Atomic diffusion in laser surface modified AISI H13 steel

This paper presents a laser surface modification process of AISI H13 steel using 0.09 and 0.4 mm of laser spot sizes with an aim to increase surface hardness and investigate elements diffusion in laser modified surface. A Rofin DC-015 diffusion-cooled CO₂ slab laser was used to process AISI H13 steel samples. Samples of 10 mm diameter were sectioned to 100 mm length in order to process a predefined circumferential area. The parameters selected for examination were laser peak power, pulse repetition frequency (PRF), and overlap percentage. The hardness properties were tested at 981 mN force. Metallographic study and energy dispersive X-ray spectroscopy (EDXS) were performed to observe presence of elements and their distribution in the sample surface. Maximum hardness achieved in the modified surface was 1017 HV_0.1. Change of elements composition in the modified layer region was detected in the laser modified samples. Diffusion possibly occurred for C, Cr, Cu, Ni, and S elements. The potential found for increase in surface hardness represents an important method to sustain tooling life. The EDXS findings signify understanding of processing parameters effect on the modified surface composition.     

Microstructure and corrosion behavior of austenitic stainless steel treated with laser

Surface modification of AISI316 stainless steel by laser melting was investigated experimentally using 2 and 4 kW laser power emitted from a continuous wave CO₂ laser at different specimen scanning speeds ranged from 300 to 1500 mm/min. Also, an investigation is reported of the introduction of carbon into the same material by means of laser surface alloying, which involves pre-coating the specimen surfaces with graphite powder followed by laser melting. The aim of these treatments is to enhance corrosion resistance by the rapid solidification associated with laser melting and also to increase surface hardness without affecting the bulk properties by increasing the carbon concentration near the surface. Different metallurgical techniques such as optical microscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD) were used to characterize the microstructure of the treated zone. The microstructures of the laser melted zones exhibited a dendritic morphology with a very fine scale with a slight increase in hardness from 200 to 230 Hv. However, the laser alloyed samples with carbon showed microstructure consisting of γ dendrite surrounded by a network of eutectic structures (γ+carbide). A significant increase in hardness from 200 to 500 Hv is obtained. Corrosion resistance was improved after laser melting, especially in the samples processed at high laser power (4 kW). There was shift in I_corr and E_corr toward more noble values and a lower passive current density than that of the untreated materials. These improvements in corrosion resistance were attributed to the fine and homogeneous dendritic structure, which was found throughout the melted zones. The corrosion resistance of the carburized sample was lower than the laser melted sample.     

Structural and Electronic Properties Study of Colombian Aurifer Soils by Mössbauer Spectroscopy and X-ray Diffraction

In this work a study on gold mineral samples is reported, using optical microscopy, X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The auriferous samples are from the El Diamante mine, located in Guachavez-Nariño (Colombia) and were prepared by means of polished thin sections. The petrography analysis registered the presence, in different percentages that depend on the sample, of pyrite, quartz, arsenopyirite, sphalerite, chalcopyrite and galena. The XRD analysis confirmed these findings through the calculated cell parameters. One typical Rietveld analysis showed the following weight percent of phases: 85.0% quartz, 14.5% pyrite and 0.5% sphalerite. In this sample, MS demonstrated the presence of two types of pyrite whose hyperfine parameters are δ ₁ = 0.280 ± 0.002 mm/s and Δ ₁ = 0.642 ± 0.002 mm/s, δ ₂ = 0.379 ± 0.002 mm/s and Δ ₂ = 0.613 ± 0.002 mm/s.     

Invisible gold in Colombian auriferous soils

Optic microscopy, X-ray diffraction (XRD), Mössbauer spectroscopy (MS), Electron microprobe analysis (EPMA) and secondary ions mass spectroscopy (SIMS) were used to study Colombian auriferous soils. The auriferous samples, collected from El Diamante mine, located in Guachavez-Nariño (Colombia), were prepared by means of polished thin sections and polished sections for EPMA and SIMS. Petrography analysis was made using an optical microscope with a vision camera, registering the presence, in different percentages, of the following phases: pyrite, quartz, arsenopyrite, sphalerite, chalcopyrite and galena. By XRD analysis, the same phases were detected and their respective cell parameters calculated. By MS, the presence of two types of pyrite was detected and the hyperfine parameters are: δ ₁ = 0.280 ± 0.01 mm/s and ΔQ ₁ = 0.642 ± 0.01 mm/s, δ ₂ = 0.379 ± 0.01 mm/s and ΔQ ₂ = 0.613 ± 0.01 mm/s. For two of the samples MS detected also the arsenopyrite and chalcopyrite presence. The mean composition of the detected gold regions, established by EPMA, indicated 73% Au and 27% Ag (electrum type). Multiple regions of approximately 200 × 200 μm of area in each mineral sample were analyzed by SIMS registering the presence of “invisible gold” associated mainly with the pyrite and occasionally with the arsenopyrite.     

The chemical stability and conductivity improvement of protonic conductor BaCe0.8 − x Zr x Y0.2O3 − δ

A series of BaCe_0.8???x Zr _x Y_0.2O_3???δ (BCZYx) (x?=?0, 0.2, 0.4, 0.6, 0.8) powders were prepared by EDTA–citrate complexing sol–gel process in this paper. The electrical conducting behavior, as well as chemical stability, was investigated. X-ray diffraction (XRD) results reveal that all samples are homogenous perovskite phases. Observed from XRD patterns and thermogravimetric curves, the samples with x?≥?0.4 survive in the pure CO₂, while samples with various Zr contents all present structurally stable against steam at 800 °C. The Zr-free sample of BaCe_0.8Y_0.2O_3???δ possesses the maximum bulk conductivity, 4.25?×?10^?2 S/cm, but decomposes into Ba(OH)₂ and Ce_0.8Y_0.2O_3???δ in steam. A negative influence of increasing Zr content on the conductivity of BCZYx can be observed by impedance tests. Considering the effect of temperature on the bulk conductivity, BCZY0.4 is preferred to be applied in SOFC as a protonic conductor, ranging from 1.52?×?10^?4 to 1.51?×?10^?3 S/cm (500–850 °C) with E _a?=?0.859 eV, which is proved to be a good protonic conductor with t _H+?≥?0.9.     

High-energy sub-nanosecond optical pulse generation with a semiconductor laser diode for pulsed TOF laser ranging utilizing the single photon detection approach

Bulk and quantum well laser diodes with a large equivalent spot size of d _a /Γ _a  ≈ 3 µm and stripe width/cavity length of 30 µm/3 mm were realized and tested. They achieved a pulse energy and pulse length of the order of ~1 nJ and ~100 ps, respectively, with a peak pulse current of 6–8 A and a current pulse width of 1 ns. The 2D characteristics of the optical output power versus wavelength and time were also analyzed with a monochromator/streak camera set-up. The far-field characteristics were studied with respect to the time-homogeneity and energy distribution. The feasibility of a laser diode with a large equivalent spot size in single photon detection based laser ranging was demonstrated to a non-cooperative target at a distance of a few tens of meters.     

Improving the empirical model for plasma nitrided AISI 316L corrosion resistance based on M?ssbauer spectroscopy

Traditional plasma nitriding treatments using temperatures ranging from approximately 650 to 730 K can improve wear, corrosion resistance and surface hardness on stainless steels. The nitrided layer consists of some iron nitrides: the cubic ?? ^?? phase (Fe₄N), the hexagonal phase ?? (Fe_2???3N) and a nitrogen supersatured solid phase ?? _N . An empirical model is proposed to explain the corrosion resistance of AISI 316L and ASTM F138 nitrided samples based on Mössbauer Spectroscopy results: the larger the ratio between ?? and ?? ^?? phase fractions of the sample, the better its resistance corrosion is. In this work, this model is examined using some new results of AISI 316L samples, nitrided under the same previous conditions of gas composition and temperature, but at different pressure, for 3, 4 and 5 h. The sample nitrided for 4 h, whose value for ??/?? ^?? is maximum (=?0.73), shows a slightly better response than the other two samples, nitrided for 5 and 3 h (??/?? ^?? = 0.72 and 0.59, respectively). Moreover, these samples show very similar behavior. Therefore, this set of samples was not suitable to test the empirical model. However, the comparison between the present results of potentiodynamic polarization curves and those obtained previously at 4 and 4.5 torr, could indicated that the corrosion resistance of the sample which only presents the ?? _N phase was the worst of them. Moreover, the empirical model seems not to be ready to explain the response to corrosion and it should be improved including the ?? _N phase.     

Irradiation effects on copper

Copper, one of the most significant metals, is exposed to IR radiation. A Nd:YAG laser (1064 nm, 1.1 MW, 12 ns) has been used to irradiate fine polished and annealed samples (4 N, 1×1×0.3 cm³) with 100 laser shots under a vacuum of ～10^?6 torr. The laser focal spot size and power density on the target were 12 μm and 3×10¹² Wm^?2 respectively. The surface and structural studies were performed by analyzing scanning electron micrographs and X-ray diffractograms (XRDs), respectively. Laser ablation results in boiling, splashing, hydrodynamical sputtering and exfoliation along with other relevant phenomena. The XRD patterns of the exposed sample indicate a change in diffraction intensity and grain sizes. The atomic planes remain undisturbed for the irradiated target. The information collected is useful for investigating the complexities found in radiation–metal interactions.     

Synthesis and electric properties of perovskite Pr0.6Ca0.4Fe0.8Co0.2O3 for SOFC applications

In this study, polycrystalline powder Pr_0.6Ca_0.4Fe_0.8Co_0.2O₃ (PCFC) was synthesized by a sol–gel process. This oxide was analyzed by X-ray powder diffraction. Synthesized Pr_0.6Ca_0.4Fe_0.8Co_0.2O₃ showed up to be single phase and belongs to the orthorhombic crystalline system with a Pbnm space group. The microstructural features of the synthesized products display particles having an irregular morphology and a size in the range of 50–100 nm. X-ray diffraction (XRD) analysis shows the chemical compatibility between the PCFC cathode and the electrolyte Sm-doped ceria since no reaction products were honored when the material was mixed and co-fired at 1,000 °C for 168 h. The thermal expansion coefficient of PCFC 16.9?×?10^?6 °C^?1 is slightly higher than that of Ce_0.8Sm_0.2O_1.9 (SDC) over the studied temperature range. The greater contribution to the total resistance of the electrode is the electrochemical resistance associated with oxygen exchange in the cathode surface (0.96 Ωcm²). The dc four-probe measurement indicated that PCFC exhibits fairly high electrical conductivity, over 100 S cm^?1 at T?≥?500 °C, making this material promising as a cathode material for intermediate temperature solid oxide fuel cells.     

The role of target-to-substrate distance on the DC magnetron sputtered zirconia thin films’ bioactivity

Zirconium dioxide thin films were deposited on 316L-stainless steel type substrates using DC unbalanced magnetron sputtering. The process parameter of this work was the target-to-substrate distance (d_t-s), which was varied from 60 to 120 mm. The crystal structure and surface topography of zirconium dioxide thin films were characterized by X-ray diffraction (XRD) and atomic force microscopy (AFM). The results demonstrate that all of the ZrO₂ thin films are composed monoclinic phase. The film sputtered at short d_t-s (60 mm) shows a rather heterogeneous, uneven surface. The grain size, roughness, and thickness of thin films were decreased by increasing d_t-s. The bioactivity was assessed by investigating the formation of hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂) on the thin film surface soaked in simulated body fluids (SBF) for 7 days. XRD and scanning electron microscopy (SEM) were used to verify the formation of apatite layers on the samples. Bone-like apatites were formed on the surface of the ZrO₂ thin film in SBF immersion experiments. A nanocrystalline hydroxyapatite (HA) with a particle size of 2-4 μm was deposited. Higher crystallinity of HA on the surface was observed when the distance d_t-s increased to more than 80 mm. Therefore, it seems that a d_t-s greater than 80 mm is an important sputtering condition for inducing HA on the zirconia film.     

Excimer laser processing as a tool for photocatalytic design of sol-gel TiO2 thin films

Nanostructured sol-gel TiO₂ thin films spin coated on silicate glass plates are subjected to excimer (KrF^*) pulsed laser irradiation in order to tailor their structure and photocatalytic properties. The surface morphology of virgin and laser-processed films are followed applying electron optical imaging and atomic force microscopy. The evolution of the surface roughness and pore formation are shown to be accompanied by optical absorption edge shift to infrared wavelength range. Conventional X-ray diffraction analysis and high-resolution transmission electron imaging are applied in order to obtain information on the phase composition. Co-existence of amorphous and anatase TiO₂ phases in nonirradiated sol-gel films is found. It is established that after laser processing the most intense XRD anatase peak is shifted to lower 2θ range. The analysis of high-resolution transmission electron images of film profiles evidences for the laser induced phase transitions. Formation of rutile and brookite TiO₂ accompanied by evolution of oxygen deficient Ti_nO_2n−1 phases are identified in the subsurface region. The contribution of laser processing for increasing the photocatalytic efficiency of laser-modified films toward the oxidation of methylene blue water solution is demonstrated. The results obtained reveal a novel-processing route for designing sol-gel titania films with improved photocatalytical activity.     

Effect of sintering conditions on the magnetic and structural properties of Fe 0.6 Mn 0.1 Al 0.3 synthesized by mechanical alloying

In order to study the effect of sintering condition on the structural and magnetic behavior of prealloyed metallic powders of Fe _0.6 Mn _0.1 Al _0.3 system, two different thermal treatments were employed. All samples were previously milled and then compacted. Later, the sintering process was carried out in two cycles. For the first one, a sintering time of 2 h was followed by a cooling process governed by the inertia of the furnace. In the second treatment, a sintering time of 0.17 h with a controlled slow ramp of 1 °C/min between 500 °C and 250 °C. All samples were characterized by X-ray diffraction and Mössbauer spectroscopy. It was found that the sintering time improves the crystallinity while the magnetic behavior was modified by the changes in the cooling rate.     

Laser radiation effects on optical and structural properties of nanostructure CdSe thin film

Cadmium selenide (CdSe) thin films were deposited on a glass substrate using the thermal evaporation method at room temperature. The changes in the optical properties (optical band gap and absorption coefficient) after irradiation by TEA N₂ laser at different energies were measured in the wavelength range 190–800 nm using a spectrophotometer. It was found that the optical band gap is decreased after irradiating the thin films. The samples were characterized using X-ray diffraction (XRD), and the grain size of the CdSe thin film was calculated from XRD data, which was found to be 41.47 nm as-deposited. It was also found that grain size increases with laser exposure. The samples were characterized using a scanning electron microscope and it was found that big clusters were formed after irradiation by TEA N₂ laser.     

Synthesis,structural characterization and ionic conductivity of NASICON-type Ba<Subscript>x/2</Subscript>Li<Subscript>1-x</Subscript>Ti<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> (0.4 ≤ x ≤ 1) materials

The NASICON series, with formula Ba_x/2Li_1-xTi₂(PO₄)₃ (0.4 ≤ x ≤ 1), has been prepared by solid-state reaction and characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR), Raman, nuclear magnetic resonance (NMR) and impedance spectroscopy (IS). XRD patterns of samples indicated the formation of single phases with rhombohedral structure (space group R-3c). The Rietveld analysis of XRD patterns was performed to deduce location of Li and Ba ions. FTIR, Raman, and NMR techniques showed the only presence of isolated PO₄ groups in analyzed phosphates. ³¹P MAS-NMR spectra were used to investigate Li and Ba distribution and ⁷Li MAS-NMR spectra to discriminated Li ions with different mobility in conduction paths. A maximum total conductivity of 2.5 × 10^?7 S cm^?1 and a minimum activation energy of 0.47 eV were obtained at room temperature for Ba_0.3Li_0.4Ti₂(PO₄)₃ (x = 0.6).     

Preparation and characterization of a new PEO-PPG blend polymer electrolyte system

This paper reports on preparation and characterization of thin films of a new zinc ion conducting blended polymer electrolyte system containing polyethylene oxide [PEO] and polypropylene glycol [PPG] complexed with zinc triflate [Zn(CF₃SO₃)₂] salt. The room temperature ionic conductivity (σ _298K) data of such PEO-PPG polymer blends prepared by solution casting technique were found to be of the order of 10^?5 S cm^?1, whereas the optimized composition containing 90:10 wt% ratio of PEO and PPG possessed an appreciably high ionic conductivity of 7.5?×?10^?5 S cm^?1. Subsequently, six different weight percentages of zinc triflate viz., 2.5, 5, 7.5, 10, 12.5 and 15, respectively, were added into the above polymer blend and resulting polymer-salt complexes were characterized by means of various analytical tools. Interestingly, the best conducting specimen namely 87.5 wt% (PEO:PPG)-12.5 wt% Zn(CF₃SO₃)₂ exhibited an enhanced room temperature ionic conductivity of 6.9?×?10^?4 S cm^?1 with an activation energy of 0.6 eV for ionic conduction. The present XRD results have indicated the occurrence of characteristic PEO peaks and effects of salt concentration on the observed intensity of these diffraction peaks. Appropriate values of degree of crystallinity for different samples were derived from both XRD and DSC analyses, while an examination of surface morphology of the blended polymer electrolyte system has revealed the formation of homogenous spherulites involving a rough surface and relevant zinc ionic transport number was found to be 0.59 at room temperature for the best conducting polymer electrolyte system thus developed.     

Energy efficiency of drilling granite and travertine with a CO2 laser and 980 nm diode laser

Using lasers to drill hard rock presents potential advantages compared to conventional mechanical drilling, such as higher penetration rates and reduced vibration. Before realistic drilling tools can be proposed, the influence of important parameters and the mechanisms involved in drilling different rocks with different lasers must be understood. In this work, we investigate the efficiency of laser drilling of granite and travertine with a CO₂ laser and a 980 nm fiber coupled diode laser. At the drilling surface, the maximum CW power delivered by the CO₂ laser was 140 W, while the diode laser delivered up to 215 W. Even at these modest power levels, it was possible to drill holes with diameters of the order of 8 mm at efficiencies varying from 40 kJ/cm³ to 150 kJ/cm³. The optimum laser exposure period of time was also investigated. Finally, x-ray diffraction and fluorescence analysis, as well as Tg (Thermogravimetry) and DTA (Differential Thermal Analysis) measurements, were performed on the rocks samples used.     

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.     

The effect of oxide layer in case of novel coolant spray at very high initial surface temperature

The significant reduction of Leidenfrost effect during the cooling of high carbon steel plate by different potential cooling methodologies does not assure their successful implementation in the fast quenching of high carbon steel plate due to the formation of oxide layer of comparatively low thermal conductivity on the quenching surface. Therefore, the role of oxide layer in case of different potential cooling methodologies needs to be addressed. In the present study, the effect of oxide layer on heat transfer rate in case of upward, downward, and both upward and downward facing spray with additives has been investigated by conducting and comparing the heat transfer cooling data of an AISI 1020 plate with the AISI 304 plate. The comparison clearly depicts that the formation of oxide layer during cooling significantly hinders the heat transfer rate in nucleate boiling regime; however, the reverse phenomenon is observed in transition boiling regime. Among all the coolants, the least effect of oxide layer on enhancement is obtained in case of NaCl (0.4 M)-added water spray due to the deposition of salt on the evaporating surface. The X-ray diffraction analysis and the thickness of the formed oxide layer clearly assert that the coolant depicting minimum oxidation characteristic is preferred.

Abbreviations: AISI: American iron and steel institute; OES: Optical emission spectrophotometer; CHF: Critical heat flux, MW/m²; IHF: Initial heat flux, MW/m²; T_CHF: Temperature at which CHF is achieved, °C; Fps: Frames per second; XRD: X-Ray diffraction; k₁: Thermal conductivity of steel plate, W/m °C; k₂: Thermal conductivity of oxide layer, W/m °C; k₃: Thermal conductivity of coolant, W/m °C; X: x-axis, mm; Y: y-axis, mm; Z: z-axis, mm     

Structure and properties of (TiVCrZrY)N coatings prepared by energetic bombardment sputtering with different nitrogen flow ratios

(TiVCrZrY)N coatings were deposited onto Si substrate by the radio-frequency (RF) magnetron sputtering of a TiVCrZrY alloy target in an N₂/Ar atmosphere. The crystal, microstructural, mechanical, and electrical properties at different N₂-to-total (N₂+Ar) flow-rate ratio (R _N) values were investigated. The coating produced in pure Ar had an equiaxed structure with a hexagonal-close-packed phase. With increased R _N, the crystallinity and grain size markedly decreased. The microstructure of (TiVCrZrY)N coatings transformed from V-shaped columnar with a rough-domed surface into fine fibrous with a smooth surface. The amorphous transition layer above the substrate was also significantly thickened. The hardness of (TiVCrZrY)N decreased from 20.9 GPa to 18.9 GPa, and the electrical resistivity increased from 398.2 μΩ?cm to 21870 μΩ?cm.     

Effect of lanthanum ions on magnetic properties of Y3Fe5O12 nanoparticles

Lanthanum ion (La³⁺)-substituted garnet nanoparticles Y_3?x La _x Fe₅O₁₂ (x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0) were fabricated by a sol–gel method. Their crystalline structures and magnetic properties were investigated by using X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and Mössbauer spectrum. The XRD results show that samples of Y_3?x La _x Fe₅O₁₂ (0.0 ≤ x ≤ 0.8) are all single phase and the sizes of particles range from 32 to 65 nm. Those of Y₂LaFe₅O₁₂ consisted of peaks from garnet and LaFeO₃ structures. Compared to pure YIG, the saturation magnetization is larger when the La concentration x = 0.2. However, with increasing La concentration (x), it decreases obviously. Meanwhile, may be due to the enhancement of the surface spin effects, the saturation magnetization rises as the particle size is increased. Different from the pure YIG, the Mössbauer spectra of Y_2.8La_0.2Fe₅O₁₂ and Y_2.2La_0.8Fe₅O₁₂ are composed of four sets of six-line hyperfine patterns. The results tell us that the substitution of La³⁺ ions with large ionic radius (1.061 Å) will give rise to a microscopic structure distortion of the a- and d-sites to different degrees, and the Zeeman sextets from a- and d-sites begin to split into two sub-sextets, which is helpful to explain the phenomenon observed in the study of the magnetic property.