The significance of passivation treatments on AISI 314 foam pieces to be used as substrates for catalytic applications

Several properties of metallic foams such as their low density, high mechanical strength and good coefficients of heat and mass transfer make them attractive for applications in catalysis. Important modifications in the composition and morphology of the metallic foam surfaces can take place when they are submitted to treatments at high temperatures. These surface changes are due to the migration of some elements from the metallic core to the pore surface, thus inducing a passivation via an oxide layer formation. This new layer avoids further metallic segregation and generates a surface roughness, both effects having a significant impact on the catalytic coating quality. This work analyzes the effects of calcination temperature and time on the chemistry and morphology of the metallic surface corresponding to the AISI 314 stainless steel foams of 50 and 60 ppi. The chemical and morphological surface changes were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy-Dispersive X-Ray (EDX) analysis and Laser Raman Spectroscopy (LRS). The application of high temperature treatments on AISI 314 foams promotes the formation of a surface layer containing chromium oxide and spinel-type compounds of chromium, iron and manganese. The optimum treatment temperature for this type of structures seems to be 900 °C because both the adhesion and thickness of the layer formed are adequate. For the sample with smaller pores (60 ppi) the optimal treatment time is close to 2 h and for that with larger pores (50 ppi) the recommended time is 20 h. Under these conditions, a compromise is found between adhesion, thickness and surface roughness, suitable for the subsequent deposition of catalytic material.     

Microstructures and electrical properties of La0.8Sr0.2MnO3 films synthesized by sol-gel method

La_0.8Sr_0.2MnO₃ (LSMO) thin films were fabricated on alumina substrates by an improved sol-gel dip-coating process. It was found that multiple dip-coating process could not be performed until the pre-firing temperature reached 600 °C. Different amounts of LSMO powders were added to precursor solution with an aim to avoid cracks in LSMO thin films during calcining caused by the shrinkage mismatch between the film and the substrate. The structure and surface morphology of the films prepared from precursors with and without LSMO powders were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). It was found that the addition of 56.4 wt.% LSMO powders into the sol-gel precursor solution significantly modified the microstructure of films. A single LSMO perovskite phase was obtained on alumina substrate after calcining at 800 °C for 4 h by the improved sol-gel method. The sheet resistance of the films prepared with different processing parameters was measured by four-point dc method. Results indicated that the sheet resistance of films decreased with increasing the number of coating applications and the amount of LSMO powders.     

Preparation of uniform TiO2 nanostructure film on 316L stainless steel by sol-gel dip coating

Sol was prepared by the mixing of tetra-η-butyle titanat, ethyl aceto acetate, and ethanol in an optimized condition. Polished 316L specimens were coated with the sol by dip-coating method. The influences of drying condition, withdrawal speed, calcination temperature, addition of dispersant, and pH of sol on TiO₂ nanostructure coating were investigated. Choosing of alcohol as drying atmosphere hindered the crack formation. The relation between coating thickness and withdrawal speed was evaluated. The optimum temperature to create a uniform distribution of nanoparticles of anatase was derived as 400 °C. Average roughness of coating was found about 10.61 nm by AFM analysis. Dispersant addition promoted formation of a uniform film as well as prevention of agglomeration. Acidic sol provided smaller particles than neutral sol.     

Microstructure evolution of sol-gel HA films

Bioactive hydroxyapatite films were fabricated on titanium alloy by a sol-gel method. The samples were firstly precoated at a low drying temperature for many times and then calcined at a relative high temperature. The phase constitution, microstructure and composition analysis were studied by X-ray diffraction (XRD), electronic probe microanalysis (EPMA), and the microstructure evolution was explained by some schematic illustrations. When the samples were precoated only once, hexagonal structure is always observed. After the samples were precoated many times, the hexagonal structure can be preserved only when the drying temperature is 500 °C or above. When the drying temperature is below 500 °C, the dried layer easily redissolved into the next coated sol because of the existence of some water-soluble ions such as NO₃⁻, consequently the hexagonal structure disappeared and a coarse surface with some small pores formed. High calcining temperature can accelerate the atomic diffusion which may integrate the adjacent grains, but excessively high temperature such as 900 °C or above would make the whole film be incinerated completely.     

The effect of non-contact heating (microwave irradiation) and contact heating (annealing process) on properties and performance of polyethersulfone nanofiltration membranes

In this work the effect of microwave irradiation on morphology and performance of polyethersulfone (PES) membranes was investigated. The membranes were prepared with 20 wt.% of PES by phase inversion method. N,N-dimethylformamide (DMF) and mixture of water and ethyl alcohol (90/10 vol.%) were employed as solvent and coagulant respectively. Polyvinylpirrolidone (PVP) with the concentration of 2 wt.% was selected as pore former. The effects of irradiation time (10, 30, 60, 90, 120 s) and microwave power (180, 360, 720 and 900 W) on structure and performance of membranes were studied. Increasing the irradiation time and power caused variation in permeate flux and ion rejection. Moreover, the effects of annealing processes (60, 70, 80 °C) were studied. Transmembrane pressure was selected around 1.5 MPa for all experiments. Scanning electron microscope (SEM) and atomic force microscope (AFM) were employed to describe the surface morphology of the prepared membranes. The effect of microwave irradiation time in different power revealed alterations in membrane surface morphology and AFM images represented that surface parameters (such as surface roughness) have been changed. The membrane exhibited moderate rejection (47%) and low permeate flux (4.5 kg/m² h) at 80 °C for NaCl solution. The SEM images indicate that the dense skin layer is formed at 80 °C annealing.     

Vanadium carbide coatings on die steel deposited by the thermo-reactive diffusion technique

Thermal reactive diffusion coating of vanadium carbide on DIN 1.2367 die steel substrate was performed in a powder mixture consisting of ferro-vanadium, ammonium chloride, alumina and naphthalene at 950, 1050 and 1150 °C for 1-5 h. The carbide layers were characterized by means of microstructure, microhardness, X-ray diffraction and chemical analysis. Depending on the coating process time and temperature, the thickness of the vanadium carbide layer formed on the substrate ranged from 2.3 to 23.2 μm. The hardness of vanadium carbide layers was about 2487 HV. Dry wear tests for uncoated and coated DIN 1.2367 die steel were carried out on pin-on-disk configuration and at a sliding speed of 0.13 m/s. The results showed superior wear properties of the coated samples. The kinetics of vanadium carbide coating by the pack method was also studied and the activation energy for the thermo-reactive diffusion process was estimated to be 173.2 kJ/mol.     

High-temperature oxidation of CrN/AlN multilayer coatings

Experiments are reported on sputter depth profiling of CrN/AlN multilayer abrasive coatings by secondary ion mass spectrometry (SIMS) coupled with sample current measurements (SCM). The coatings were deposited by a closed-field unbalanced magnetron sputtering. It is shown that after oxidation tests, performed in air at 900 °C for 2 h and at 1100 °C for 4 h, the layered structure begins to degrade but is not destroyed completely. Oxidation at 1100 °C for 20 h causes total destruction of the coatings that can be attributed to a fast diffusion of oxygen, nickel, manganese and other elements along defect paths (grain boundaries, dislocations, etc.) in the coating. There are practically no nitrides in the near-surface layer after such a treatment and all the metallic components are in the oxidized form as follows from the data obtained by X-ray photoelectron spectroscopy (XPS). According to XPS and mass-resolved ion scattering spectrometry (MARISS), the surface content of Al in the heat-treated coatings has decreased in comparison with the as-received sample and that of Cr increased. Both XPS and MARISS data exhibit real increase in superficial concentration of the substrate materials (Mn and Ni) that is controversial if using SIMS alone. SCM turned out to be an informative depth profiling method complementary to more expensive and complicated SIMS, being particularly useful for structures with different secondary electron emission properties of the layers. SCM with predetermined SIMS calibration allows a routine characterization of coatings and other multilayer structures, particularly, in situations where the expenses of analysis can be justified.     

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.     

Economical synthesis of nanocrystalline alumina using an environmentally low-cost binder

Sol-gel, a commonly used technique, involves the formation of an amorphous gel from a precursor solution. In this research nanocrystalline alumina powders have been synthesized through a new sol-gel simplified method. The route involved using an environmentally low-cost binder and aluminum nitrate in an aqueous medium. The added metal ions were dispersed in the gelled binder matrix. The gelled mass was dried and characterized by simultaneous thermogravimetric and differential thermal analysis (TG-DTA) and calcined at 350, 400, 530, 650, and 900 °C for 2 h. The samples were evaluated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The used binder can be applied to form a perfect matrix for the entrapment of metal ions that during heat treatment, gives rise to ultrafine amorphous or crystalline alumina particles. In this study, the transition phases of alumina with particle sizes of 15-25 nm as well as aluminum oxide hydrate phase were produced by the heat treatment of the gelled mass at temperature 650 °C. By increasing the calcinations temperature to 900 °C, alumina transition phases were changed and aluminum oxide hydrate eliminated. The particle sizes at this temperature were obtained in the range 15-30 nm. The particle size and crystallite size of products measured from XRD and TEM were in good agreement.     

Effect of magnesium addition on the wetting of alumina by aluminium

In this report the wetting behaviour between polycrystalline alumina substrates and molten aluminium doped with magnesium as a wetting agent has been studied using the sessile drop technique. The time required for equilibrium attainment is investigated. To explore the formation of possible phases at the interface, electron microscopic studies along with EDX analysis have been employed. It is found that magnesium reduces the time and temperature required for equilibrium in the Al/Al₂O₃ system. The Al-7 wt% Mg and Al-10 wt% Mg alloys can wet alumina at temperatures as low as 900 °C. It is also found that molten aluminium doped with magnesium can wet polycrystalline alumina at temperatures below 1000 °C. A thin reaction layer was observed at the Al-Mg/Al₂O₃ interface in the present study.     

Improvement of corrosion resistance of nitrided low alloy steel by plasma post-oxidation

Post-oxidizing treatments can be performed to improve the corrosion resistance of nitrided steel samples. In this paper, plasma nitriding treatments were performed at 540 °C for 4 h using ammonia as the working gas, and plasma post-oxidizing treatments were carried out at temperatures ranging from 350 °C to 500 °C for 2 h in oxygen gas. The treated samples were characterized by using optical microscopy, SEM, XRD, and electrochemical polarization. The X-ray analysis revealed the formation of iron-nitride phases of ?-Fe_2-3N and γ′-Fe₄N during plasma nitriding and iron oxide phases of hematite (Fe₂O₃) and magnetite (Fe₃O₄) through the post-oxidizing treatment. In particular, it was found that the very thin magnetite layer 0.8-1.5 μm in thickness on top of the compound layer was obtained by plasma post-oxidized at 400 °C and 450 °C. It was also demonstrated that the corrosion characteristics of the nitrided compound layer were further improved by post-oxidation treatment.     

The effect of heat treatment on the physical properties of sol-gel derived ZnO thin films

Zinc oxide (ZnO) thin films were deposited on microscope glass substrates by sol-gel spin coating method. Zinc acetate (ZnAc) dehydrate was used as the starting salt material source. A homogeneous and stable solution was prepared by dissolving ZnAc in the solution of monoethanolamine (MEA). ZnO thin films were obtained after preheating the spin coated thin films at 250 °C for 5 min after each coating. The films, after the deposition of the eighth layer, were annealed in air at temperatures of 300 °C, 400 °C and 500 °C for 1 h. The effect of thermal annealing in air on the physical properties of the sol-gel derived ZnO thin films are studied. The powder and its thin film were characterized by X-ray diffractometer (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure (JCPDS 36-1451) and show the c-axis grain orientation. Increasing annealing temperature increased the c-axis orientation and the crystallite size of the film. The annealed films are highly transparent with average transmission exceeding 80% in the visible range (400-700 nm). The measured optical band gap values of the ZnO thin films were between 3.26 eV and 3.28 eV, which were in the range of band gap values of intrinsic ZnO (3.2-3.3 eV). SEM analysis of annealed thin films has shown a completely different surface morphology behavior.     

The preparation of c-axis epitaxial Bi-2212 films on STO(1 0 0) by sol-gel method

Bi₂Sr₂Ca₁Cu₂O_8+δ (Bi-2212) films were grown on (1 0 0) oriented SrTiO₃ (STO) substrate using sol-gel spin-coating method. The effects of heat treatment conditions and coating times on the phase formation and surface morphology were investigated using thermal analysis, optical microscope, X-ray diffraction, and scanning electronic microscopy. Mixed phases were formed from 820 to 840 °C, and Bi-2212 single phase was obtained at 830 °C for 3 h. c-axis epitaxial films with smooth surfaces were obtained by drying at 600 °C and coating for 5 times.     

Effect of nanoscale thin films of Dy2Fe14B on the magnetic hysteresis characteristics of melt-spun ribbons of Nd2Fe14B

The effectiveness of nanoscale Dy₂Fe₁₄B thin films on coercivity and energy product of melt-spun ribbons of Nd₂Fe₁₄B at high temperatures was investigated. It is hypothesized that the nanoscale Dy-thin film will act as an obstacle for the nucleation of reverse domains and also maximize the energy of domain walls and thereby improve the magnetic performance at high temperatures. Pulsed laser deposition (PLD) of amorphous Dy₂Fe₁₄B layers on Nd₂Fe₁₄B melt-spun ribbons was performed for a nominal thickness of 40 nm. The coated ribbons were then annealed in environmentally controlled quartz furnace at two different cycles (750 °C for 15 min and 900 °C for 2 h) to cause crystallization. Magnetic hysteresis tests conducted at 300 and 400 K revealed that there is small but consistent improvement in the magnetic properties of the coated ribbons annealed at 750 °C for 15 min. However, higher temperature annealing (900 °C for 2 h) drastically reduced the magnetic properties. The incomplete recrystallization of amorphous structure at 750 °C for 15 min and large grain growth and formation of non-magnetic phases at 900 °C for 2 h are believed to be responsible for not meeting the expected magnetic performance.     

Chemical reactivity of PVD-coated WC-Co tools with steel

The chemical reactivity of CrN, ZrN, TiC_xN_1−x and naCo^® PVD coatings on a WC-Co cemented carbide substrate with steel has been evaluated by means of the static interaction couples technique. Diffusion experiments with coated and uncoated tools were carried out at 900, 1100 and 1300 °C in order to establish the maximum temperature at which the substrate-coating-workpiece combinations are chemically stable. Computational equilibrium thermodynamics was used to identify the interaction products formed at elevated temperature and the chemical solubility of the different coating materials into iron. A metallic (Fe, Co) fcc solid solution was identified at the steel side of the interface from 1100 °C on for all the coated tools and from 900 °C for the uncoated carbide. In addition to this interaction product, the ?-carbide was identified at 1300 °C on the WC-Co side of the interface. Both of the experimental findings and thermodynamic equilibrium solubility calculations demonstrated that the PVD-coated WC-Co tools exhibit a lower chemical reactivity with respect to the uncoated tools.     

Thermal expansion coefficient of alumina films developed by oxidation of a FeCrAl alloy determined by a deflection technique

Thermal expansion coefficients of α alumina films formed by oxidation of an oxide dispersion strengthened (ODS) FeCrAl alloy have been determined between 20 and 900 °C using an original deflection test. This technique is based on the curvature of a dissymmetrical sample consisting of a thin and elongated metallic substrate covered on one of its large sides by an oxide film. The average value of the expansion coefficient of the compact columnar α alumina film is found to equal 10.3 × 10⁻⁶ K⁻¹ which is higher than most values given in the literature.     

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.     

Effect of reaction parameters on the growth of MWCNTs using mesoporous Sb/MCM-41 by chemical vapour deposition

Mesoporous Si-MCM-41 molecular sieve was synthesized hydrothermally and different wt.% of Sb (1.0, 2.0, 3.0, 5.0, 10.0, 15.0 and 20.0) was loaded on it by wet impregnation method. The Sb/MCM-41 materials were characterized by various physico-chemical techniques such as XRD, TGA and TEM. The TEM image showed a honeycomb structure of the host material. They were used as catalytic templates for the growth of MWCNTs by CVD method with different temperatures at 700, 800, 900 and 1000 °C using acetylene as a carbon precursor. The reaction temperature was optimized for the better formation of MWCNTs and they were purified and then characterized by XRD, SEM, HR-TEM and Raman spectroscopy techniques. The formation of MWCNTs with diameter in the range of 4−6 nm was observed from HR-TEM. The good thermal stability and high productivity of catalyst observed in this study revealed that the 2 wt.% Sb loaded MCM-41 could be a promising support for the catalytic synthesis of MWCNTs at 800 °C by CVD method.     

Preparation and properties of electroless Ni-P-SiO2 composite coatings

Dispersible SiO₂ nanoparticles were co-deposited with electroless Ni-P coating onto AISI-1045 steel substrates in the absence of any surfactants in plating bath. The resulting Ni-P/nano-SiO₂ composite coatings were heat-treated for 1 h at 200 °C, 400 °C, and 600 °C, respectively. The hardness and wear resistance of the heat-treated composite coatings were measured. Moreover, the structural changes of the composite coatings before and after heat treatment were investigated by means of X-ray diffraction (XRD), while their elemental composition and morphology were analyzed using an energy dispersive spectrometer (EDS) and a scanning electron microscope (SEM). Results show that co-deposited SiO₂ particles contributed to increase the hardness and wear resistance of electroless Ni-P coating, and the composite coating heat-treated at about 400 °C had the maximum hardness and wear resistance.     

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.