Comparison of the Microstructural, Mechanical and Corrosion Resistance Properties of Ti6Al4V Samples Manufactured by LENS and Subjected to Various Heat Treatments.

In this paper, the influences of two post-heat treatments on the structural, mechanical and corrosion resistance properties of additively manufactured Ti6Al4V alloys were discussed in detail. The materials were produced using the laser engineering net shaping (LENS) technique, and they were subjected to annealing without pressure and hot isostatic pressing (HIP) under a pressure of 300 MPa for 30 min at temperatures of 950 °C and 1050 °C. Annealing without pressure led to the formation of a thin plate structure, which was accompanied by decreasing mechanical properties and increasing elongation and corrosion resistance values. For the HIP process, the formation of a thick plate structure could be observed, resulting in the material exhibiting optimal mechanical properties and unusually high elongation. The best mechanical and corrosion resistance properties were obtained for the material subjected to HIP at 950 °C.

Morphological and semiconductive properties of the anodic oxide layers made on Fe3Al alloy by anodizing in tartaric-sulfuric acid mixture.

It has recently been found that the anodizing of FeAl alloys allows the formation of iron-aluminum oxide layers with interesting semiconducting properties. However, the lack of systematic research on different anodizing regimes is hampering their full exploitation in numerous photoelectrochemical-related applications. This study address, for the first time, the systematic effect of the electrolyte composition on the formation of self-ordered oxide films by anodizing on cast Fe3Al alloy. The Fe3Al alloy was anodized in 3 electrolytes with different water-ethylene glycol (EG) ratios (pure water, 25 vol.%-EG, and 50 vol.%-EG solutions) at a constant tartaric-sulfuric acids concentration, different voltages (10-20 V) and treatment times (2-60 min). After anodizing, all anodic oxide layers were annealed at 900 °C to form semiconductive iron-aluminum crystalline phases. Conventional techniques were used to systematically ascertain the morphological (SEM/EDS, XRD, eddy-current measurements) and semiconductive (UV-VIS reflectance spectroscopy) properties of these oxide layers. The results confirmed the formation of homogeneous and self-ordered anodic oxide layers at 10 and 15 V, regardless of the electrolyte composition. Namely, anodic films formed in electrolytes containing EG showed lower pore sizes, growth rates, and film thicknesses than those anodic films formed in the aqueous-based electrolyte. The annealing post-treatment results in different Fe-Al oxides (FexOy, FeAl2O4, etc.) with superior band gap values than those for non-annealed films.

High Critical Current Density in the Textured Nanofiber Structure in Multifilament MgB2 Wires Made by the Powder-In-Tube (PIT) Technique.

We show that the structure of multifilament MgB2 wires made by the powder-in-tube (PIT) method can be texturized by annealing the structure under high isostatic pressure. Our results show that we obtained continuous fibers with a uniform diameter of 250 nm in all 36 filaments, a small grain size of approximately 50 nm and a high density of the superconducting material. These results contribute to a significant improvement in the critical current density in high magnetic fields, e.g., 100 A/mm2 at 14 T and 4.2 K.

Characterization of Cobalt-Based Stellite 6 Alloy Coating Fabricated by Laser-Engineered Net Shaping (LENS).

The results of microstructure and mechanical properties evaluation of a Stellite 6 (Co-6) alloy deposited on X22CrMoV12-1 substrate by the laser-engineered net shaping (LENSTM) technology are presented in this paper. The Stellite 6 alloy is widely used in industry due to its excellent wear resistance at elevated temperatures and corrosive environments. Specific properties of this alloy are useful in many applications, e.g., as protective coatings in steam turbine components. In this area, the main problems are related to the fabrication of coatings on complex-shaped parts, the low metallurgical quality of obtained coatings, and its insufficient adhesion to a substrate. The results of recently performed investigations proved that the LENS technology is one of the most effective manufacturing techniques of the Co-6 alloy coatings (especially deposited on complex-shaped turbine parts). The microstructural and phase analyses of obtained Stellite 6 coatings were carried out by light microscopy techniques and X-ray diffraction analysis. A chemical homogeneity of Co-6 based layers and a fluctuation of chemical composition in coating-substrate zone after the laser deposition were analyzed using an energy dispersive X-ray spectrometer coupled with scanning electron microscopy. The room temperature strength and ductility of the LENS processed layers were determined in static bending tests.

Properties of Polyethylene Terephthalate (PET) after Thermo-Oxidative Aging.

The influence of the thermo-oxidative aging semi-crystalline polyethylene terephthalate process on the thermal and mechanical properties was analysed in the article. For this purpose, PET was aged at 140 °C for 21, 35 and 56 days. The research showed that as a result of aging, the amount of the crystalline phase increases by about 8%, which translates into the properties of the aged material. The glass transition and melt temperature of lamellar crystals formed during first and second crystallisation increase with aging. The mechanical properties of the material were analysed in the temperature range of 25 to 75 °C. The tests were showing an increase in Young's modulus and a decrease in elongation at the break as a result of aging. This phenomenon was particularly visible during tests at 75 °C and during the morphological observation of the fracture surface, where the fracture character of the material changes from ductile to brittle. In the case of the material aged for the longest time, the temperature has a negligible influence on the elongation at break.

Suitability of Laser Engineered Net Shaping Technology for Inconel 625 Based Parts Repair Process.

In this paper, the Inconel 625 laser clads characterized by microstructural homogeneity due to the application of the Laser Engineered Net Shaping (LENS, Optomec, Albuquerque, NM, USA) technology were studied in detail. The optimized LENS process parameters (laser power of 550 W, powder flow rate of 19.9 g/min, and heating of the substrate to 300 °C) enabled to deposit defect-free laser cladding. Additionally, the laser clad was applied in at least three layers on the repairing place. The deposited laser clads were characterized by slightly higher mechanical properties in comparison to the Inconel 625 substrate material. Microscopic observations and X-ray Tomography (XRT, Nikon Corporation, Tokyo, Japan) confirmed, that the substrate and cladding interface zone exhibited a defect-free structure. Mechanical properties and flexural strength of the laser cladding were examined using microhardness and three-point bending tests. It was concluded, that the LENS technology could be successfully applied for the repair since a similar strain distribution was found after Digital Image Correlation measurements during three-point bending tests.

Microstructure Evolution of 316L Steel Prepared with the Use of Additive and Conventional Methods and Subjected to Dynamic Loads: A Comparative Study.

The mechanical properties and microstructure evolution caused by dynamic loads of 316L stainless steel, fabricated using the Laser Engineered Net Shaping (LENS) technique and hot forging method were studied. Full-density samples, without cracks made of 316L stainless steel alloy powder by using the LENS technique, are characterized by an untypical bi-modal microstructure consisting of macro-grains, which form sub-grains with a similar crystallographic orientation. Wrought stainless steel 316L has an initial equiaxed and one-phase structure, which is formed by austenite grains. The electron backscattered diffraction (EBSD) technique was used to illustrate changes in the microstructure of SS316L after it was subjected to dynamic loads, and it was revealed that for both samples, the grain refinement increases as the deformation rate increases. However, in the case of SS316L samples made by LENS, the share of low-angle boundaries (sub-grains) decreases, and the share of high-angle boundaries (grains of austenite) increases. Dynamically deformed wrought SS316L is characterized by the reverse trend: a decrease in the share of high-angle boundaries and an increase in the share of low-angle boundaries. Moreover, additively manufactured SS316L is characterized by lower plastic flow stresses compared with hot-forged steel, which is caused by the finer microstructure of wrought samples relative to that of additive samples. In the case of additively manufactured 316L steel samples subjected to a dynamic load, plastic deformation occurs predominantly through dislocation slip, in contrast to the wrought samples, in which the dominant mechanism of deformation is twinning, which is favored by a high deformation speed and low stacking fault energy (SFE) for austenite.

Self-Organized Anodic Oxides on Titanium Alloys Prepared from Glycol- and Glycerol-Based Electrolytes.

The anodization of commercially pure Ti alloy (99.5 wt %) and two biomedical titanium alloys, Ti6Al7Nb and Ti6Al4V, was performed, and the resulting anodic oxides were studied. The biomedical alloys were made by Laser Engineered Net Shaping. The glycol-based and glycerol-based electrolytes with 0.3 M ammonium fluoride and 2 wt % of deionized water content were tested. It was found that electrolyte type as well as the chemical composition of the base substrate affected the final morphology and chemical composition of the anodic oxide formed. A higher current density, ionic mobility, and oxide growth rate were obtained in glycol-based electrolyte as compared to those obtained in glycerol-based electrolyte for all tested alloys. A self-organized nanotubular and nanoporous morphology of the anodic oxide in both types of electrolyte was obtained. In each electrolyte, the alloy susceptibility to oxidation increased in the following order: Ti6Al4V < Ti 99.5% < Ti6Al7Nb, which can be correlated to the oxidation susceptibility of the base titanium alloy. It was observed that the more impurities/alloying elements in the substrate, the lower the pore diameters of anodic oxide. There was a higher observed incorporation of electrolyte species into the anodic oxide matrix in the glycerol-based electrolyte compared with that in glycol-based electrolyte.

Microstructure and Properties of Inconel 625 Fabricated Using Two Types of Laser Metal Deposition Methods.

The effect of using two different deposition systems on the microstructure and mechanical properties was studied in this paper. For this purpose, laser-engineered net shaping (LENS) and high-power CO2 laser deposition processes were applied to fabricate Inconel 625 samples. The microstructure of the Inconel 625 produced by both additive techniques was characterized using light microscopy (LM), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The mechanical properties were characterized by tensile tests and microhardness measurements. High-power laser application resulted in a strong <100> build texture, while, at low powers, the {011} <100> Goss component increased. Both types of deposited materials showed dendritic microstructures with Ti-, Mo-, and Nb-rich zones at the cell boundaries, where numerous precipitates (Nb2C, NbC, titanium carbides, Nb3Ni, and NbNiCr) were also observed. It was also noted that both variants were characterized by the same slope with a proportional length, but the Inconel 625 fabricated via LENS showed a higher average yield strength (YS; 524 MPa vs. 472 MPa) and ultimate tensile strength (UTS; 944 MPa vs. 868 MPa) and lower elongation (35% vs. 42%) than samples obtained with the high-power CO2 laser deposition process.

Superelastic Behavior of Ti-Nb Alloys Obtained by the Laser Engineered Net Shaping (LENS) Technique.

The effect of Nb content on microstructure, mechanical properties and superelasticity was investigated for a series of Ti-xNb alloys, fabricated by the laser engineered net shaping method, using elemental Ti and Nb powders. The microstructure of as-deposited materials consisted of columnar ß-phase grains, elongated in the built direction. However, due to the presence of undissolved Nb particles during the deposition process, an additional heat treatment was necessary. The observed changes in mechanical properties were explained in relation to the phase constituents and deformation mechanisms. Due to the elevated oxygen content in the investigated materials (2 at.%), the specific deformation mechanisms were observed at lower Nb content in comparison to the conventionally fabricated materials. This made it possible to conclude that oxygen increases the stability of the ß phase in ß-Ti alloys. For the first time, superelasticity was observed in Ti-Nb-based alloys fabricated by the additive manufacturing method. The highest recoverable strain of 3% was observed in Ti-19Nb alloy as a result of high elasticity and reverse martensitic transformation stress-induced during the loading.

The Tribaloy T-800 Coatings Deposited by Laser Engineered Net Shaping (LENSTM).

A Tribaloy family of alloys (CoMoCrSi) are characterized by a substantial resistance to wear and corrosion within a wide range of temperatures. These properties are a direct result of their microstructure including the presence of Laves phase in varying proportions. Tribaloy T-800 exhibits the highest content of Laves phase of all other commercial Tribaloy alloys, which provides high hardness and wear resistance. On the other hand, a large content of the Laves phase brings about a high sensitivity to brittle fracture of this alloy. The main objective of this work was a development of the Tribaloy T-800 coatings on the Ni-based superalloy substrate (RENE 77), which employs a Laser Engineered Net Shaping (LENSTM) technique. Technological limitations in this process are susceptibility of T-800 to brittle fracture as well as significant thermal stresses due to rapid cooling, which is an inherent attribute of laser techniques. Therefore, in this work, a number of steps that optimized the LENSTM process and improved the metallurgical soundness of coatings are presented. Employing volume and local substrate pre-heating resulted in the formation of high quality coatings devoid of cracks and flaws.

Structural and Optical Characterization of ZnS Ultrathin Films Prepared by Low-Temperature ALD from Diethylzinc and 1.5-Pentanedithiol after Various Annealing Treatments.

The structural and optical evolution of the ZnS thin films prepared by atomic layer deposition (ALD) from the diethylzinc (DEZ) and 1,5-pentanedithiol (PDT) as zinc and sulfur precursors was studied. A deposited ZnS layer (of about 60 nm) is amorphous, with a significant S excess. After annealing, the stoichiometry improved for annealing temperatures ≥400 °C and annealing time ≥2 h, and 1:1 stoichiometry was obtained when annealed at 500 °C for 4 h. ZnS crystallized into small crystallites (1-7 nm) with cubic sphalerite structure, which remained stable under the applied annealing conditions. The size of the crystallites (D) tended to decrease with annealing temperature, in agreement with the EDS data (decreased content of both S and Zn with annealing temperature); the D for samples annealed at 600 °C (for the time ≤2 h) was always the smallest. Both reflectivity and ellipsometric spectra showed characteristics typical for quantum confinement (distinct dips/peaks in UV spectral region). It can thus be concluded that the amorphous ZnS layer obtained at a relatively low temperature (150 °C) from organic S precursor transformed into the layers built of small ZnS nanocrystals of cubic structure after annealing at a temperature range of 300-600 °C under Ar atmosphere.

Influence of Manufacturing Technology on the Structure of 80W-20Re Heavy Sinters.

Preliminary measurement results of 80W-20Re heavy sinters are presented in this paper. Tested samples were taken from three different technology processes, i.e., resistance sintering (RS), pulse plasma sintering (PPS), and conventional sintering in a vacuum furnace. In the first two cases, the obtained sinters were of similar usable properties (porosity and microhardness), while for vacuum sintering, the material with high porosity was obtained. At the same time, it was found that sintering with the use of electric current (RS, PPS) generates microstructures with highly elongated grains.

Static and Dynamic Loading Behavior of Ti6Al4V Honeycomb Structures Manufactured by Laser Engineered Net Shaping (LENSTM) Technology.

Laser Engineered Net Shaping (LENSTM) is currently a promising and developing technique. It allows for shortening the time between the design stage and the manufacturing process. LENS is an alternative to classic metal manufacturing methods, such as casting and plastic working. Moreover, it enables the production of finished spatial structures using different types of metallic powders as starting materials. Using this technology, thin-walled honeycomb structures with four different cell sizes were obtained. The technological parameters of the manufacturing process were selected experimentally, and the initial powder was a spherical Ti6Al4V powder with a particle size of 45-105 µm. The dimensions of the specimens were approximately 40 × 40 × 10 mm, and the wall thickness was approximately 0.7 mm. The geometrical quality and the surface roughness of the manufactured structures were investigated. Due to the high cooling rates occurring during the LENS process, the microstructure for this alloy consists only of the martensitic α' phase. In order to increase the mechanical parameters, it was necessary to apply post processing heat treatment leading to the creation of a two-phase α + ß structure. The main aim of this investigation was to study the energy absorption of additively manufactured regular cellular structures with a honeycomb topology under static and dynamic loading conditions.

The Microstructure Evolution of a Fe3Al Alloy during the LENS Process.

A Fe3Al intermetallic alloy has been successfully prepared by the laser-engineered net shaping (LENS) process. The applied process parameters were selected to provide various cooling rates during the solidification of the laser-melted material. The macro- and microstructure and the micro- and macrotexture of Fe3Al samples were investigated. The influence of the cooling rate on grain morphology and texture is discussed. For the applied cooling rate range of 0.64 × 104 K/s-2.6 × 104 K/s, the structure is characterized by the presence of columnar grains for which the growth is directed upwards from the substrate. The intensity of the microtexture varies with the height of the sample and the cooling rate. The intensity of the texture increases with the decrease in the cooling rate. The samples that were obtained with low and medium cooling rates are characterized by the well-developed <100> and <111> macrotextures. The Fe3Al alloy that was produced with a high cooling rate did not show a specific texture, which is reflected in the fairly uniform distribution of the normalized density intensity. Only a very weak texture with a <100> type component was observed.

The Effect of the Traverse Feed Rate on the Microstructure and Mechanical Properties of Laser Deposited Fe3Al (Zr,B) Intermetallic Alloy.

The results of the fabrication of components made with Fe-30%Al-0.35%Zr-0.1%B alloy powder using the Laser Engineered Net Shaping (LENSTM) system operated at different traverse feed rates are described in this paper. The temperature of the molten metal pool was recorded during this process. Depending on the assumed feed rate, the formation of Zr⁻based precipitates with various morphologies and distributions was observed in the structure of the investigated material. It was found that as the traverse speed increased, spheroidization, refinement, and a more homogeneous distribution of these precipitates occurred.

The Application of Globular Water-Atomized Iron Powders for Additive Manufacturing by a LENS Technique.

The water-atomized ATOMET 28, 1001, 4701, and 4801 powders, manufactured by Rio Tinto Metal Powders, were used for additive manufacturing by a laser engineered net shaping (LENS) technique. Their overall morphology was globular and rounded with a size distribution from about 20 to 200 µm. Only the ATOMET 28 powder was characterized by a strong inhomogeneity of particle size and irregular polyhedral shape of powder particles with sharp edges. The powders were pre-sieved to a size distribution from 40 to 150 µm before LENS processing. One particular sample-LENS-fabricated from the ATOMET 28 powder-was characterized by the largest cross-sectional (2D) porosity of 4.2% and bulk porosity of 3.9%, the latter determined by microtomography measurements. In contrast, the cross-sectional porosities of bulk, solid, nearly cubic LENS-fabricated samples from the other ATOMET powders exhibited very low porosities within the range 0.03⁻0.1%. Unexpectedly, the solid sample-LENS-fabricated from the reference, a purely spherical Fe 99.8 powder-exhibited a porosity of 1.1%, the second largest after that of the pre-sieved, nonspherical ATOMET 28 powder. Vibrations incorporated mechanically into the LENS powder feeding system substantially improved the flow rate vs. feeding rate dependence, making it completely linear with an excellent coefficient of fit, R² = 0.99. In comparison, the reference powder Fe 99.8 always exhibited a linear dependence of the powder flow rate vs. feeding rate, regardless of vibrations.

The Structure of FeAl Sinters Fabricated Using Cyclic Loading.

A two stage process including a sintering under a cyclic loading is proposed as an alternative fabrication method of dense FeAl intermetallics from elemental powder mixtures. The first stage (pre-sintering) is conducted at two temperature values (620 °C and 670 °C, respectively) under a static and a cyclic loading with a frequency of 20, 40 and 60 Hz. The second one includes a pressureless sintering at temperature of 1250 °C, under a protective argon atmosphere. A suitable selection of pre-sintering parameters (temperature, type and frequency of pressing) allows approximately five times grain size reduction of FeAl phase in comparison to particle size of raw Fe and Al powder material (40-60 µm), as well as induces an effective fragmentation of oxide layers. For the sinters obtained using 60 Hz loading frequency an oxide particle size of 4.0 or 4.5 µm (smaller for sintering with liquid phase) is observed. Material obtained after the full heat treatment are characterized by a fine-grained structure of chemically homogeneous FeAl phase with uniformly distributed Al2O3 spherical particles along grain boundaries. Moreover, it was found that temperature and frequency of loading during the presintering process also affect a consolidation level of the Fe-Al powder mixture, which increases with rising both temperature and frequency.