Characterization and oxidation behavior of NiCoCrAlY coating fabricated by electrophoretic deposition and vacuum heat treatment

Electrophoretic deposition (EPD) was showed to be a feasible and convenient method to fabricate NiCoCrAlY coatings on nickel based supperalloys. The microstructure and composition of the NiCoCrAlY coatings after vacuum heat treatment were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray analysis (EDAX). Isothermal-oxidation test was performed at 1100 °C in static air for 100 h. The results show that the major phases in electrophoretic deposited and vacuum heat treated NiCoCrAlY coating are γ-Ni and γ′-Ni₃Al phases, also there is an extremely small quantity of Al₂O₃ in the coating. Composition fluctuations occur in the coating and a certain amount of titanium diffuse from the superalloy substrate to the top of the coating during vacuum heat treatment. The oxidation test results exhibit that the oxidation kinetics of this coating has two typical stages. The protective oxide layer is mainly formed in the initial linear growth stage and then the oxide layer hinders further oxidation of the coating in the subsequent parabolic growth stage. The coating can effectively protect the superalloy substrate from oxidation. A certain amount of rutile TiO₂ is formed in the coating during oxidation and it is adverse to the oxidation resistance of the coating.     

Preparation and in vitro characterization of aerosol-deposited hydroxyapatite coatings with different surface roughnesses

Hydroxyapatite (HA) coatings with different surface roughnesses were deposited on a Ti substrate via aerosol deposition (AD). The effect of the surface roughness on the cellular response to the coating was investigated. The surface roughness was controlled by manipulating the particle size distribution of the raw powder used for deposition and by varying the coating thickness. The coatings obtained from the 1100 °C-heated powder exhibited relatively smooth surfaces, whereas those fabricated using the 1050 °C-heated powder had network-structured rough surfaces with large surface areas and were superior in terms of their adhesion strengths and in vitro cell responses. The surface roughness (R_a) values of the coatings fabricated using the 1050 °C-heated powder increased from approximately 0.65 to 1.03 μm as the coating thickness increased to 10 μm. The coatings with a rough surface had good adhesion to the Ti substrate, exhibiting high adhesion strengths ranging from 37.6 to 29.5 MPa, depending on the coating thickness. The optimum biological performance was observed for the 5 μm-thick HA coating with an intermediate surface roughness value of 0.82 μm.     

Characteristic and biocompatibility of the TiO2-based coatings containing amorphous calcium phosphate before and after heat treatment

TiO₂-based coating containing amorphous calcium phosphate (CaP) was prepared on titanium alloy by microarc oxidation (MAO). The increase in the EDTA-2Na concentration was unfavorable for the crystallization of TiO₂. After heat treatment, the amorphous CaP was crystallized. The thickness of the MAO coatings did not change when heat-treated at 400, 600 and 700 °C; while it increased slightly after heat treatment at 800 °C due to the crystallization of amorphous CaP and growth of TiO₂. No apparent discontinuity between the coatings and substrates was observed at various heat-treatment temperatures, indicating the MAO coatings with good interfacial bonding to the substrate. The heat treatment did not alter the chemical composition of the MAO coating and the chemical states of Ti, Ca and P elements. However, it increased the roughness (Ra) of the MAO coating and improved the wetting ability of the MAO coating. In this work, preliminary investigation of the MG63 cell proliferation on the surface of the MAO and heat-treated MAO coatings was conducted. The MAO coating surface with about Ra = 220 nm may be suitable for the MG63 cell adhesion and proliferation. The increased roughness of the heat-treated MAO coatings may result in a decrease in the ability for cell adhesion and proliferation.     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Microstructure and high-temperature corrosion behaviors of aluminide coatings by low-temperature pack aluminizing process

Aluminide coatings were produced on carbon steel and Fe-5Cr-Mo alloy at a relatively lower temperature below 600 °C in shorter treatment time by a combination of surface refinement process and pack aluminizing process. Repetitive ball impact, generated by mechanical vibration, caused the top-layer refinement of substrates in a conventional pack aluminizing process. The effects of temperature and treatment time on the formation of aluminide coatings were analyzed. The microstructure of the coatings was investigated by SEM, AFM and XRD. The aluminide coatings were one-layer, compacted structure with ultrafine grains and uniform elemental distribution. High-temperature oxidation and sulphidation tests were carried out at 600 °C in air for 200 h and 10% SO₂ + Ar gas mixture atmosphere for 50 h, respectively. The mass gains and spallation indicated that the aluminide coatings significantly improved the high-temperature oxidation and sulphidation resistance.     

Microstructure, mechanical properties, and oxidation resistance of nanocomposite Ti-Si-N coatings

Ti-Si-N coatings with different silicon contents (0-12 at.%) were deposited onto Si(1 0 0) wafer, AISI M42 high speed steel, and stainless steel plate, respectively. These coatings were characterized and analyzed by using a variety of analytical techniques, such as XRD, AES, SEM, XPS, nanoindentation measurements, Rockwell C-type indentation tester, and scratch tester. The results revealed that the hardness was strongly correlated to the amount of silicon addition into a growing TiN film. The maximum hardness of 47.1 GPa was achieved as the Si content was 8.6 at.%. In the mechanical and oxidation resistance measurements, the Ti-Si-N coatings showed three distinct behaviors. (i) The coatings with Si contents of no more than 8.6 at.% performed good adhesion strength quality onto the HSS substrates. (ii) The fracture toughness of the coatings decreased with the increase in Si content. (iii) The Ti-Si-N coating with 8.6 at.% Si showed the excellent oxidation resistance behavior. The cutting performance under using coolant conditions was also evaluated by a conventional drilling machine. The drills with Ti-Si-N coatings performed much better than the drills with TiN coating and the uncoated drills.     

RB-SiC表面改性Si涂层的制备与性能

 为了获得高质量光学表面的碳化硅反射镜,利用射频磁控溅射方法,在直径70 mm的RB-SiC基片上沉积了厚约100 μm的Si改性涂层,对改性层进行超光滑加工,并对改性层的表面形貌及性能进行了测试。ZYGO表面粗糙度仪测试结果表明,抛光后Si改性涂层表面粗糙度均方根值达到了0.496 nm;X射线衍射仪测试显示,制备Si改性涂层为多晶结构;使用拉力机做附着力测试,结果表明膜基附着力大于10.7 MPa。证明采用磁控溅射技术制备的Si改性涂层均匀、致密、附着力好,能够满足RB-SiC材料表面改性要求。     

Effect of plasma pretreatment on adhesion and mechanical properties of UV-curable coatings on plastics

An attempt was made to study the effect of plasma surface activation on the adhesion of UV-curable sol-gel coatings on polycarbonate (PC) and polymethylmethacrylate (PMMA) substrates. The sol was synthesized by the hydrolysis and condensation of a UV-curable silane in combination with Zr-n-propoxide. Coatings deposited by dip coating were cured using UV-radiation followed by thermal curing between 80 °C and 130 °C. The effect of plasma surface treatment on the wettability of the polymer surface prior to coating deposition was followed up by measuring the water contact angle. The water contact angle on the surface of as-cleaned substrates was 80° ± 2° and that after plasma treatment was 43° ± 1° and 50° ± 2° for PC and PMMA respectively. Adhesion as well as mechanical properties like scratch resistance and taber abrasion resistance were evaluated for coatings deposited over plasma treated and untreated surfaces.     

Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

Alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres were synthesized by conventional anodization route. Scanning Electron Microscopy (SEM), Atomic Force microscopy (AFM), X-Ray Diffraction (XRD) and Energy Dispersive X-Ray spectroscopy (EDAX) were used to characterize the morphology and crystalloid structure of ASZNC fibres. Current density (DC) is one of the important parameters to get the alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres by this route. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity. The root mean square roughness of the sample observed from atomic force microscopic analysis is about 71.5 nm which is comparable to the average grain size of the coatings which is about 72 nm obtained from X-Ray diffraction. The results indicate that, the ASZNC fibres are arranged well in the nanostructure. The thickness of the coating increased with the anodizing time, but the coatings turned rougher and more porous. At the initial stage the growth of ceramic coating increases inwards to the metal substrate and outwards to the coating surface simultaneously. Subsequently, it mainly grows towards the metal substrate and the density of the ceramic coating increases gradually, which results in the decrease of the total thickness as anodizing time increases. This new approach of preparing ASZNC ceramic fibres may be important in applications ranging from gas sensors to various engineering materials.     

A novel graded bioactive high adhesion implant coating

One method to increase the clinical success rate of metal implants is to increase their bone bonding properties, i.e. to develop a bone bioactive surface leading to reduced risks of interfacial problems. Much research has been devoted to modifying the surface of metals to make them become bioactive. Many of the proposed methods include depositing a coating on the implant. However, there is a risk of coating failure due to low substrate adhesion. This paper describes a method to obtain bioactivity combined with a high coating adhesion via a gradient structure of the coating. Gradient coatings were deposited on Ti (grade 5) using reactive magnetron sputtering with increasing oxygen content. To increase the grain size in the coating, all coatings were post annealed at 385 °C. The obtained coating exhibited a gradual transition over 70 nm from crystalline titanium oxide (anatase) at the surface to metallic Ti in the substrate, as shown using cross-section transmission electron microscopy and X-ray photoelectron spectroscopy depth profiling. Using scratch testing, it could be shown that the adhesion to the substrate was well above 1 GPa. The bioactivity of the coating was verified in vitro by the spontaneous formation of hydroxylapatite upon storage in phosphate buffer solution at 37 °C for one week.The described process can be applied to implants irrespective of bulk metal in the base and should introduce the possibility to create safer permanent implants like reconstructive devices, dental, or spinal implants.     

Mechanical performance of apatite/TiO2 composite coatings formed on Ti and NiTi shape memory alloy

To make metals bioactive for orthopaedic applications, apatite/TiO₂ composite coatings were formed on Ti and NiTi shape memory alloy (SMA) using a H₂O₂-oxidation and hot water aging technique and the subsequent accelerated biomimetic process. In the current investigation, nanoindentation, scratch testing and frictional testing were employed to assess mechanical properties and the adhesion of apatite/TiO₂ composite coatings formed on Ti and NiTi SMA. Nanoindentation testing conducted on cross-sections of composite coatings indicated that there was no significant difference in nanohardness and elastic modulus between apatite/TiO₂ composite coatings formed on Ti and NiTi SMA samples. The enhancement of the adhesion between the apatite layer and the metal substrates arose from the TiO₂ intermediate layer in the composite coating. The highest values of coating adhesion strength for Ti and NiTi SMA samples, as measured by scratch tests, were 22.58 N and 19.07 N, respectively. However, compared to corresponding Ti samples, NiTi SMA samples had better tribological properties.     

Mechanical properties of Mo-Ru thin films with Ni interlayer of different thickness

Noble metal coatings are usually introduced to increase lifetime of glass molding die. In this study, Mo-Ru coatings with Ni interlayer were deposited on tungsten carbide by DC sputtering processes at an elevated temperature of 550 °C to modify the properties in molding die materials. Phase identification was investigated by X-ray diffractometry (XRD). The surface morphology and composition of coatings were evaluated by atomic force microscopy (AFM) and field-emission electron probe microanalyzer (FE-EPMA), respectively. Hardness of the Mo-Ru films was measured by nanoindentation testing. In the aspects of adhesion, the influence on interlayer of different thickness was probed by the scratch test, and the different composition of Mo-Ru resulted in various kinds of fracture configurations. The scratch test exhibited spalling and chipping failure between substrate and layer.     

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.     

The effect of substrate bias voltages on impact resistance of CrAlN coatings deposited by modified ion beam enhanced magnetron sputtering

CrAlN coatings were deposited on silicon and AISI H13 steel substrates using a modified ion beam enhanced magnetron sputtering system. The effect of substrate negative bias voltages on the impact property of the CrAlN coatings was studied. The X-ray diffraction (XRD) data show that all CrAlN coatings were crystallized in the cubic NaCl B1 structure, with the (1 1 1), (2 0 0) (2 2 0) and (2 2 2) diffraction peaks observed. Two-dimensional surface morphologies of CrAlN coatings were investigated by atomic force microscope (AFM). The results show that with increasing substrate bias voltage the coatings became more compact and denser, and the microhardness and fracture toughness of the coatings increased correspondingly. In the dynamic impact resistance tests, the CrAlN coatings displayed better impact resistance with the increase of bias voltage, due to the reduced emergence and propagation of the cracks in coatings with a very dense structure and the increase of hardness and fracture toughness in coatings.     

Fabrication and characterization of rod-like nano-hydroxyapatite on MAO coating supported on Mg-Zn-Ca alloy

The poor corrosion resistance of magnesium alloys is a dominant problem that limits their clinical application. In order to solve this challenge, micro-arc oxidation (MAO) was used to fabricate a porous coating on magnesium alloys and then electrochemical deposition (ED) was done to fabricate rod-like nano-hydroxyapatite (RNHA) on MAO coating. The cross-section morphology of the composite coatings and its corresponding energy dispersion spectroscopy (EDS) surficial scanning map of calcium revealed that HA rods were successfully deposited into the pores. The three dimensional morphology and scanning electron microscopy (SEM) image of the composite coatings showed that the distribution of the HA rods was dense and uniform. Atomic force microscope (AFM) observation of the composite coatings showed that the diameters of HA rods varied from 95 nm to 116 nm and the root mean square roughness (RMS) of the composite coatings was about 42 nm, which were favorable for cellular survival. The bonding strength between the HA film and MAO coating increased to 12.3 MPa, almost two times higher than that of the direct electrochemical deposition coating (6.3 MPa). Compared with that of the substrate, the corrosion potential of Mg-Zn-Ca alloy with composite coatings increased by 161 mV and its corrosion current density decreased from 3.36 × 10⁻⁴ A/cm² to 2.40 × 10⁻⁷ A/cm² which was due to the enhancement of bonding strength and the deposition of RNHA in the MAO pores. Immersion tests were carried out at 36.5 ± 0.5 °C in simulated body fluid (SBF). It was found that RNHA can induce the rapid precipitation of calcium orthophosphates in comparison with conventional HA coatings. Thus magnesium alloy coated with the composite coatings is a promising candidate as biodegradable bone implants.     

Properties of Cu film and Ti/Cu film on polyimide prepared by ion beam techniques

Cu film and Ti/Cu film on polyimide substrate were prepared by ion implantation and ion beam assisted deposition (IBAD) techniques. Three-dimension white-light interfering profilometer was used to measure thickness of each film. The thickness of the Cu film and Ti/Cu film ranged between 490 nm and 640 nm. The depth profile, surface morphology, roughness, adhesion, nanohardness, and modulus of the Cu and Ti/Cu films were measured by scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindenter, respectively. The polyimide substrates irradiated with argon ions were analyzed by scanning electron microscopy (SEM) and AFM. The results suggested that both the Cu film and Ti/Cu film were of good adhesion with polyimide substrate, and ion beam techniques were suitable to prepare thin metal film on polyimide.     

Using Zn as target to fabricate ZnO coating by thermal oxidation in air on quartz substrate

In this work, ZnO coatings were fabricated by the RF-sputtering method on quartz substrates in an inert gas ambient of Ar followed by a thermal oxidation process in air at different temperatures. The effect of thermal oxidation temperatures on the structures and photoluminescence (PL) properties of the coatings were studied. The structural characteristics of the samples were analyzed by X-ray diffraction (XRD) and atomic force microscope (AFM). The PL spectra were obtained by using a Xe laser as a light source with an excitation wavelength of 325 nm at room temperature. The force-curves were obtained by AFM. The results show that all the prepared ZnO coatings have a compact hexagonal wurtzite structure. With the increasing annealing temperature from 400 °C to 600 °C, the particle size, surface RMS roughness, photoluminescence intensity and adhesion force of the prepared ZnO coatings were increased as well.     

Influence of Si substrate preparation on surface chemistry and morphology of L-CVD SnO2 thin films studied by XPS and AFM

Results of experimental studies of the influence of substrate preparation on the surface chemistry and surface morphology of the laser-assisted chemical vapour deposition (L-CVD) SnO₂ thin films are presented in this paper. The native Si(1 0 0) substrate cleaned by UHV thermal annealing (TA) as well as thermally oxidized Si(1 0 0) substrate cleaned by ion bombardment (IBA) have been used as the substrates. X-ray photoemission spectroscopy (XPS) has been used for the control of surface chemistry of the substrates as well as of deposited films. Atomic force microscopy (AFM) has been used to control the surface morphology of the L-CVD SnO₂ thin films deposited on differently prepared substrates. Our XPS shows that the L-CVD SnO₂ thin films deposited on thermally oxidized Si(1 0 0) substrate after cleaning with ion bombardment exhibit the same stoichiometry, i.e. ratio [O]/[Sn] = 1.30 as that of the layers deposited on Si(1 0 0) substrate previously cleaned by UHV prolonged heating. AFM shows that L-CVD SnO₂ thin films deposited on thermally oxidized Si(1 0 0) substrate after cleaning with ion bombardment exhibit evidently increasing rough surface topography with respect to roughness, grain size range and maximum grain height as the L-CVD SnO₂ thin films deposited on atomically clean Si substrate at the same surface chemistry (nonstoichiometry) reflect the higher substrate roughness after cleaning with ion bombardment.     

Influence of deposition parameters on hard Cr-Al-N coatings deposited by multi-arc ion plating

The Cr-Al-N coatings were synthesized at various substrate bias voltages and nitrogen partial pressures by multi-arc ion plating (M-AIP). The relationships between deposition parameters and coating properties were investigated. Morphologies, phase structures, hardness and adhesion strength of the coatings were analyzed by SEM, XRD, XPS, nano-indenter and scratch tester. The results indicated that with the increase of substrate bias voltages, the surface macroparticles and deposition rate reduced mainly for the resputtering phenomenon. The (Cr, Al)N solid-solution phase kept unchanged, but the Cr₂N and AlN phases disappeared gradually. Due to the change of phase structures and residual compressive stress, the hardness values decreased and the adhesion strength decreased initially and then increased. Similarly, with the increase of nitrogen partial pressures, the phase structures of CrAlN coatings varied from Cr + Cr₂N + (Cr,Al)N to Cr₂N + (Cr,Al)N. The surface macroparticles increased due to the decreasing resputtering efficiency, and the deposition rate increased initially and then decreased due to the resputtering phenomenon. With increasing nitrogen partial pressures, adhesion strength decreased initially and then increased. The microhardness increased mainly due to the increase of Cr₂N contents and decrease of metal macroparticles.     

Microstructure and selected properties of hot-work tool steel with PVD coatings after laser surface treatment

The paper presents the effect of HPD laser treatment on the microstructure and selected properties of the PVD CrN, (Ti,Al) and Ti(C,N) coatings deposited onto hot-work tool steel substrates. The microstructure and surface topography of the investigated samples are characteristic of the diversified morphology connected with the applied laser beam power. Employment of laser beam at 0.7 kW power to the laser treatment of samples with Ti(C,N) coatings causes clear coating adhesion growth because of the diffusive processes induced by heat release. Because of the higher value of the (Ti,Al)N absorption coefficient one can state that the observed substrate materials change and finally coatings destruction in case of those samples is the most noticeable. The moderate effect of the laser beam treatment of the hot-work tool steel with the PVD coating was observed for CrN coatings. However, for laser beam power above 0.5 kW differences in the thermal expansion coefficients of the substrate materials and coatings generate coating crackings.