuring spectra were fitted using the SCOUT software and dielectric function of each layer was determined. The three layer stack absorber on copper was then designed using those optical properties. The thickness of the individual layers was optimized until a solar absorptance of 95.5% was obtained resulting in a total thickness of about 215 nm (65 nm/51 nm/100 nm for the individual layers, respectively). A thermal emittance of 5% for an absorber temperature of 100 °C was obtained by analyzing the measuring data from a FTIR spectrometer with integrating sphere. During continuous thermal annealing at 278 °C for 600 h the absorptance decreased by 0.4%Savo Sola

Characterization of TiAlSiN/TiAlSiON/SiO2 optical stack designed by modelling calculations for solar selective applications

Preparation and characterization of TiAlSiN/TiAlSiON/SiO2 solar selective absorber is reported in this contribution. All layers were deposited in a continuous mode using a industrial equipment, the nitride and oxynitride were prepared by reactive magnetron sputtering and the SiO2 layer by Plasma Enhanced Chemical Vapour Deposition. The optical constants of individual layers were calculated by modelling of spectral transmittance and reflectance of the individual layers. The three layer stack absorber was then designed using those optical properties. The thickness of the individual layers was optimized until a solar absorptance of 96% was obtained resulting in a total thickness of about 200 nm, deposited in copper and extruded aluminium absorbers. An emissivity of 5 % for an absorber temperature of 100 ºC was obtained by analyzing the measuring data from a FTIR spectrometer with integrating sphere. After test duration of 600 h, the samples subjected to a thermal annealing at 278 ºC in air showed a performance criterion (PC) below 4% for, while the samples in the humidity tests showed a PC below 2 %.Savo Sola

A design of selective solar absorber for high temperature applications

This study presents a design of multilayer solar selective absorber for high temperature applications. The optical stack of this absorber is composed of four layers deposited by magnetron sputtering on stainless steel substrates. The first is a back-reflector tungsten layer, which is followed by two absorption layers based on CrAlSiNx/ CrAlSiOyNx structure for phase interference. The final layer is an antireflection layer of SiAlOx. The design was theoretically modelled with SCOUT software using transmittance and reflectance curves of individual thin layers, which were deposited on glass substrates. The final design shows simultaneously high solar absorbance = 95.2 % and low emissivity ε= 9.8% (at 400 ºC) together with high thermal stability at 400 ºC, in air, and 600 ºC in vacuum for 650 h.The authors acknowledge the support of FCT in the framework of the Strategic Funding UID/FIS/04650/2013 and the financial support of FCT, POCI and PORL operational programs through the project POCI-01-0145- FEDER-016907 (PTDC/CTM-ENE/2882/2014), co-financed by European community fund FEDER.info:eu-repo/semantics/publishedVersio

Solar selective absorbers based on Al2O3:W cermets and AlSiN/AlSiON layers

Solar selective coatings based on double Al2O3:W cermet layers and AlSiN/AlSiON bilayer structures were prepared by magnetron sputtering. Both were deposited on stainless steel substrates using a metallic tungsten (W) layer as back reflector. The coating stacks were completed by an antireflection (AR) layer composed of Al2O3, SiO2, or AlSiOx. Spectrophotometer measurements, X-Ray diffraction, Scanning electron microscopy, Energy Dispersive X-Ray Spectroscopy and Rutherford Backscattering Spectrometry were used to characterize the optical properties, crystalline structure, morphology and composition of these coatings. The spectral optical constants of the single layers were calculated from the reflectance and transmittance measurements and used to design the optical stack. The coatings exhibit a solar absorptance of 93%-95% and an emissivity of 7%-10% (at 400 ºC). The coatings also exhibit excellent thermal stability, with small changes in the optical properties of the coating during heat-treatments at 400 ºC in air for 2500 h and at 580 ºC in vacuum for 850 h. The coating based on the AlSiN/AlSiON bilayer structure was obtained with an Al:Si ratio of 2.5:1. These coatings revealed similar performance as the one obtained with coatings based on Al2O3:W cermet layers.The authors acknowledge the funding from the Finnish Funding Agency for Technology and Innovation, Tekes, and from FEDER funds through the “Programa Operacional Factores de Competitividade – COMPETE” and from national funds by FCT- “Fundação para a Ciência e a Tecnologia”, under project no. PEst-C/FIS/UI0607/2011.info:eu-repo/semantics/publishedVersio

Influence of nitrogen content on the structural, mechanical and electrical properties of TiN thin films

This paper reports on the preparation of TiNx thin films by d.c. reactive magnetron sputtering. The coating thickness ranged from 1.7 to 4.2 Am and the nitrogen content varied between 0 and 55 at.%. X-Ray diffraction showed the development of the hexagonal a-Ti phase, with strong [002] orientation for low nitrogen contents, where the N atoms fit into octahedral sites in the Ti lattice as the amount of nitrogen is increased. For nitrogen contents of 20 and 30 at.%, the q-Ti2N phase appears with [200] orientation. With further increasing the nitrogen content, the y-TiN phase becomes dominant. The electrical resistivity of the different compositions reproduces this phase behavior. The hardness of the samples varied from approximately 8 GPa for pure titanium up to 27 GPa for a nitrogen content of 30 at.%, followed by a slight decrease at the highest contents. A similar increase of stresses with nitrogen is observed. Structure and composition with the consequent changes in crystalline phases and the lattice distortion were found to be crucial in the evolution of the mechanical properties

Optical and structural analysis of solar selective absorbing coatings based on AlSiOx:W cermets

It is reported in this work the development and study of the optical and structural properties of a solar selective absorber cermet based on AlSiOx:W. A four-layer composite film structure, W/AlSiOx:W(HA)/AlSiOx:W(LA)/AlSiOx, was deposited on stainless steel substrates using the magnetron sputtering deposition method. Numerical calculations were performed to simulate the spectral properties of multilayer stacks with varying metal volume fraction cermets and film thickness. The chemical analysis was performed using X-ray photoelectron spectroscopy and the results show that in the high metal volume fraction cermet layer, AlSiOx:W(HA), about one third of W atoms are in the W-O oxidation state, another third in the Wx+ oxidation state and the last third in the W4+, W5+ and W6+ oxidation states. The X-ray diffractograms of AlSiOx:W layers show a broad peak indicating that both, W and AlSiOx, are amorphous. These results indicate that this film structure has a good spectral selective property that is suitable for solar thermal applications, with the coatings exhibiting a solar absorptance of 94-95.5% and emissivities of 8-9% (at 100 degrees C) and 10-14% (at 400 degrees C). The samples were subjected to a thermal annealing at 450 degrees C, in air, and 580 degrees C, in vacuum and showed very good oxidation resistance and thermal stability. Morphological characterizations were carried out using scanning electron microscopy and atomic force microscopy. Rutherford Backscattering experiments were also performed to analyze the tungsten depth profile.The authors acknowledge the support of the Portuguese Foundation for Science and Technology (FCT) in the framework of the Strategic Funding UID/FIS/04650/2013. The authors are also grateful to the financial support of FCT, POCI and PORL operational programs through the project POCI-01-0145-FEDER-016907 (PTDC/CTM-ENE/2882/2014), co-financed by European community fund FEDER. The authors also acknowledge GIST Japan for using the XPS-Kratos.info:eu-repo/semantics/publishedVersio

Effect of nitrogen gas flow on amorphous Si–C–N films produced by PVD techniques

Si C N thin films were deposited by reactive magnetron sputtering on glass and steel substrates. The films were grown in a x y z rotation mode over a carbon and a silicon targets in a mixed Ar/N2 atmosphere at a substrate temperature of 300 °C. The 2 substrates were held grounded or at a negative bias of -25 and -50 V. The film characteristics were also controlled by nitrogen flow. Binary and ternary films were obtained. The films were analysed with respect to microstructure, state of chemical bonding and optical properties by Raman spectroscopy (RS) and optical transmittance. RS was used as a probe of micro-structural modifications induced by deposition conditions. The main features observed in RS spectra are the well-known D- and G-bands characteristic of amorphous carbon. The position, widths and intensity ratio of these bands are found to be dependent on the film composition. The refractive index, the absorption coefficient and also the thickness were calculated from transmittance spectra obtained between 200 and 2500 nm. The hardness and Young’s modulus of the films were measured by nano-indentation experiments. The average hardness and Young’s modulus of the produced coatings was 21 and 200 GPa, respectively

Solar selective absorbing coatings based on AlSiN/AlSiON/AlSiOy layers

Coatings with a double absorbing layer based on AlSiN/AlSiON were deposited on stainless steel sub-strates by magnetron sputtering technique, with different Al:Si ratios. A tungsten layer was used asa back reflector and AlSiOyor SiOxthin films were used as antireflection top layers. Prior the structuredesign, several single layers were deposited on glass substrates by varying the reactive gases flows, whichallowed the stacking of a series of layers with different optical properties. Experimental transmittanceand reflectance were modelled for the assessment of the spectral optical constants, which were thenused to design a coating stack with optimized solar absorptance and thermal emittance. Optical prop-erties, microstructure, morphology, composition and chemical bonding were investigated by employingoptical spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffrac-tion and X-ray photoelectron spectroscopy. The samples were annealed in air at 400◦C and vacuum at580◦C with the purpose to evaluate their oxidation resistance and thermal stability, which was sub-sequently correlated with the Al:Si ratio. Optimum results were achieved for an Al:Si ratio of 2.3:1,whereas for significantly higher Si content resulted in detrimental performance. The solar absorbanceand thermal emittance for the optimized multilayer selective coatings is 93–94% and 7–10% (at 400◦C),respectively.The authors acknowledge the funding from the Finnish Funding Agency for Technology and Innovation, Tekes, and from FEDER funds through the "Programa Operacional Factores de Competitividade - COMPETE" and from national funds by FCT - "Fundacao para a Ciencia e a Tecnologia", under project no. PEst-C/FIS/UI0607/2011

Performance of chromium nitride and titanium nitride coatings during plastic injection moulding

Monolithic coatings of chromium nitride, titanium nitride and multilayer titaniumychromium nitride coatings were produced by r.f. and d.c. reactive magnetron sputtering in order to determine their potential to be used as protective coatings for machinery parts of plastic injection moulding or extruding machines. The tribological and mechanical behaviour of these coatings were studied. Monolithic coatings showed lower wear rates, measured by pin-on-disc experiments, when compared with multilayer coatings. The oxidation of the surface was also lower in monolithic coatings. The performance of the coatings during plastic processing was tested in a dye fitted to an injection moulding machine and using glass reinforced thermoplastic. The wear rates of the nitride-based coatings during plastic processing was more than two orders of magnitude better then some traditional methods of protecting the surfaces such as hardening the steel by heat treatment, electrodepositing hard chromium or nitriding the steel surface. The physical vapour deposition coatings also showed higher corrosion protection during plastic processing tests