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.     

Fabrication of protective tantalum carbide coatings on carbon fibers using a molten salt method

Protective tantalum carbide (TaC) coatings were fabricated successfully on carbon fibers in the temperature range of 950-1100 °C using a molten salt method. A salt mixture composed of LiCl-KCl-KF was used as a reaction medium in which the tantalum and the carbon fiber substrates reacted to form the TaC coatings. The structure and morphology of the TaC coatings were characterized by XRD, SEM and EDX analyses. The results show that the reaction temperature and time have significant influence on the thickness, integrity and surface morphology of the TaC coatings. A uniform, adherent and crack-free TaC coating can be obtained by controlling the reaction temperature and time. Thermo-gravimetric analysis indicated that the oxidation resistance of the carbon fibers was improved remarkably by coating them with a high-quality TaC layer.     

Preparation and characterization of boron nitride coatings on carbon fibers from borazine by chemical vapor deposition

Boron nitride (BN) coatings were deposited on carbon fibers by chemical vapor deposition (CVD) using borazine as single source precursor. The deposited coatings were characterized by scanning electron microscopy (SEM), Auger electron spectroscopy (AES), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. The effect of temperatures on growth kinetics, morphology, composition and structure of the coatings was investigated. In the low temperature range of 900 °C-1000 °C, the growth rate increased with increasing temperature complying with Arrhenius law, and an apparent active energy of 72 kJ/mol was calculated. The coating surface was smooth and compact, and the coatings uniformly deposited on individual fibers of carbon fiber bundles. The growth was controlled by surface reaction. At 1000 °C, the deposition rate reached a maximum (2.5 μm/h). At the same time, the limiting step of the growth translated to be mass-transportation. Above 1100 °C, the growth rate decreased drastically due to the occurrence of gas-phase nucleation. Moreover, the coating surface became loose and rough. Composition and structure examinations revealed that stoichiometric BN coatings with turbostratic structure were obtained below 1000 °C, while hexagonal BN coatings were deposited above 1100 °C. A penetration of carbon element from the fibers to the coatings was observed.     

Effect of microarc oxidation coating on fatigue performance of Ti-Al-Zr alloy

Ceramic coatings of different thickness were fabricated on Ti6Al2Zr1Mo1V alloy by microarc oxidation (MAO), and the effect of the coating on fatigue life was evaluated by 810 Material Test System. The microstructure, phase and chemical composition of the coatings were determined by SEM, XRD and EDS techniques. The coating mainly consists of rutile and a small amount of anatase TiO₂. With oxidation time ranging from 10 to 30 min, the coating thickness increases from 13 to 25 μm, while the interface between coating and substrate becomes more zigzag, characterized by increasing overgrowth regions of coating into substrate. Under the same cyclic stress of 750 MPa, the fatigue life decreases from 2.08 × 10⁶ cycles for uncoated specimen to about 3 × 10⁴ cycles for microarc oxidized specimen. Under the cyclic stress, the thicker the coating, the more cracks initiate in the overgrowth regions of coating into substrate near the interface, which are considered as the notch sites of stress concentration to induce the crack initiation, also is the key factor to cause the facture.     

Self-lubricative coating grown by micro-plasma oxidation on aluminum alloys in the solution of aluminate-graphite

Aluminum trioxide ceramic coatings with high hardness were grown on surfaces of 2024 Aluminum alloys by micro-plasma oxidation in an aluminate electrolytic solution, which highly improve wear-resisting properties of 2024 Aluminum alloys. However, ceramic coating surfaces are porous and very coarse, which is disadvantageous to practical applications. In this paper, in order to increase the density of the pores and decrease the friction coefficient of the ceramic coatings, different concentrations (2-8 g/l) of graphite were added into the aluminate electrolytic solution. The thickness and hardness of the produced ceramic coatings were measured by HVS-100 micro-hardness tester and thickness tester. The friction coefficient of the coatings was studied by a frictionometer. The phase composition and surface morphology of the MPO films were evaluated through X-ray diffraction (XRD) and scanning electron microscope (SEM). The results show that the thickness of the ceramic coating is about 22 ± 1 μm, surfaces of the ceramic coatings are very uniform and that the coatings consist of mainly aluminum trioxides and a certain amount of graphite, which indicates graphite have entered the ceramic films during the micro-plasma oxidation process. Wear properties results show that the friction coefficient of the ceramic coatings decreased when graphite entered the ceramic films. When the concentration of graphite is 4 g/l, the wear properties of the coatings is the most excellent and the friction coefficient decreases to the lowest, that is 0.09.     

Characteristics and heat treatment of cold-sprayed Al-Sn binary alloy coatings

In this study, Al-Sn binary alloy coatings were prepared with Al-5 wt.% Sn (Al-5Sn) and Al-10 wt.% Sn (Al-10Sn) gas atomized powders by low pressure and high pressure cold spray process. The microstructure and microhardness of the coatings were characterized. To understand the coarsening of tin in the coating, the as-sprayed coatings were annealed at 150, 200, 250 and 300 °C for 1 h, respectively. The effect of annealing on microstructure and the bond strength of the coatings were investigated. The results show that Al-5Sn coating can be deposited by high pressure cold spray with nitrogen while Al-10Sn can only be deposited by low pressure cold spray with helium gas. Both Al-5Sn and Al-10Sn coatings present dense structures. The fraction of Sn in as-sprayed coatings is consistent with that in feed stock powders. The coarsening and/or migration of Sn phase in the coatings were observed when the annealing temperature exceeds 200 °C. Furthermore, the microhardness of the coatings decreased significantly at the annealing temperature of 250 °C. EDXA analysis shows that the heat treatment has no significant effect on fraction of Sn phase in Al-5Sn coatings. Bonding strength of as-sprayed Al-10Sn coating is slightly higher than that of Al-5Sn coating. Annealing at 200 °C can increase the bonding strength of Al-5Sn coatings.     

Microstructures and tribological properties of CrN/ZrN nanoscale multilayer coatings

Nanoscale multilayer CrN/ZrN coatings with bilayer thicknesses ranging from 11.7 to 66.7 nm were prepared by reactive magnetron sputtering techniques. The structure of the thin films was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction results showed that CrN individual layers presented a <1 1 1> preferred orientation in the multilayer coatings. The diffraction peaks of CrN shifted continuously to low diffraction angle with decreasing bilayer thickness. TEM observations showed that the multilayer did not form a superlattice structure instead of the coexistence of nanocrystalline CrN and ZrN layers. Columnar growth for all the coatings was observed by cross-sectional SEM. Nanoindentation tests showed that the multilayer coatings had almost a constant nanohardness of 29 GPa in spite of the variations of bilayer thickness. Pin-on-disk tests indicated that both the friction coefficients and wear rates increased when decreasing bilayer thickness. However, in comparison with the monolayer coating, the multilayer coatings exhibited excellent wear resistance.     

Low infrared emissivity of polyurethane/Cu composite coatings

Polyurethane/Cu composite coatings with low infrared emissivity near to 0.10 at the wavelength of 8-14 μm were prepared by a simple and convenient process. The influences of the content of Cu powder, surface roughness, coating thickness and temperature on infrared emissivity of the coatings were systematically investigated. The results indicated that the emissivity decreases significantly with increasing content of Cu powder and coating thickness. The coatings with smooth surface exhibit lower emissivity values than those with rough coatings. Moreover, we found the relationship between the emissivity of coatings and temperature presents a “U” type, and the emissivity reaches to the minimum at about 380 K. The mechanisms of low emissivity were proposed by optical theories, which are found to be in a good agreement with the experimental results.     

Effects of duty ratio at low frequency on growth mechanism of micro-plasma oxidation ceramic coatings on Ti alloy

The aim of this work is to study the effects of duty ratio on the growth mechanism of the ceramic coatings on Ti-6Al-4V alloy prepared by pulsed single-polar MPO at 50 Hz in NaAlO₂ solution. The phase composition of the coatings was studied by X-ray diffraction, and the morphology and the element distribution in the coating were examined through scanning electron microscopy and energy dispersive spectroscopy. The thickness of the coatings was measured by eddy current coating thickness gauge. The corrosion resistance of the coated samples was examined by linear sweep voltammetry technique in 3.5% NaCl solution. The changes of the duty ratio (D) of the anode process led to the changes of the mode of the spark discharge during the pulsed single-polar MPO process, which further influenced the structure and the morphology of the ceramic coatings. The coatings prepared at D = 10% were composed of a large amount of Al₂TiO₅ and a little γ-Al₂O₃ while the coatings prepared at D = 45% were mainly composed of α-Al₂O₃ and γ-Al₂O₃. The coating thickness and the roughness were both increased with the increasing D due to the formation of Al₂O₃. The formation of Al₂TiO₅ resulted from the spark discharge due to the breakdown of the oxide film, while the formation of Al₂O₃ resulted from the spark discharge due to the breakdown of the vapor envelope. The ceramic coatings improved the corrosion resistance of Ti-6Al-4V alloy. And the surface morphology and the coating thickness determined the corrosion resistance of the coated samples prepared at D = 45% was better than that of the coated samples prepared at D = 10%.     

Formation of titania composite coatings on carbon steel by plasma electrolytic oxidation

Titania composite coatings were prepared on carbon steel by plasma electrolytic oxidation in silicate electrolyte and aluminate electrolyte with titania powers doping in the electrolytes. The microstructure of the coatings was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The properties of the coatings including bond strength, thickness, thermal shock resistance and corrosion resistance varying with the quantities of titania powers in the electrolytes were studied. Investigation results revealed that the coating obtained in silicate electrolyte was composed of anatase-TiO₂, rutile-TiO₂ crystal phases and some Fe, Si, P elements; coating obtained in aluminate electrolyte consisted of anatase-TiO₂, Al₂TiO₅ and some Fe, P elements. Coatings obtained in two types of electrolytes show porous and rough surface. With increasing the concentration of titania powers in the electrolytes, the coating surface first became more compact and less porous and then became more porous and coarse. The bond strength and thickness were not strongly affected by concentration of titania powers in electrolytes. The valves were 23 MPa and for 66 μm for coatings obtained in aluminate electrolyte, and 21 MPa and 35 μm for coatings obtained in silicate electrolyte. Coatings obtained in silicate electrolyte showed a little better thermal shock resistance than those obtained in aluminate electrolyte and the best coatings were obtained with middle concentration of titania powers in the electrolytes. All coated samples showed better corrosion resistance than the substrate in 3.5 wt% NaCl solution. The best coatings were also obtained with middle concentration of titania powers doping in both electrolytes whose corrosion current density was decreased by 2 orders of magnitude compared with the substrate.     

Influence of heat treatment on tribological properties of electroless Ni-P and Ni-P-Al2O3 coatings on Al-Si casting alloy

Evolution of tribological properties of electroless Ni-P and Ni-P-Al₂O₃ coating on an Al-10Si-0.3Mg casting alloy during heat treatment is investigated in this work. The pre-treated substrate was plated using a bath containing nickel hypophosphite, nickel lactate and lactic acid. For preparation of fiber-reinforced coating Al₂O₃ Saffil fibers pre-treated in demineralised water were used. The coated samples were heat treated at 400-550 °C/1-8 h. Tribological properties were studied using the pin-on-disc method. It is found that the best coating performance is obtained using optimal heat treatment regime (400 °C/1 h). Annealing at higher temperatures (450 °C and above) leads to the formation of intermetallic compounds that reduce the coating wear resistance. The reason is that the intermetallic phases adversely affect the coating adherence to the substrate. The analysis of wear tracks proves that abrasion is major wear mechanism, however due to the formed intermetallic sub-layers, partial coating delamination may occur during the pin-on-disc test on the samples annealed at 450 °C and above. It was found that fiber reinforcement reduces this scaling and increases wear resistance of coatings as compared to the non-reinforced Ni-P coatings.     

Fabrication of silver stabilization layer of coated conductor using organic silver complexes

Silver stabilizing layer of coated conductor has been prepared by dip coating method using organic silver complexes containing 10 wt.% silver as a starting material. Coated silver complex layer was dried in situ with hot air and converted to crystalline silver by post heat treatment in flowing oxygen atmosphere. A dense continuous silver layer with good surface coverage and proper thickness of 230 nm is obtained by multiple dip coatings and heat treatments. The film heat treated at 500 °C showed good mechanical adhesion and crystallographic property. The interface resistivity between superconducting YBCO layer and silver layer prepared by dip coating was measured as 0.67 × 10⁻¹³ Ω m².     

Plasma sprayed Al2O3/FeCrAl composite coatings for electromagnetic wave absorption application

Al₂O₃/FeCrAl composite coatings were fabricated by atmosphere plasma spraying technique. Microstructure and dielectric properties in the frequency range from 8.2 to 12.4 GHz were investigated. The microstructure of composite coatings shows a uniform dispersion of metal particles with litter pores and microcracks in the composite coatings. The relaxation polarization and interfacial polarization in the coatings would contribute to enhance ?′ with rising FeCrAl content, and the associated loss could be considered as a dominating factor enhancing ?″. By calculating the microwave-absorption as a single-layer absorber, for the composite coatings with 41 wt.% FeCrAl content, the reflection loss values exceeding −10 dB are achieved in the frequency range of 9.1-10.6 GHz when the coating thickness is 1.3 mm.     

Improved moisture resistance of SrS:Eu phosphors with nanoscale SiO2 coating

Orange-emitting SrS:Eu²⁺ phosphors were coated with nanoscale SiO₂ and their photoluminescence (PL) degradation behavior in moist air was investigated. The SiO₂ coating was obtained by sol-gel process using diethoxydimethylsilane (DEDMS) and the coating content was varied from 0.5 to 2 wt%. The coatings were composed of a uniform, continuous, and amorphous SiO₂ layer of 30-50 nm thickness and the coating thickness was not varied significantly with the coating content. No peak shift and no decrease of PL intensity were observed after coating. The PL intensity of the coated phosphors decreased to ∼75% of the original value after 10 h exposure to moist air, while the uncoated phosphor decreased to ∼33%, which indicates the improved moisture resistance of the nanoscale SiO₂ coated SrS:Eu²⁺ phosphors.     

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.     

Microstructure, bonding strength and thermal shock resistance of ceramic coatings on steels prepared by plasma electrolytic oxidation

Ceramic coatings were successfully prepared on steel by plasma electrolytic oxidation (PEO) in aluminate electrolyte and silicate electrolyte, respectively. The microstructure of the coatings including surface morphology, phase and element composition were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The bonding strength between the ceramic coating and the substrate was tested using different methods including tensile tests and shearing tests. The thermal shock resistance of the coatings was also evaluated. The results indicated that coatings obtained in both electrolytes were porous and coarse. The average diameters of the pores were below 10 μm. PEO coatings obtained in aluminate electrolyte were composed of Fe₃O₄ and FeAl₂O₄, while those obtained in silicate electrolyte were in a noncrystal state. PEO coatings obtained in aluminate electrolyte showed similar change trend of tensile strength and shearing strength with increasing treating time, namely, a relatively high values with middle time treating and low value with short and long time treating. The best coating was the samples treated with 30 min, whose tensile strength was 20.6 MPa and shearing strength was 16 MPa. The tensile strength and shearing strength of coatings obtained in silicate electrolyte were not strongly influenced by the treating time, the values of which were range in 14 ± 2 MPa and 11 ± 2 MPa, respectively. Coatings obtained in both electrolytes showed the best thermal shock resistance with middle time treating. Coatings obtained in silicate electrolyte show a little better thermal shock resistance than those obtained in aluminate electrolyte.     

Deposition of thick and adherent Teflon-like coating on industrial scale stainless steel shell using pulsed dc and RF PECVD

A unique combination of pulsed dc and radio frequency (RF) discharge deposition was used to deposit thick (∼5 μm) and adherent (2-4 MPa) Teflon-like coatings on a stainless steel (SS) shell of 2 m diameter size, through plasma enhanced chemical vapor deposition (PECVD). The details of deposition on such a big industrial scale component are reported for the first time. In this method, highly adherent thin interface layers were grown on SS shell that was electrically grounded, using pulsed dc discharge, followed by RF discharge deposition to build up the required coating thickness. The fluorocarbon precursor molecules, required for the deposition of Teflon-like coating, are generated indigenously by pyrolyzing the Teflon powder. The deposited coating was studied for its chemical bond state, surface roughness (Ra), morphology, thickness, and adhesive strength. These studies were carried out by using XPS, AFM, SEM, etc. The adhesive strength of the coating was measured by pin-pull test as per ASTM D4541 standard test. The coatings deposited with pulsed dc discharge were observed to have higher adhesive strength when compared with those deposited with RF discharge.     

In situ formation of low friction ceramic coatings on carbon steel by plasma electrolytic oxidation in two types of electrolytes

In situ formation of ceramic coatings on Q235 carbon steel was achieved by plasma electrolytic oxidation (PEO) in carbonate electrolyte and silicate electrolyte, respectively. The surface and cross-section morphology, phase and elemental composition of PEO coatings were examined by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS). The bond strength of the coating was determined using a direct pull-off test. The hardness as well as tribological properties of the ceramic coating was primarily studied. The results indicated that the coating obtained in carbonate electrolyte was Fe₃O₄, while the coating achieved from silicate electrolyte was proved to be amorphous. Both kinds of coatings showed coarse and porous surface. The Fe₃O₄ coatings obtained in carbonate electrolyte showed a high bonding strength to the substrate up to 20 ± 2 MPa and the value was 15 ± 2 MPa for the amorphous coatings obtained in carbonate electrolyte. The micro hardness of the amorphous coating and the Fe₃O₄ coating was 1001 Hv and 1413 Hv, respectively, which was more than two and three times as that of the Q235 alloy substrate (415 Hv). The friction coefficient exhibited by amorphous coating and Fe₃O₄ coating was 0.13 and 0.11, respectively, both lower than the uncoated Q235 substrate which ranged from 0.17 to 0.35.     

Coating formation by plasma electrolytic oxidation on ZC71/SiC/12p-T6 magnesium metal matrix composite

Plasma electrolytic oxidation (PEO) of a ZC71/SiC/12p-T6 magnesium metal matrix composite (MMC) is investigated in relation to coating growth and corrosion behaviour. PEO treatment was undertaken at 350 mA cm⁻² (rms) and 50 Hz with a square waveform in stirred 0.05 M Na₂SiO₃.5H₂O/0.1 M KOH electrolyte. The findings revealed thick, dense oxide coatings, with an average hardness of 3.4 GPa, formed at an average rate of ∼1 μm min⁻¹ for treatment times up to 100 min and ∼0.2 μm min⁻¹ for later times. The coatings are composed mainly of MgO and Mg₂SiO₄, with an increased silicon content in the outer regions, constituting <10% of the coating thickness. SiC particles are incorporated into the coating, with formation of a silicon-rich layer at the particle/coating interface due to exposure to high temperatures during coating formation. The distribution of the particles in the coating indicated growth of new oxide at the metal/coating interface. The corrosion rate of the MMC in 3.5% NaCl is reduced by approximately two orders of magnitude by the PEO treatment.     

Deposition and characterization of TiAlSiN nanocomposite coatings prepared by reactive pulsed direct current unbalanced magnetron sputtering

This work reports the performance of high speed steel drill bits coated with TiAlSiN nanocomposite coating at different Si contents (5.5-8.1 at.%) prepared using a four-cathode reactive pulsed direct current unbalanced magnetron sputtering system. The surface morphology of the as-deposited coatings was characterized using field emission scanning electron microscopy. The crystallographic structure, chemical composition and bonding structure were evaluated using X-ray diffraction, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, respectively. The corrosion behavior, mechanical properties and thermal stability of TiAlSiN nanocomposite coatings were also studied using potentiodynamic polarization, nanoindentation and Raman spectroscopy, respectively. The TiAlSiN coating thickness was approximately 2.5-2.9 μm. These coatings exhibited a maximum hardness of 38 GPa at a silicon content of approximately 6.9 at.% and were stable in air up to 850 °C. For the performance evaluation, the TiAlSiN coated drills were tested under accelerated machining conditions by drilling a 12 mm thick 304 stainless steel plate. Under dry conditions the uncoated drill bits failed after drilling 50 holes, whereas, TiAlSiN coated drill bits (Si = 5.5 at.%) drilled 714 holes before failure. Results indicated that for TiAlSiN coated drill bits the tool life increased by a factor of more than 14.