Microstructure and Mechanical Properties of NiTi-Based Eutectic Shape Memory Alloy Produced via Selective Laser Melting In-Situ Alloying by Nb

This paper presents the results of selective laser melting (SLM) process of a nitinol-based NiTiNb shape memory alloy. The eutectic alloy Ni₄₅Ti₄₅Nb₁₀ with a shape memory effect was obtained by SLM in-situ alloying using a powder mixture of NiTi and Nb powder particles. Samples with a high relative density (>99%) were obtained using optimized process parameters. Microstructure, phase composition, tensile properties, as well as martensitic phase transformations temperatures of the produced alloy were investigated in as-fabricated and heat-treated conditions. The NiTiNb alloy fabricated using the SLM in-situ alloying featured the microstructure consisting of the NiTi matrix, fine NiTi+β-Nb eutectics, as well as residual unmelted Nb particles. The mechanical tests showed that the obtained alloy has a yield strength up to 436 MPa and the tensile strength up to 706 MPa. At the same time, in-situ alloying with Nb allowed increasing the hysteresis of martensitic transformation as compared to the alloy without Nb addition from 22 to 50 °C with an increase in A_f temperature from −5 to 22 °C.     

Microstructure and Properties of As-Cast and Heat-Treated 2017A Aluminium Alloy Obtained from Scrap Recycling

The continuous increase in the consumption of aluminium and its alloys has led to an increase in the amount of aluminium scrap. Due to environmental protection, and to reduce the costs of manufacturing aluminum in recent years, a lot of research is devoted to recycling of aluminum alloys. The paper presents the results of research concerning the possibility of manufacturing standardized alloy 2017A from commercial and post-production scrap by continuous casting. Obtained from recycling process ingots were subjected to analysis of chemical composition and intermetallic phase composition. Based on the results of light microscopy (LM), scanning electron microscopy + electron dispersive spectroscopy (SEM + EDS), and X-ray diffraction (XRD) the following phases in the as-cast state were identified: θ-Al₂Cu, β-Mg₂Si, Al₇Cu₂Fe, Q-Al₄Cu₂Mg₈Si₇, and α-Al₁₅(FeMn)₃(SiCu)₂. During solution heat treatment most of the primary precipitates of intermetallic phases, like θ-Al₂Cu, β-Mg₂Si, and Q-Al₄Cu₂Mg₈Si₇, were dissolved in the solid solution α-Al, and during natural and artificial aging they precipitate as strengthening phases θ-Al₂Cu and Q-Al₄Cu₂Mg₈Si₇ with high dispersion. The highest hardness—150.3 HB—of 2017A alloy was obtained after solution heat treatment from 510 °C and aging at 175 °C. In the static tensile test the mechanical (R_m and R_p0.₂) and plastic (A₅) properties were determined for 2017A alloy in the cast state and after T4 heat treatment. The highest strength properties—tensile strength R_m = 450.5 MPa and yield strength R₀.₂ = 268.7 MPa with good relative elongation A₅ = 14.65%, were obtained after solution heat treatment at 510 °C/6 h/water quenching and natural aging at 25 °C for 70 h. The alloy manufactured from recycled scrap is characterized by relatively high mechanical properties.     

Formation of Phases and Microstructures in Al-8Si Alloys with Different Mg Content

Mg-containing high-silicon aluminum alloy is a heat-treatable aluminum alloy that is now widely used in the aerospace and automotive industries because of its high specific strength, high wear resistance and corrosion resistance, low thermal expansion coefficient, and low cost. More attention has been paid to optimizing the microstructure to increase the performance of this type of aluminum alloy. In the present work, the solidification processes of Mg-free and Mg-containing (0.33–1.32%) Al-8Si alloys were analyzed by the experimental results combined with the thermodynamic calculation. The results showed that α-Al, Si, and Al₅FeSi were in the Mg-free Al-8Si alloy ingots, while the Al₅FeSi phases in alloys with Mg additions were transformed into π phases (Al₈Mg₃FeSi₆) by the reaction L+Al₅FeSi→α-Al+Si+Al₈Mg₃FeSi₆. There was a binary eutectic reaction of L→α-Al+Al₅FeSi when the Mg content exceeded 0.51% and the Fe content was higher than 0.17%. With the increase of Mg content, the volume of Mg₂Si was gradually increased while the divorced eutectic phenomenon of the quaternary eutectic structure (α-Al+Si+Mg₂Si+Al₈Mg₃FeSi₆) was weakened and the eutectic structure was significantly refined.     

Preparation of Continuous Alumina Fiber with Nano Grains by the Addition of Iron Sol

Continuous alumina fiber exhibits excellent mechanical properties owing to its dense microstructure with fine grains. In this study, alumina fiber was prepared by the sol–gel method using iron sol as a nucleating agent. It was proposed that the α-Al₂O₃ grain size be adjusted based on the modification of colloidal particle size. The effect of holding temperature and reaction material ratio on the iron colloidal particle size was studied. The microstructure of alumina fiber was characterized by scanning electron microscopy (SEM). The experiment results indicated that iron colloidal particle size increases with the holding temperature and the NH₄HCO₃/Fe(NO₃)₃·9H₂O ratio. The alumina fiber with uniform nano α-Al₂O₃ grains was obtained by calcination at 1400 °C for 5 min. The mean grain size tends to rise with the mean colloidal particle size. Using the iron sol as a nucleating agent, the fiber with a mean grain size of 22.5 nm could be formed. The tensile strength of fibers increased with the decrease of grain size.     

Very-High-Cycle Fatigue Behavior of Inconel 718 Alloy Fabricated by Selective Laser Melting at Elevated Temperature

This study investigates the very-high-cycle fatigue (VHCF) behavior at elevated temperature (650 °C) of the Inconel 718 alloy fabricated by selective laser melting (SLM). The results are compared with those of the wrought alloy. Large columnar grain with a cellular structure in the grain interior and Laves/δ phases precipitated along the grain boundaries were exhibited in the SLM alloy, while fine equiaxed grains were present in the wrought alloy. The elevated temperature had a minor effect on the fatigue resistance in the regime below 10⁸ cycles for the SLM alloy but significantly reduced the fatigue strength in the VHCF regime above 10⁸ cycles. Both the SLM and wrought specimens exhibited similar fatigue resistance in the fatigue life regime of fewer than 10⁷–10⁸ cycles at elevated temperature, and the surface initiation mechanism was dominant in both alloys. In a VHCF regime above 10⁷–10⁸ cycles at elevated temperature, the wrought material exhibited slightly better fatigue resistance than the SLM alloy. All fatigue cracks are initiated from the internal defects or the microstructure discontinuities. The precipitation of Laves and δ phases is examined after fatigue tests at high temperatures, and the effect of microstructure on the formation and the propagation of the microstructural small cracks is also discussed.     

Mitigating Inhomogeneity and Tailoring the Microstructure of Selective Laser Melted Titanium Orthorhombic Alloy by Heat Treatment,Hot Isostatic Pressing,and Multiple Laser Exposures

Titanium orthorhombic alloys based on intermetallic Ti₂AlNb-phase are attractive materials for lightweight high-temperature applications. However, conventional manufacturing of Ti₂AlNb-based alloys is costly and labor-consuming. Additive Manufacturing is an attractive way of producing parts from Ti₂AlNb-based alloys. High-temperature substrate preheating during Selective Laser Melting is required to obtain crack-free intermetallic alloys. Due to the nature of substrate preheating, the temperature profile along the build height might be uneven leading to inhomogeneous microstructure and defects. The microstructural homogeneity of the alloy along the build direction was evaluated. The feasibility of mitigating the microstructural inhomogeneity was investigated by fabricating Ti₂AlNb-alloy samples with graded microstructure and subjecting them to annealing. Hot isostatic pressing allowed us to achieve a homogeneous microstructure, eliminate residual micro defects, and improve mechanical properties with tensile strength reaching 1027 MPa and 860 MPa at room temperature and 650 °C, correspondingly. Annealing of the microstructurally graded alloy at 1050 °C allowed us to obtain a homogeneous B2 + O microstructure with a uniform microhardness distribution. The results of the study showed that the microstructural inhomogeneity of the titanium orthorhombic alloy obtained by SLM can be mitigated by annealing or hot isostatic pressing. Additionally, it was shown that by applying multiple-laser exposure for processing each layer it is possible to locally tailor the phase volume and morphology and achieve microstructure and properties similar to the Ti2AlNb-alloy obtained at higher preheating temperatures.     

Reversible Redox Property of Co(III) in Amorphous Co-Doped SiO2/γ-Al2O3 Layered Composites

This paper reports on a unique reversible reducing and oxidizing (redox) property of Co(III) in Co-doped amorphous SiO₂/γ-Al₂O₃ composites. The Fenton reaction during the H₂O₂-catalyzed sol–gel synthesis utilized in this study lead to the partial formation of Co(III) in addition to Co(II) within the composites. High-resolution transmission electron microscopy (HRTEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) analyses for the composite powder sample with a composition of Al:Si:Co = 85:10:5 showed the amorphous state of the Co-doped SiO₂ that modified γ-Al₂O₃ nanocrystalline surfaces. In situ X-ray absorption fine structure (XAFS) spectroscopic analysis suggested reversible redox reactions of Co species in the composite powder sample during heat-treatment under H₂ at 500 °C followed by subsequent cooling to RT under Ar. Further analyses by in situ IR spectroscopy combined with cyclic temperature programmed reduction/desorption (TPR/TPD) measurements and X-ray photoelectron spectroscopic (XPS) analysis revealed that the alternating Co(III)/(II) redox reactions were associated with OH formation (hydrogenation)-deformation (dehydrogenation) of the amorphous aluminosilicate matrix formed in situ at the SiO₂/γ-Al₂O₃ hetero interface, and the redox reactions were governed by the H₂ partial pressure at 250–500 °C. As a result, a supported mesoporous γ-Al₂O₃/Co-doped amorphous SiO₂/mesoporous γ-Al₂O₃ three-layered composite membrane exhibited an H₂-triggered chemical valve property: mesopores under H₂ flow (open) and micropores under He flow (closure) at 300–500 °C.     

Wear and Corrosion Resistance of Plasma Electrolytic Oxidation Coatings on 6061 Al Alloy in Electrolytes with Aluminate and Phosphate

Phosphate and aluminate electrolytes were used to prepare plasma electrolytic oxidation (PEO) coatings on 6061 aluminum alloy. The surface and cross-section microstructure, element distribution, and phase composition of the PEO coatings were characterized by SEM, EDS, XPS, and XRD. The friction and wear properties were evaluated by pin-on-disk sliding tests under dry conditions. The corrosion resistance of PEO coatings was investigated by electrochemical corrosion and salt spray tests in acidic environments. It was found that the PEO coatings prepared from both phosphate and aluminate electrolytes were mainly composed of α-Al₂O₃ and γ-Al₂O₃. The results demonstrate that a bi-layer coating is formed in the phosphate electrolyte, and a single-layered dense alumina coating with a hardness of 1300 HV is realizable in the aluminate electrolyte. The aluminate PEO coating had a lower wear rate than the phosphate PEO coating. However, the phosphate PEO coating showed a better corrosion resistance in acidic environment, which is mainly attributed to the presence of an amorphous P element at the substrate/coating interface.     

Achieving Ti-5Al-4Sn-2Zr-1Mo-0.25Si-1Nb Alloys with High Strength and Moderate Ductility through Selective Laser Melting

Ti-5Al-4Sn-2Zr-1Mo-0.25Si-1Nb (TA32) titanium alloy is a kind of near α high temperature titanium alloy with great application prospects in aero-engine afterburners and cruise missiles. However, there are still few studies on the microstructure and mechanical properties of TA32 specimens produced by selective laser melting (SLM) technology. In this study, TA32 specimens with high strength (tensile strength of 1267 MPa) and moderate ductility (elongation after fracture of 8%) were obtained by selective laser melting. The effect of laser power on the microstructure and mechanical behavior was studied and the results demonstrated that the average grain size increases with increasing laser power from 200 W to 400 W. Micro-zone composition analysis was carried out by energy dispersion spectrum (EDS), showing that the Al concentration inner grains is higher than that near grain boundaries. Fracture analysis results demonstrated that the fracture mode of SLM TA32 specimens was cleavage fracture. The tensile strength of the specimens built with a laser power of 250 W at 500 °C, 550 °C and 600 °C was measured as 869 MPa, 819 MPa and 712 MPa, respectively.     

Microstructural Tailoring and Enhancement in Compressive Properties of Additive Manufactured Ti-6Al-4V Alloy through Heat Treatment

Among laser additive manufacturing, selective laser melting (SLM) is one of the most popular methods to produce 3D printing products. The SLM process creates a product by selectively dissolving a layer of powder. However, due to the layerwise printing of metal powders, the initial microstructure is fully acicular α′-martensitic, and mechanical properties of the resultant product are often compromised. In this study, Ti-6Al-4V alloy was prepared using SLM method. The effect of heat treatment was carried out on as-built SLM Ti-6Al-4V alloy from 650–1000 °C to study respective changes in the morphology of α/α′-martensite and mechanical properties. The phase transition temperature was also analyzed through differential thermal analysis (DTA), and the microstructural studies were undertaken by optical microscopy (OM) and scanning electron microscopy (SEM). The mechanical properties were assessed by microhardness and compressive tests before and after heat treatment. The results showed that heat treated samples resulted in a reduction in interior defects and pores and turned the morphology of the α′-martensite into a lamellar (α + β) structure. The strength was significantly reduced after heat treatment, but the elongation was improved due to the reduction in columnar α′-martensite phase. An optimum set of strength and elongation was found at 900 °C.     

Corrosion Behavior of Detonation Gun Sprayed Fe-Al Type Intermetallic Coating

The detonation gun sprayed Fe-Al type coatings as an alternative for austenitic valve steel, were investigated using two different methods of testing corrosion resistance. High temperature, 10-hour isothermal oxidation experiments at 550, 750, 950 and 1100 °C show differences in the oxidation behavior of Fe-Al type coatings under air atmosphere. The oxide layer ensures satisfying oxidation resistance, even at 950 and 1100 °C. Hematite, α-Al₂O₃ and metastable alumina phases were noticed on the coatings top surface, which preserves its initial thickness providing protection to the underlying substrate. In general, only negligible changes of the phase composition of the coatings were noticed with simultaneous strengthening controlled in the micro-hardness measurements, even after 10-hours of heating at 1100 °C. On the other hand, the electrochemical corrosion tests, which were carried out in 200 ppm Cl⁻ (NaCl) and pH ~4 (H₂SO₄) solution to simulate the acid-rain environment, reveal higher values of the breakdown potential for D-gun sprayed Fe-Al type coatings than the ones for the bulk Fe-Al type alloy and Cr21Mn9Ni4 austenitic valve steel. This enables these materials to be used in structural and multifunctional applications in aggressive environments, including acidic ones.     

Deformation Behavior and Tensile Properties of the Semi-Equiaxed Microstructure in Near Alpha Titanium Alloy

The tensile deformation and fracture behavior of a particular semi-equiaxed microstructure (S-EM) in a near alpha titanium alloy TA19 are investigated by an in situ method. In the S-EM, the thin β lamellae grow through the equiaxed α_p phase (α_p), and the original α_p/β_trans interface in the bimodal microstructure largely disappears, forming a blurry interface between the semi-equiaxed α_p phase (equiaxed α_p phase that is grew through by the thin β lamellae) and the transformed β microstructure (β_trans). The formation of dense slip bands inside the semi-equiaxed α_p phase in the S-EM is inhibited by the thin β lamellae during the tensile deformation. The special characteristics of the S-EM reduce the stress concentration at the interface, and the crack initiation probability in the blurry semi-α_p/β_trans interface decreased compared to the distinct α_p/β_trans interface in a conventional equiaxed microstructure (EM). Moreover, the ultimate tensile strength of the S-EM is higher than that of the EM with a slight loss of plasticity.     

In Situ Observation of the Tensile Deformation and Fracture Behavior of Ti–5Al–5Mo–5V–1Cr–1Fe Alloy with Different Microstructures

The plastic deformation processes and fracture behavior of a Ti–5Al–5Mo–5V–1Cr–1Fe alloy with bimodal and lamellar microstructures were studied by room-temperature tensile tests with in situ scanning electron microscopy (SEM) observations. The results indicate that a bimodal microstructure has a lower strength but higher ductility than a lamellar microstructure. For the bimodal microstructure, parallel, deep slip bands (SBs) are first noticed in the primary α (α_p) phase lying at an angle of about 45° to the direction of the applied tension, while they are first observed in the coarse lath α (α_L) phase or its interface at grain boundaries (GBs) for the lamellar microstructure. The β matrix undergoes larger plastic deformation than the α_L phase in the bimodal microstructure before fracture. Microcracks are prone to nucleate at the α_p/β interface and interconnect, finally causing the fracture of the bimodal microstructure. The plastic deformation is mainly restricted to within the coarse α_L phase at GBs, which promotes the formation of microcracks and the intergranular fracture of the lamellar microstructure.     

Sodium Solid Electrolytes: NaxAlOy Bilayer-System Based on Macroporous Bulk Material and Dense Thin-Film

A new preparation concept of a partially porous solid-state bilayer electrolyte (BE) for high-temperature sodium-ion batteries has been developed. The porous layer provides mechanical strength and is infiltrated with liquid and highly conductive NaAlCl₄ salt, while the dense layer prevents short circuits. Both layers consist, at least partially, of Na-β-alumina. The BEs are synthesized by a three-step procedure, including a sol-gel synthesis, the preparation of porous, calcined bulk material, and spin coating to deposit a dense layer. A detailed study is carried out to investigate the effect of polyethylene oxide (PEO) concentration on pore size and crystallization of the bulk material. The microstructure and crystallographic composition are verified for all steps via mercury intrusion, X-ray diffraction, and scanning electron microscopy. The porous bulk material exhibits an unprecedented open porosity for a Na_xAlO_y bilayer-system of ≤57% with a pore size of ≈200–300 nm and pore volume of ≤0.3 cm³∙g⁻¹. It contains high shares of crystalline α-Al₂O₃ and Na-β-alumina. The BEs are characterized by impedance spectroscopy, which proved an increase of ionic conductivity with increasing porosity and increasing Na-β-alumina phase content in the bulk material. Ion conductivity of up to 0.10 S∙cm⁻¹ at 300 °C is achieved.     

Reinforced 3D Composite Structures of γ-, α-Al2O3 with Carbon Nanotubes and Reduced GO Ribbons Printed from Boehmite Gels

The ability of boehmite to form printable inks has sparked interest in the manufacturing of 3D alumina (Al₂O₃) and composite structures by enabling direct ink writing methods while avoiding the use of printing additives. These materials may exhibit high porosity due to the printing and sintering procedures, depending on the intended application. The 3D-printed porous composite structures of γ-Al₂O₃ and α-Al₂O₃ containing 2 wt.% of carbon nanotubes or reduced graphene oxide ribbons were fabricated from boehmite gels, followed by different heat treatments. The reinforcing effect of these carbon nanostructures was evidenced by compression tests carried out on the different alumina structures. A maximum relative increase of 50% in compressive strength was achieved for the γ-Al₂O₃ composite structure reinforced with reduced graphene oxide ribbons, which was also accompanied by an increase in the specific surface area.     

Oxidation Behavior of Inconel 740H Nickel Superalloy in Steam Atmosphere at 750 °C

The oxidation behavior of the nickel superalloy Inconel 740H was studied at 750 °C for 100, 250, 500, 1000, and 2000 h in a steam atmosphere. Microstructure observations were performed using scanning electron microscopes and scanning-transmission electron microscope. The phase identification of existing oxidation products was conducted by electron diffraction in transmission electron microscope. The obtained results showed that the microstructure of Inconel 740H was stable during the oxidation process. The kinetic data showed that the superalloy has the ability to form protective oxide layers that are characterized by good adhesion and no tendency to spallation during the test. The oxidation products were mainly composed of external and internal oxides mainly at grain boundaries. The oxides in the external layer were Cr₂O₃, MnTiO_3,, and α-Al₂O₃ after 2000 h of oxidation. Internal oxides were α-Al₂O₃ and TiO₂. The occurrence of discontinuities in the internal oxidation zone was also observed after 500 h of test. It was found that the thickness of the internal oxidation zone was greater than the thickness of the external oxide layer, which proves the strong tendency of the superalloy to form internal oxides after oxidation in the steam atmosphere.     

Directionally-Dependent Mechanical Properties of Ti6Al4V Manufactured by Electron Beam Melting (EBM) and Selective Laser Melting (SLM)

An investigation of mechanical properties of Ti6Al4V produced by additive manufacturing (AM) in the as-printed condition have been conducted and compared with wrought alloys. The AM samples were built by Selective Laser Melting (SLM) and Electron Beam Melting (EBM) in 0°, 45° and 90°—relative to horizontal direction. Similarly, the wrought samples were also cut and tested in the same directions relative to the plate rolling direction. The microstructures of the samples were significantly different on all samples. α′ martensite was observed on the SLM, acicular α on EBM and combination of both on the wrought alloy. EBM samples had higher surface roughness (Ra) compared with both SLM and wrought alloy. SLM samples were comparatively harder than wrought alloy and EBM. Tensile strength of the wrought alloy was higher in all directions except for 45°, where SLM samples showed higher strength than both EBM and wrought alloy on that direction. The ductility of the wrought alloy was consistently higher than both SLM and EBM indicated by clear necking feature on the wrought alloy samples. Dimples were observed on all fracture surfaces.     

Preparation and Characterization of High-Strength Glass-Ceramics via Ion-Exchange Method

Lithium aluminosilicate glass-ceramics (LAS GCs) are ideal shell materials for mobile phones; however, the mechanical properties of LAS GCs are comparatively lower than that of other shell materials. In this work, the impact of TiO₂/(TiO₂ + ZrO₂) ratio on properties of LAS GCs was studied and the ion-exchange methods were applied to improve the mechanical properties of LAS GCs. The results show that LAS GCs with TiO₂/(TiO₂ + ZrO₂) = 1/2 exhibit the best flexural strength (109 MPa) and Vickers hardness (525 Kg/mm²). The as-prepared glass was nucleated at 560 °C for 1 h and crystallized at 720 °C for 0.5 h. The main crystalline phases of LAS GCs are β-quartz solid solution, β-spodumene solid solution, and Li₂SiO₃. Moreover, the flexural strength and Vickers hardness of LAS GCs with TiO₂/(TiO₂ + ZrO₂) = 1/2 further increased to 356 MPa and 838 Kg/mm² after an ion-exchange at 420 °C for 6 h in pure KNO₃ molten salt. The LAS GCs with enhanced mechanical strength have the potential to be applied as mobile phone back panels.     

Studying the Effect of High Substrate Temperature on the Microstructure of Vacuum Evaporated TAPC: C60 Organic Solar Thin Films

Organic solar cells (OSCs), also known as organic photovoltaics (OPVs), are an emerging solar cell technology composed of carbon-based, organic molecules, which convert energy from the sun into electricity. Key for their performance is the microstructure of the light-absorbing organic bulk heterojunction. To study this, organic solar films composed of both fullerene C₆₀ as electron acceptor and different mole percentages of di-[4-(N,N-di-p-tolyl-amino)-phenyl]-cyclohexane (TAPC) as electron donor were evaporated in vacuum in different mixing ratios (5, 50 and 95 mol%) on an ITO-coated glass substrate held at room temperature and at 110 °C. The microstructure of the C₆₀: TAPC heterojunction was studied by grazing incidence wide angle X-ray scattering to understand the effect of substrate heating. By increasing the substrate temperature from ambient to 110 °C, it was found that no significant change was observed in the crystal size for the C₆₀: TAPC concentrations investigated in this study. In addition to the variation done in the substrate temperature, the variation of the mole percent of the donor (TAPC) was studied to conclude the effect of both the substrate temperature and the donor concentration on the microstructure of the OSC films. Bragg peaks were attributed to C₆₀ in the pure C₆₀ sample and in the blend with low donor mole percentage (5%), but the C₆₀ peaks became nondiscernible when the donor mole percentage was increased to 50% and above, showing that TAPC interrupted the formation of C₆₀ crystals.     

Electrochemical Investigation of the Corrosion of Different Microstructural Phases of X65 Pipeline Steel under Saturated Carbon Dioxide Conditions

The aim of this research was to investigate the influence of metallurgy on the corrosion behaviour of separate weld zone (WZ) and parent plate (PP) regions of X65 pipeline steel in a solution of deionised water saturated with CO₂, at two different temperatures (55 °C and 80 °C) and at initial pH~4.0. In addition, a non-electrochemical immersion experiment was also performed at 80 °C in CO₂, on a sample portion of X65 pipeline containing part of a weld section, together with adjacent heat affected zones (HAZ) and parent material. Electrochemical impedance spectroscopy (EIS) was used to evaluate the corrosion behaviour of the separate weld and parent plate samples. This study seeks to understand the significance of the different microstructures within the different zones of the welded X65 pipe in CO₂ environments on corrosion performance; with particular attention given to the formation of surface scales; and their composition/significance. The results obtained from grazing incidence X-ray diffraction (GIXRD) measurements suggest that, post immersion, the parent plate substrate is scale free, with only features arising from ferrite (α-Fe) and cementite (Fe₃C) apparent. In contrast, at 80 °C, GIXRD from the weld zone substrate, and weld zone/heat affected zone of the non-electrochemical sample indicates the presence of siderite (FeCO₃) and chukanovite (Fe₂CO₃(OH)₂) phases. Scanning Electron Microscopy (SEM) on this surface confirmed the presence of characteristic discrete cube-shaped crystallites of siderite together with plate-like clusters of chukanovite.