Influence of post-treatment on the corrosion resistance of PEO coated AM50B and AM60B Mg alloys

Magnesium alloys are highly reactive and require protection for their successful applications. In this work, coatings of 10 μm and 25 μm nominal thicknesses were prepared by Plasma Electrolytic Oxidation on AM50B and AM60B alloys. The effect of subsequent post-PEO treatments such as alkaline phosphate, alkaline silicate and sol-gel sealing was studied on coatings with 10 μm thickness. The microstructure and composition of the PEO coatings and post-treated coatings were analysed by Scanning Electron Microscope and Energy Dispersive X-ray Spectroscopy. Phase analysis of the coatings was carried out using X-ray Diffraction method. Potentiodynamic polarization method was used to evaluate the corrosion behaviour of these coatings in 3.5% NaCl solution. Electrochemical corrosion results indicated that the sealed PEO coatings of 10 μm thickness showed better corrosion resistance than the unsealed PEO coatings of 25 μm thickness. The structural surface defects of the PEO coatings were sealed by post-treatments resulting in decreases in surface roughness and open pores. Sol-gel post-treatment provided the most effective sealing to the PEO coatings.     

The effect of nitric acid surface treatment on CaP deposition of Ti6Al4V open-cell foams in SBF solution

The effect of nitric acid surface treatment on CaP deposition of an open-cell Ti6Al4V foam (60% porous and 300-500 ?m in pore size), prepared by means of the space holder method using 94 and 66 μm average particle size powders, was investigated in a simulated body fluid (SBF) solution up to 14 days. Although, nitric acid surface treatment did not change the foam flat surface roughness values significantly, it increased surface area difference greatly by introducing nano scale undulations on the surface. The increased surface area difference was found to be more pronounced in smaller particle size foam samples. A continuous relatively thin CaP coating layer formed after 5 and 14 days of SBF immersion in nitric acid surface treated small and larger average particle size foam specimens, respectively. Whereas, the cells of untreated foam specimen were observed to be filled with CaP precipitates and a continuous CaP layer development was found after 14 days of SBF immersion. These results were also confirmed with the grazing incidence XRD and FTIR analysis of SBF immersed specimens.     

Infrared emissivity of Sr doped lanthanum manganites in coating form

The Sr doped lanthanum manganite coatings were prepared using La_0.8Sr_0.2MnO₃ particles and epoxy modified polyurethane as pigment and resin matrix, respectively. The structure, morphology, surface roughness and infrared normal emissivity (?_N) in the 3-5 and 8-14 μm wavebands of the samples were systematically investigated. With the increase of La_0.8Sr_0.2MnO₃ pigment, the ?_N of the coatings decreases and the ?_N values in the 8-14 μm waveband are higher than those in the 3-5 μm waveband. The surface roughness has no significant effect on the infrared emissivity of LSMO coatings. For 50% LSMO coating, the sample shows variable-emissivity property in the 8-14 μm waveband and the emissivity property remains unchanged before and after ultraviolet irradiation.     

Characterization of thick ceramic and cermet coatings deposited by an industrial-scale LAFAD process

The unidirectional LAFAD dual-arc vapor plasma source yields 100% ionized metal vapor plasma flow and more than 50% ionized gaseous plasma in the coating chamber. The LAFAD technology deposits thick ceramic and cermet coatings with multi-elemental nanostructured architectures, nearly defect-free morphology and atomically smooth surfaces at high deposition rates. The productivity of one unidirectional LAFAD vapor plasma source integrated into an industrial-scale batch coating system ranges from 3-4 µm/h for nitride base coatings and up to 6 µm/h for oxi-ceramic coatings with good uniformity over large deposition areas, making it an attractive alternative to other PVD processes for a wide variety of applications. The 20 µm to 100 μm monolithic and Ti/TiN microlaminated LAFAD coatings exhibit low residual compressive stresses, i.e. < 1.5 GPa, resulting in exceptionally good adhesive and cohesive toughness. The fracture resistance of ultra-thick LAFAD coatings vs. coating architecture will be discussed.     

Effect of Slurry Composition on Plate Weight in Ceramic Shell Investment Casting

This paper deals with the study of the effect of primary slurry parameters on the plate weight (ceramic retention test) in ceramic shell investment casting process. Four controllable factors of the zircon flour and fused-silica powder based slurries were studied at three levels each by Taguchi’s parametric approach and single-response optimization of plate weight was conducted to identify the main factors controlling its stability. Variations in coating thickness with plate weight were calculated for each slurry and ceramic shell moulds were made on wax plate using primary slurry and coarse fused-silica sand as stucco. The Scanning Electronic Microscopy (SEM) technique has been used to study the surface morphology of zircon flour and fused silca powder particles as well as primary coating (shell surface). X-ray Diffraction (XRD) analysis was done to identify the various phases present in the ceramic slurry coating. Optical profilometer has been used to measure the surface roughness of the shells. The result reveals that the surface condition of shell can be improved by increasing the plate weight, corresponding to higher filler loading in the slurry. Confirmation experiments were conducted at an optimal condition showed that the surface quality of the ceramic shell mould were improved significantly. Castings were produced using Al-7%Si alloy in recommended parameters through ceramic shell investment casting process. Surface roughness of the produced casting were measured and presented in this paper.     

Effect of microplasma modes and electrolyte composition on micro-arc oxidation coatings on titanium for medical applications

A method of micro-arc oxidation (MAO) has been used for the obtaining of the bioactive calcium-phosphate coatings on the surface of nanostructured titanium. A homogeneous alkaline electrolyte containing phosphate ions and calcium (II) complexes with EDTA was used. An effect of changes of current modes on the coating characteristics has been studied. Obtained coatings have the molar ratio Ca/P up to 1.5 and include the phase of calcium phosphate β-Ca₃(PO₄)₂. The adhesion strength of coatings to the titanium substrate is in the range 10-35 MPa, the thickness is up to 100 μm. The experiments in vivo have been carried out. They have shown 75% probability of new bone tissue growth on coatings with roughness of 2.5-5.5 μm.     

Effect of the suspension composition on the microstructural properties of high velocity suspension flame sprayed (HVSFS) Al2O3 coatings

Seven different Al₂O₃-based suspensions were prepared by dispersing two nano-sized Al₂O₃ powders (having analogous size distribution and chemical composition but different surface chemistry), one micron-sized powder and their mixtures in a water + isopropanol solution. High velocity suspension flame sprayed (HVSFS) coatings were deposited using these suspensions as feedstock and adopting two different sets of spray parameters.The characteristics of the suspension, particularly its agglomeration behaviour, have a significant influence on the coating deposition mechanism and, hence, on its properties (microstructure, hardness, elastic modulus). Dense and very smooth (Ra ~ 1.3 μm) coatings, consisting of well-flattened lamellae having a homogeneous size distribution, are obtained when micron-sized (~ 1-2 μm) powders with low tendency to agglomeration are employed. Spray parameters favouring the break-up of the few agglomerates present in the suspension enhance the deposition efficiency (up to > 50%), as no particle or agglomerate larger than ~ 2.5 μm can be fully melted. Nano-sized powders, by contrast, generally form stronger agglomerates, which cannot be significantly disrupted by adjusting the spray parameters. If the chosen nanopowder forms small agglomerates (up to a few microns), the deposition efficiency is satisfactory and the coating porosity is limited, although the lamellae generally have a wider size distribution, so that roughness is somewhat higher. If the nanopowder forms large agglomerates (on account of its surface chemistry), poor deposition efficiencies and porous layers are obtained.Although suspensions containing the pure micron-sized powder produce the densest coatings, the highest deposition efficiency (~ 70%) is obtained by suitable mixtures of micron- and nano-sized powders, on account of synergistic effects.     

Corrosion and tribocorrosion behaviour of thermally sprayed ceramic coatings on steel

This research aims at investigating the corrosion and tribocorrosion behaviour of thermally sprayed ceramic coatings deposited on steel specimens and exposed to a 3.5% NaCl solution. The coatings have been prepared by plasma spraying Cr₂O₃ and Al₂O₃/13% TiO₂ powders on a Ni/20% Cr bond coating. Combined wear-corrosion conditions have been achieved by sliding an alumina antagonist on the lateral surface of coated steel cylinders, during their exposure to the aggressive solution.Polarization resistance values monitored during 3 days exposures and polarization curves recorded at the end of the immersion period show that both coatings only partially protect steel substrate from corrosion. Sliding conditions (under 2 N load and 20 rpm or 10 N and 100 rpm) induce a limited increase of the substrate corrosion rates, likely as a consequence of an increase in the defect population of the ceramic coatings.On Cr₂O₃-coated specimens, tribocorrosion is more severe at 10 N and 100 rpm, while on Al₂O₃/13% TiO₂-coated specimens, a stronger corrosion attack is achieved at 2 N and 20 rpm. Profilometer analysis and wear track observations by optical and scanning electron microscopes evidence that on both coatings abrasion of the surface asperities produce both a surface polishing effect and, at high loads, the formation of a tribofilm, more continuous on Al₂O₃/13% TiO₂. On this coating the tribofilm reduces the amount of surface defects and limits the corrosion attack to a certain extent.     

The structure and high temperature corrosion performance of medium-thickness aluminide coatings on nickel-based superalloy GTD-111

Simple and Si-modified aluminide coatings having medium-thickness (40-60 μm) have been applied on the superalloy GTD-111 by a slurry technique. Hot corrosion and cyclic oxidation performance of the uncoated and the coated superalloy were investigated by exposing samples to a molten film of Na₂SO₄-40 %wt NaVO₃-10%wt NaCl at 780 °C and 1 h cyclic oxidation at 1100 °C in air, respectively. The presence of silicon in the aluminide structure increased the oxidation resistance by a factor of 1.7 times. In addition, a SiO₂-containing scale, which formed on the Si-containing coating surface, was stable during of the hot corrosion testing.     

基于泡沫模原型的消失模复合型壳制备工艺

利用发泡成型工艺制备高质量的泡沫模原型,在泡沫模表面制作2～3层硅溶胶-水玻璃复合陶瓷型壳,之后采用自硬水玻璃砂作陶瓷型壳背衬。陶瓷型壳在200～250℃保温30min失模及二氯甲烷溶剂溶失方式失模,焙烧工艺为800℃保温1h。结果表明,该制壳工艺简单、周期短、成本低,制得复合型壳表面光洁、强度高,并浇注出了质量较高的ZL101合金铸件。     

Ceria/stannate multilayer coatings on AZ91D Mg alloy

In this work, CeO₂/stannate multilayer coatings on AZ91D magnesium alloy were successfully obtained by chemical conversion and sol–gel dip coating. The stannate conversion coatings were prepared from a stannate aqueous bath containing Na₂SnO₃, CH₃COONa, Na₃PO₄ and NaOH at different temperatures and immersion times. Ceria films were produced on stannate/AZ91D starting from Ce(III) nitrate solutions in H₂O. In some cases, the PVA was added as chelating agent. Ceria top coatings were fired at 200 °C for 1 h. Coating microstructure was examined by FE-SEM. Finally, the corrosion resistance features of the coatings were tested by the electrochemical impedance spectroscopy (EIS) in 3 wt.% NaCl solution. The effect of PVA addition was evaluated in terms of microstructure and corrosion resistance features. CeO₂/stannate multilayer films, 3 μm thick, uniform, well adherent and nearly crack free were obtained. The formation of CeO₂ phase was confirmed by XRD and XPS analyses. The XPS depth profiles showed a limited diffusion of Mg towards the ceramic film. The EIS tests showed a significant improvement of corrosion resistance of the multilayer coatings (~ 16.6 kΩ after 48 h in NaCl solution) with respect to the blank alloy (~ 2.4 kΩ after 48 h in NaCl solution).     

薄壁光整消失模壳型铸造的型壳研究

试验研究了壳型制备中不同黏结剂、不同耐火粉料及粉液比对泡沫消失模型壳强度和表面粗糙度的影响.采用在型壳表面添加水玻璃砂背衬的方法,减少了(硅溶胶)型壳层数、缩短了制壳周期、提高了型壳强度.针对消失模壳型铸造用型壳表面质量要求高的问题,探讨了改善泡沫模表面粗糙度的工艺方法.通过优化蒸汽发泡成形工艺参数和在模样表面涂上光整剂等措施降低了模样表面粗糙度.为制造基于泡沫消失模的薄壁光整壳型奠定了初步基础.     

真空低压消失模壳型铸件表面质量改善研究

系统地考察了泡沫模表面质量、型壳表面质量以及金属与铸型间的润湿等因素对铸件表面质量的影响规律,并提出相应的改善措施.结果表明:泡沫模珠粒间的沟槽对型壳及铸件表面质量造成较大的影响.通过在泡沫模表面涂挂光洁剂,可以显著提高型壳和铸件的表面质量.增大泡沫模的密度也可以提高铸件的表面质量.涂料性能对铸件表面质量也有很大影响,硅溶胶型壳强度高、表面质量较好;随着粉料目数的增大,铸件表面质量不断提高.由于金属液与型腔不润湿,型腔与金属液间气膜的存在会对铸件表面质量有一定的影响,应设法消除或削弱气膜;采用真空和压力下浇注,可以减小气膜,提高铸件表面质量.     

Effect of superalloy substrate and bond coating on TBC lifetime

Several different single-crystal superalloys were coated with different bond coatings to study the effect of composition on the cyclic oxidation lifetime of an yttria-stabilized zirconia (YSZ) top coating deposited by electron beam physical vapor deposition from a commercial source. Three different superalloys were coated with a 7 μm Pt layer that was diffused into the surface prior to YSZ deposition. One of the superalloys, N5, was coated with a low activity, Pt-modified aluminide coating and Pt-diffusion coatings with 3 and 7 μm of Pt. Three coatings of each type were furnace cycled to failure in 1 h cycles at 1150 °C to assess average coating lifetime. The 7 μm Pt diffusion coating on N5 had an average YSZ coating lifetime > 50% higher than a Pt-modified aluminide coating on N5. Without a YSZ coating, the Pt-modified aluminide coating on N5 showed the typical surface deformation during cycling, however, the deformation was greatly reduced when constrained by the YSZ coating. The 3 μm Pt diffusion coating had a similar average lifetime as the Pt-modified aluminide coating but a much wider scatter. The Pt diffusion bond coating on superalloy X4 containing Ti exhibited the shortest YSZ coating lifetime, this alloy-coating combination also showed the worst alumina scale adhesion without a YSZ coating. The third generation superalloy N6 exhibited the longest coating lifetime with a 7 μm Pt diffusion coating.     

Method to determine hot permeability and strength of ceramic shell moulds

This paper reports on an improved method to evaluate both the strength and the permeability of ceramic shell specimens under high temperature conditions. In order to maintain safe testing conditions and use lower testing pressure, a spherical wax model, larger than the standard ping-pong ball, was used to prepare ceramic shells. Compressed air was introduced into ceramic shell specimen held at 900 °C. Air flow and pressure drop across the shell wall were measured and hot permeability was calculated according to Darcy's law. Air pressure was subsequently increased and recorded up to bursting point. A hoop stress formula was used to calculate the hot strength from the bursting pressure. This very simple method is easy to implement in foundries.     

Effect of surface nanocrystallization on the microstructural and corrosion characteristics of AZ91D magnesium alloy

Surface distinct deformed layers with thicknesses up to 150 μm, with grain size in the top most surface is in the nanometer scale, were produced on AZ91D magnesium alloy using surface mechanical attrition treatment (SMAT). Effects of different ball size on the properties of the SMATed samples were investigated. The microstructural, grain size, hardness and roughness features of the treated surfaces were characterized using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), micro-indenter and digital roughness meter, respectively. Corrosion behavior of the samples was evaluated using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. It is found that the ball diameter does not have a significant effect on the top surface grain size, but the thickness of the deformed layer increases with increase of ball size, from 50 μm for 2 mm balls to 150 μm for 5 mm balls. For all of the SMATed samples, the top surface microhardness value increased significantly and did not show any obvious change for samples treated with different balls. Corrosion studies show that the corrosion resistance of the sample treated with 2 mm balls is higher than that of those treated with 3 mm and 5 mm balls. This can be mainly attributed to the surface roughness and defects density of the samples, which are higher for the SMATed samples with 3 mm and 5 mm balls compared with that of sample SMATed with 2 mm balls.     

Synthesis of diamond-like carbon coatings on aluminum 6061 T-91 substrates by laser sintering of ultra-nanocrystalline diamond powders

Diamond-like carbon (DLC) coatings have been prepared on aluminum 6061 T-91 substrates with the aid of electrostatic spray deposition (ESD) of ultra-nanocrystalline diamond powders (2-8 nm) followed by direct laser sintering technique. A continuous-wave CO₂ laser was utilized, producing a dense, adherent DLC coating with a nominal thickness of 10 μm under optimal laser parameters that included laser power of 200 W, spot size of 1 mm by 0.1 mm and scanning speed of 254 mm/s. The evidence of DLC formation and its purity was obtained by characterizing the samples with Raman spectroscopy, X-ray diffraction and scanning electron microscopy/energy dispersive spectroscopy. Functional evaluation of DLC coatings was performed using scratch, micro-hardness, fracture toughness and surface roughness tests. Raman measurements showed the presence of a broader peak at around 1332 cm^− 1 (characteristic of pure diamond) for electrostatically deposited samples and the presence of DLC with a broad asymmetric hump in the region of 1000 to 1600 cm^− 1 for laser-sintered samples. X-ray diffraction and energy dispersive spectroscopy confirmed the presence of carbon phases in the coatings. Scanning electron microscopy examination showed a fairly uniform and dense coating with a nominal thickness of 10 μm and a heat affected zone of 60-80 μm. These coatings exhibited micro-hardness in the range of 2150 to 2350 kg/mm² when measured using a Vickers diamond pyramid indenter at a load of 0.5 N. In some localized regions, hardness of 9000 kg/mm² was obtained. Scratch tests revealed a fairly homogenous coating with strong adhesive nature having almost four times the average critical force when compared against the electrostatically deposited sample. Fracture toughness and surface roughness are well within the acceptable ranges of DLC coatings. The capability of laser sintering to produce thick DLC coatings with outstanding mechanical and tribological properties and excellent bonding with aluminum offers the possibility to tailor an extreme lightweight, strong and wear-resistant material.     

Nanoindentation on the surface of thermally sprayed coatings

The ability to quantify surface mechanical properties is valuable for assessing the quality of thermal spray coatings. This is especially important for prostheses where loading is placed directly on the surface. Hydroxyapatite was classified to small (20-40 μm), medium (40-60 μm) and large (60-80 μm) particle sizes and thermal sprayed to produce a coating from spread solidified hydroxyapatite droplets. It was revealed for the first time, that nanoindentation can be successfully used to determine the hardness and elastic modulus on the surface of well spread solidified droplets at the hydroxyapatite coating surface. Comparison with indentation results from polished cross-section exhibited comparable values and statistical variations. The hardness was 5.8 ± 0.6, 5.4 ± 0.5 and 5.0 ± 0.6 GPa on coatings produced from small, medium and large sized powder. Similarly, the elastic modulus decreased from 121 ± 7, 118 ± 7 to 114 ± 7 GPa, respectively. Use of several indentation loads gave comparable results with sintered hydroxyapatite suggesting good inter-splat bonding within the coating. MicroRaman spectroscopy and X-ray diffraction confirmed a larger degree of dehydroxylation for the smaller particles also revealing a lower elastic modulus. This shows the influence of particle size and possibly dehydroxylation of hydroxyapatite on the mechanical properties of the coating surface.     

Electrodeposition and tribological characterisation of nickel nanocomposite coatings reinforced with nanotubular titanates

Metal nanocomposite nickel coatings reinforced with regularly shaped nanotubular titanates (multi-layered wall structure with ca. 5 nm internal diameter and 30 to 500 nm tube length) were electrodeposited from a modified Watts nickel electrolyte. Tribological properties of the coatings are characterised via measurements of the coating hardness, surface friction, wear rate and elastic modulus. Surface microstructures of the coatings were imaged (SEM and TEM analyses). The nanotubular titanates were shown to be embedded within the bulk of the coating and some particles protruded from the top surface. The nanotubular titanates in the nickel coating acted akin to a cross-linked and mesh-like matrix to enhance the dispersion-strengthening mechanism against external load. Nanocomposite nickel coatings reinforced with nanotubular titanates have shown (a) ~ 22% reduction in surface friction against a spherical diamond tip, (b) ~ 29% enhancement in wear resistance in a 3-body slurry abrasive wear test (steel counter body and 5 μm SiC particles), (c) ~ 102% improvement in coating hardness and (d) ~ 26% improvement in elastic modulus when compared with a nickel coating containing irregularly shaped nanosized titanium dioxide particles.     

Deposition, characterization and performance evaluation of ceramic coatings on metallic substrates for supercritical water-cooled reactors

A series of ceramic coatings have been prepared on P91 substrates by spray pyrolysis processes and on Zr-2.5Nb substrates by a plasma electrolytic oxidation process. Preliminary results show that coatings obtained with different solution compositions and procedures can reduce the oxidation weight gain of P91 samples by factors of 2-10 for exposure times up to 500 h in deaerated supercritical water at 500 °C and 25 MPa. Results also show that the weight gain of a P91 sample with an alumina (Al₂O₃) coating is about nine times less than that of uncoated P91 after exposures for 400 h in deaerated supercritical water at 650 °C and 25 MPa. These results indicate that the Al₂O₃ coating shows promising results for preventing oxidation of P91 under supercritical water conditions. The samples with ceramic coatings on Zr-2.5Nb substrates show marginally improved corrosion resistance compared to the bare substrates.