Characterization of AISI 4140 borided steels

The present study characterizes the surface of AISI 4140 steels exposed to the paste-boriding process. The formation of Fe₂B hard coatings was obtained in the temperature range 1123-1273 K with different exposure times, using a 4 mm thick layer of boron carbide paste over the material surface. First, the growth kinetics of boride layers at the surface of AISI 4140 steels was evaluated. Second, the presence and distribution of alloying elements on the Fe₂B phase was measured using the Glow Discharge Optical Emission Spectrometry (GDOES) technique. Further, thermal residual stresses produced on the borided phase were evaluated by X-ray diffraction (XRD) analysis. The fracture toughness of the iron boride layer of the AISI 4140 borided steels was estimated using a Vickers microindentation induced-fracture testing at a constant distance of 25 μm from the surface. The force criterion of fracture toughness was determined from the extent of brittle cracks, both parallel and perpendicular to the surface, originating at the tips of an indenter impression. The fracture toughness values obtained by the Palmqvist crack model are expressed in the form K_C(π/2) > K_C > K_C(0) for the different applied loads and experimental parameters of the boriding process.     

Electrolytical production of Ni + Mo + Si composite coatings with enhanced content of Si

Ni + Mo + Si composite coatings were prepared by co-deposition of nickel with molybdenum and silicon powders from a nickel solution in which Mo and Si particles were suspended by stirring. The layers have been deposited on a carbon steel substrate (St3S) under galvanostatic conditions. The content of Si in deposited layers was about 2-5 wt.% depending on deposition current density and the value of electric charge. For comparison Ni + Mo composite coatings were obtained under analogous current conditions. Composite coatings of enhanced Si content (15 wt.%) were deposited from an electrolyte in which 40 g/dm³ of Si covered with electroless plated nickel was dispersed. Deposition current density was equal 0.1 A/cm² and the value of electric charge Q = 500 C/cm². The thickness of the coatings was about 100-300 μm depending on their kind, electric charge and the deposition current density. Surface and cross-section morphology were investigated by scanning electron microscope (SEM). All deposited coatings are characterized by great, developed surface area. No internal stresses causing their cracking were observed. Chemical composition of the layers was determined by X-ray fluorescence spectroscopy (XRF) method and quantitative X-ray analysis (QXRD). It was stated, that the content of molybdenum and silicon in Ni + Mo + Si coatings depends on deposition current density and the amount of the powder in bath. The results of structural investigation of the obtained layers by the X-ray diffraction (XRD) method show, that they consist in crystalline Mo or Mo and Si phases built into Ni matrix. Moreover, Ni + Mo + Si composite coatings were modified by thermal treatment. It has been found that the thermal treatment of Ni + Mo + Si composite coatings caused that the new phases (NiSi, Mo₂Ni₃Si and Ni₆Mo₆C_1.06) were obtained.     

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.     

Nanolayered multilayer coatings of CrN/CrAlN prepared by reactive DC magnetron sputtering

Single-phase CrN and CrAlN coatings were deposited on silicon and mild steel substrates using a reactive DC magnetron sputtering system. The structural characterization of the coatings was done using X-ray diffraction (XRD). The XRD data showed that both the CrN and CrAlN coatings exhibited B1 NaCl structure with a prominent reflection along (2 0 0) plane. The bonding structure of the coatings was characterized by X-ray photoelectron spectroscopy and the surface morphology of the coatings was studied using atomic force microscopy. Subsequently, nanolayered CrN/CrAlN multilayer coatings with a total thickness of approximately 1 μm were deposited on silicon substrates at different modulation wavelengths (Λ). The XRD data showed that all the multilayer coatings were textured along {2 0 0}. The CrN/CrAlN multilayer coatings exhibited a maximum nanoindentation hardness of 3125 kg/mm² at a modulation wavelength of 72 Å, whereas single layer CrN and CrAlN deposited under similar conditions exhibited hardness values of 2375 and 2800 kg/mm², respectively. Structural changes as a result of heating of the multilayer coatings in air (400-800 °C) were characterized using XRD and micro-Raman spectroscopy. The XRD data showed that the multilayer coatings were stable up to a temperature of 650 °C and peaks pertaining to Cr₂O₃ started appearing at 700 °C. These results were confirmed by micro-Raman spectroscopy. Nanoindentation measurements performed on the heat-treated coatings revealed that the multilayer coatings retained hardness as high as 2250 kg/mm² after annealing up to a temperature of 600 °C.     

Evaluation of boron mobility on the phases FeB, Fe2B and diffusion zone in AISI 1045 and M2 steels

The present study evaluates the growth kinetics of boride layers at the material surface on AISI 1045 and M2 steels during the paste boriding process. This surface hardening technique produces on the material two characteristic phases FeB, Fe₂B and a transition zone, denominated diffusion zone, in the layer/substrate interface. The thermochemical treatment was done at three different temperatures: 1193, 1223 and 1273 K with two treatment times: 2 and 6 h for the 1045 steel, and 1223, 1253 and 1273 K with the same treatment times for M2 steel, modifying the boron potentials in equilibrium at the substrates surfaces. Using the mass balance equation, and assuming a linear concentration profile at the interfaces, the mobility of boron was determined on both types of steels. The influence of boron potential, treatment time and temperatures is clearly observed on the growth kinetics of boride layers.     

Effects of hydrogen and oxygen on the electrochemical corrosion and wear-corrosion behavior of diamond films deposited by hot filament chemical vapor deposition

A diamond film was deposited on silicon substrate using hot filament chemical vapor deposition (HFCVD), and H₂ and O₂ gases were added to the deposition process for comparison. This work evaluates how adding H₂ and O₂ affects the corrosion and wear-corrosion resistance characteristics of diamond films deposited on silicon substrate. The type of atomic bonding, structure, and surface morphologies of various diamond films were analyzed by Raman spectrometry, X-ray diffraction (XRD) and atomic force microscopy (AFM). Additionally, the mechanical characteristics of diamond films were studied using a precision nano-indentation test instrument. The corrosion and wear-corrosion resistance of diamond films were studied in 1 M H₂SO₄ + 1 M NaCl solution by electrochemical polarization. The experimental results show that the diamond film with added H₂ had a denser surface and a more obvious diamond phase with sp³ bonding than the as-deposited HFCVD diamond film, effectively increasing the hardness, improving the surface structure and thereby improving corrosion and wear-corrosion resistance properties. However, the diamond film with added O₂ had more sp² and fewer sp³ bonds than the as-deposited HFCVD diamond film, corresponding to reduced corrosion and wear-corrosion resistance.     

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.     

Bilayer period effect on corrosion-erosion resistance for [TiN/AlTiN]n multilayered growth on AISI 1045 steel

The aim of this work is to study the electrochemical behavior, under a corrosion-erosion condition, of [TiN/AlTiN]_n multilayer coatings with bilayers periods of 1, 6, 12 and 24, deposited by a magnetron sputtering technique on Si (1 0 0) and AISI 1045 steel substrates.The TiN and AlTiN structure for multilayer coatings were evaluated via X-ray diffraction (XRD) analysis. Silica particles were used as an abrasive in the corrosion-erosion test within a 0.5 M H₂SO₄ solution at an impact angle of 30° over the surface. The electrochemical characterization was carried out using a polarization resistance technique (Tafel), in order to observe changes in the corrosion rate as a function of the bilayers number (n) or bilayer period (Λ). Corrosion rate values of 359 mpy in uncoated steel substrate and 1.016×10⁻⁶ mpy for substrate coated with [TiN/AlTiN]₂₄ under impact angle of 30° were found. This behavior was related with the mass loss curve for all coatings and the surface damage was analyzed using SEM images. These results indicate that TiN/AlTiN multilayer coatings deposited on AISI 1045 steel provide a practical solution for applications in erosive-corrosive environments.     

Corrosion behaviour of AISI 304 stainless steel with Cu coatings in H2SO4

The work addresses the influence of cementation and electrodeposition of copper coatings on the corrosion resistance of AISI 304 stainless steel immersed in 30 wt.% H₂SO₄ at temperatures of 25 and 50 °C. Corrosion process was evaluated by gravimetric tests, DC measurements and electrochemical impedance spectroscopy (EIS). The specimen surfaces were analysed by scanning electron microscopy, X-ray photoelectron spectroscopy (XPS) and X-ray diffraction. The corrosion performance of AISI 304 stainless steel in sulphuric acid solution was greatly improved by copper coatings. The amount of copper deposited by the cementation process was sufficient to protect the stainless steel of corrosion. A greater amount of copper obtained by electrodeposition treatments does not supply further improvement in the corrosion behaviour. The improved corrosion resistance is related to copper dissolution at the initial stages of immersion tests and the presence of Cu²⁺ in the solution, which makes the medium more oxidizing, increasing the stability of the passive layer. In addition, the presence of copper at the surface reduces the overpotential of cathodic reaction, enabling the transition from an active region to the passive one.     

Preparation and annealing study of TaNx coatings on WC-Co substrates

To prevent Co diffusion from cemented carbides at high temperatures, we fabricated TaN_x coatings by reactive direct current (d.c.) magnetron sputtering onto 6 wt.% cobalt cemented carbide substrates, to form diffusion barrier layers. Varying the nitrogen flow ratio, N₂/(Ar + N₂), from 0.05 to 0.4 during the sputtering process had a significant effect on coating structure and content. Deposition rate reduced as the nitrogen flow ratio increased. The effects of nitrogen flow ratio on the crystalline characteristics of the TaN_x coatings were examined by X-ray diffraction. The TaN_x coatings annealing conditions were 500, 600, 700, and 800 °C for 4 h in air. We evaluated the performance of the diffusion barrier using both Auger electron spectroscopy depth-profiles and X-ray diffraction techniques. We also investigated oxidation resistance of the TaN_x coatings annealed in air, and under a 50 ppm O₂-N₂ atmosphere, to evaluate the fabricated layers effectiveness as a protective coating for glass molding dies.     

Microstructure and antibacterial properties of microwave plasma nitrided layers on biomedical stainless steels

Nitriding of AISI 303 austenitic stainless steel using microwave plasma system at various temperatures was conducted in the present study. The nitrided layers were characterized via scanning electron microscopy, glancing angle X-ray diffraction, transmission electron microscopy and Vickers microhardness tester. The antibacterial properties of this nitrided layer were evaluated. During nitriding treatment between 350 °C and 550 °C, the phase transformation sequence on the nitrided layers of the alloys was found to be γ → (γ + γ_N) → (γ + α + CrN). The analytical results revealed that the surface hardness of AISI 303 stainless steel could be enhanced with the formation of γ_N phase in nitriding process. Antibacterial test also demonstrated the nitrided layer processed the excellent antibacterial properties. The enhanced surface hardness and antibacterial properties make the nitrided AISI 303 austenitic stainless steel to be one of the essential materials in the biomedical applications.     

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.     

Microscopic observation of lateral diffusion at Si-SiO2 interface by photoelectron emission microscopy using synchrotron radiation

The lateral surface diffusion at Si-SiO₂ interface has been observed at nanometer scale using photoelectron emission microscopy (PEEM) combined with synchrotron soft X-ray excitation. The samples investigated were Si-SiO_x micro-patterns prepared by O₂⁺ ion implantation in Si (0 0 1) wafer using a mask. The lateral spacial resolution of the PEEM system was about 41 nm. The brightness of each spot in the PEEM images changed depending on the photon energy around the Si K-edge, in proportion to the X-ray absorption intensity of the corresponding valence states. It was found that the lateral diffusion occurs by 400-450 °C lower temperature than that reported for the longitudinal diffusion at the Si-SiO₂ interface. It was also found that no intermediate valence states such as SiO (Si²⁺) exist at the Si-SiO₂ interface during the diffusion. The observed differences between lateral and longitudinal diffusion are interpreted by the sublimated property of silicon monoxide (SiO).     

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.     

Surface texturing of the carbon steel AISI 1045 using femtosecond laser in single pulse and scanning regime

Surface texturing of the metals, including steels, gained a new dimension with the appearance of femtosecond lasers. These laser systems enable highly precise modifications, which are very important for numerous applications of metals. The effects of a Ti:sapphire femtosecond laser with the pulse duration of 160 fs, operating at 775 nm wavelength and in two operational regimes - single pulse (SP) and scanning regime, on a high quality AISI 1045 carbon steel were studied. The estimated surface damage threshold was 0.22 J/cm² (SP). Surface modification was studied for the laser fluences of 0.66, 1.48 and 2.37 J/cm². The fluence of 0.66 J/cm², in both working regimes, induced texturing of the material, i.e. formation of periodic surface structures (PSS). Their periodicity was in accordance with the used laser wavelength. Finally, changes in the surface oxygen content caused by ultrashort laser pulses were recorded.     

Study of vacancy on diamond (1 0 0) (2 × 1) surface from first-principles

Structure and energy related properties of neutral and charged vacancies on relaxed diamond (1 0 0) (2 × 1) surface were investigated by means of density functional theory. Calculations indicate that the diffusion of a single vacancy from the top surface layer to the second layer is not energetically favored. Analysis of energies in charged system shows that neutral state is most stable on diamond (1 0 0) (2 × 1) surface. The multiplicity of possible states can exist on diamond (1 0 0) surface in dependence on the surface Fermi level, which supports that surface diffusion of a vacancy is mediated by the change of vacancy charge states. Analysis of density of states shows surface vacancy can be effectively measured by photoelectricity technology.     

Influence of treating frequency on microstructure and properties of Al2O3 coating on 304 stainless steel by cathodic plasma electrolytic deposition

Alumina ceramic coatings were fabricated on 304 stainless steel by cathodic plasma electrolytic deposition (CPED). Influence of treating frequency of the power supply on the microstructure and properties of the coatings were studied. The results indicated that coatings obtained at various frequencies on 304 stainless steels were all composed of α-Al₂O₃ and γ-Al₂O₃, and α-Al₂O₃ was the dominant phase. The contents of α-Al₂O₃ decreased gradually in a very small rate with increasing the frequency and γ-Al₂O₃ gradually increased. The surface of alumina ceramic coating was porous. With increasing the frequency, the coating surface gradually became less rough and more compact, resulting in low surface roughness. The bonding strength of Al₂O₃ coating was higher than 22 MPa and was not strongly affected by treating frequency. With increasing the frequency, the alumina coated steels showed better and gradually increasing corrosion resistance than the uncoated one in 3.5% NaCl solution. The coating steel with desirable corrosion resistance was obtained at 800 Hz whose corrosion current potential and corrosion density were −0.237 V and 7.367 × 10⁻⁸ A/cm², respectively.     

Synthesis and characterization of porous silicon layers for 1D photonic crystal application

In this paper, we studied the optical and physical properties of electrochemically prepared porous silicon layers. The atomic force microscopy analysis showed that the etching depth, pore diameter and surface roughness increase as the etching time increased from 30 to 50 mA/cm². By tuning two current densities J₁ = 50 mA/cm² and J₂ = 30 mA/cm², two samples of 1D porous silicon photonic crystals were fabricated. The layered structure of 1D photonic crystals has been confirmed by scanning electron microscopy measurement which showed white and black strips of two distinct refractive index layers. Finally, the measured reflectance spectra of 1D porous silicon photonic crystals were compared with simulated results.     

Analysis of the current-transport mechanism across a CVD diamond/silicon interface

This work presents a study on the mechanism of injection and charge transport through a CVD diamond/n⁺-Si interface. The current-voltage-temperature characteristics of CVD diamond/silicon heterojunctions measured in the temperature range 119-400 K have been interpreted according to thermionic theory and thermionic field-emission theory. This junction shows deviations from the ideal thermionic theory current model, suggesting the presence of surface states, thin-layer depletion and/or non-homogeneity in the diamond/silicon interface. The T₀ anomaly has been used to explain the behaviour of the ideality factor with temperature. At very low temperatures tunnelling may occur because the E₀₀ values for these junctions are close to the value expected by thermionic field-emission theory. The usual activation-energy plot deviates from linearity at low temperatures. This deviation has been corrected supposing a ln(J_S/T²) versus 10³/nT plot. Under these conditions the Richardson constant is found to be 0.819 A cm⁻² K⁻², which is close to the theoretical value of 1.2 A cm⁻² K⁻². Field-emission device is a promising application for diamond/silicon structure.     

Microstructure and corrosion resistance of the layers formed on the surface of precipitation hardenable plastic mold steel by plasma-nitriding

Plasma-nitriding is used to improve the wear resistance and corrosion resistance of plastic mold steels by modifying the surface layers of these steels. In this study, a precipitation hardenable plastic mold steel (NAK80) was plasma-nitrided at 470, 500, and 530 °C for 4, 8, and 12 h under 25% N₂ + 75% H₂ atmosphere in an industrial nitriding facility. The microstructures of the base material and nitrided layers as well as the core hardness were examined, and various phases present were determined by X-ray diffraction. The corrosion behaviors were evaluated using anodic polarization tests and salt fog spray tests in 3.5% NaCl solution.The results had shown that plasma-nitriding does not cause the core to soften by overaging. Nitriding and aging could be achieved simultaneously in the same treatment cycle. Plasma-nitriding of NAK80 mold steel produced a nitrided layer composed of an outer compound layer constituting a mixture of ?-nitride and γ′-nitride and an adjacent nitrogen diffusion layer on the steel surface. The amount of ?-nitride and total nitrides increased with an increase in nitriding temperature and nitriding time. Corrosion study revealed that plasma-nitriding significantly improved the corrosion resistance in terms of corrosion potential, corrosion and pitting current density, and corrosion rate. This improvement was found to be directly related to the increase in the amount of ?-nitride at the surface, indicating the amount of ?-nitride controlling the corrosion resistance.