Metallographic Sections Research Articles

Mechanisms of Increasing Weld Depth during Temporal Power Modulation in High‐Power Laser Beam Welding

Understanding the fundamental mechanisms of action for increasing weld depth during temporal power modulation in laser beam welding could allow dissimilar rotational welding without the introduction of concomitant turbulence, but with enhanced intermixing. The investigations are conducted on 30 mm‐diameter round bars of stainless steel alloy 1.4301 and nickel base alloy 2.4856 utilizing a 16 kW disk laser beam source. Modulation frequencies are 0/50/100/200 Hz at low, medium, and high amplitudes of laser beam power. The influence on the process and weld characteristics is investigated through high‐speed imaging with grayscale analysis, keyhole depth measurements, metallographic sections, and energy‐dispersive X‐ray spectroscopy analysis. The objectives are successfully achieved, and the underlying mechanism is maintaining the keyhole depth at a higher level for modulation frequencies of 200 Hz and a high amplitude of laser beam power, which is related to the keyhole inertia. Based on this, a novel welding mode with a constant keyhole depth is proposed. Furthermore, up to 20% increase in weld depth is achieved, a saturation limit for the modulation frequency is identified, intermixing within the weld is enhanced, and a model for predicting the weld depth based solely on measurements of the surface width is developed.

A Dynamic Volumetric Heat Source Model for Laser Additive Manufacturing

Melt pool scale models of laser powder bed fusion (LPBF) offer insights into the process-structure-property relationships in additive manufacturing (AM). These models often neglect physical phenomena such as vapor cavity formation and fluid mechanics to reduce computational demands. Instead, volumetric heat source models are used to represent the effects that these phenomena have on the predicted melt pool dimensions. Generally, the dimensions and effective absorption of the volumetric heat source are calibrated to reproduce melt pool dimensions observed in metallographic cross sections taken from single-track experiments on bare plate. However, the transient nature of LPBF often deviates the melt pool dimensions from the assumed steady-state conditions of single-track experiments, motivating the need for a volumetric heat source model that more generally considers the dynamic relationship between melt pool shape and laser-material interactions. Here, we introduce a two-parameter volumetric heat source model that integrates several existing models into a generalized mathematical expression, providing independent control over the radial heat distribution via the parameter k and the volumetric shape of the heat source via the parameter m. This parameterization enables the calibration of melt pool shape predictions through simultaneous adjustment of these parameters, while keeping the radial heat source dimensions consistent with the experimental spot size (D4σ) and constraining the heat source depth and absorption to physically derived expressions for cavities. Consequently, the proposed volumetric heat source model adapts to changes in the local melt pool conditions due to scanning strategy and part geometry by dynamically adjusting the heat source depth and absorption. We demonstrate the capabilities of the proposed model through comparisons with a collection of experiments from the Additive Manufacturing Benchmark (AMBench).

Evaluating copper plating process for filling micro vias with thin surface Cu by the 1-(4-carboxyphenyl)-5-mercapto-1H-tetrazole additive

The 1-(4-carboxyphenyl)-5-mercapto-1 h-tetrazole (CMHT) as a novel leveler for the overfilling of micro-blind vias was investigated in acidic copper electroplating. The synergistic effect between CMHT and other additives were confirmed through chronoamperometry, cyclic voltammetry and electrochemical impedance spectroscopy. The results showed a convection-dependent interaction between the CMHT and suppressor (propyleneoxide (PO)-ethylene oxide (EO)-propylene oxide (PO), named PEP). Metallographic section testing demonstrated that the CMHT not only have excellent microvia filling performances, but also only have 19.1 μm thin surface Cu for micro blind vias with a diameter of 150 µm and a depth of 80 µm by the electrodepositing 60 min of 2 A/dm2. The quantum chemical calculations experiments revealed also that the CMHT parallel orientation of the benzene ring and tetrazole heterocycle can enhance the effective adsorption area. The obtained results from electrochemical test and quantum chemical calculations were in reasonably good agreement.

Challenges and possibilities of the manual metallographic serial sectioning process using the example of a quantitative microstructural analysis of graphite in cast iron

Abstract The 3D microstructure analysis presented in this study focuses on the nodular graphite of an EN-GJS grade cast iron. The shape is analyzed based on shape factor and aspect ratio as well as average particle size and distribution. The shape of graphites in cast iron materials is critical to the mechanical properties of these alloys and is essential for the characterization of the material. Metallographic serial sectioning creates a digital twin of the material, which is removed layer by layer and visualized layer by layer under an optical microscope. From this three-dimensional twin, any number of planes can be digitally projected and analyzed. Conventional quantitative 3D analysis examines the voxel count and composition of a body in 3D space. The analysis presented here applies stereological 2D analysis methods to three spatial planes of the material. Two of the planes are digital projections of the twin. The two reconstructed planes of the material are chosen so that the direction vectors of all three planes form an angle of 90° to each other. The methodology is described in detail and the challenges and opportunities of the serial section method presented here are discussed.

Effects of heat treatment on the microstructure and corrosion behavior of manganese aluminum bronzes

Abstract Due to a much lower nickel content, manganese aluminum bronzes (MAB) are a cost-effective alternative to nickel aluminum bronzes (NAB). When the material is processed, different microstructures are observable in the material which have an impact on the corrosion resistance of MAB alloys. MAB samples were annealed at 900 °C and quenched in water. After that, annealing treatments at 600, 500, 400 and 300 °C for up to 24 h were performed and the samples were again quenched in water. Metallographic sections were prepared from all samples and potentiostatic corrosion tests at different potentials were performed in synthetic seawater. It was found that the sample annealed at 900 °C and quenched in water as well as those samples which underwent a second annealing treatment at low temperatures for shorter times exhibited a greater corrosion tendency than those undergoing a second annealing treatment at higher temperatures. X-ray diffraction measurements revealed that phase transformations and changes in grain size occurred during the annealing treatments. The increase in corrosion resistance as a result of annealing at higher temperatures is probably due to the strong intergrowth of the phases that are formed.

Debonding of Porous Coating: A Late Failure Mode of Uncemented, Partially Threaded Acetabular Components—Retrieval Analysis

Titanium plasma-sprayed (TPS) porous coatings have been used in total hip arthroplasty for decades. They are considered reliable, and very few failure cases have been described so far. This retrieval study described a series of 20 acetabular components—where total or partial debonding occurred during in vivo use and aimed to explain the underlying failure mechanisms. Implants were examined using optical and electron microscopy (SEM), metallographic sections of retrievals were prepared while pathologic samples of periprosthetic tissues were examined for presence of wear debris. Data from metallographic slides indicated that debonding was initiated at free borders of the coating and tended to progress at the interface between the TPS layer and the shell. In some cases, total debonding occurred leading material wear of both the TPS layer and acetabular shell leading to massive release of metallic debris and accelerated polyethylene wear in third body mechanism. SEM examination demonstrated that splats forming the TPS layer exhibited features suggesting a high temperature gradient between the plasma sprayed layer and the substrate material existed, leading to porosity of splats and suboptimal bonding strength. This study demonstrated that coating application parameters and certain design features (screw holes, fins) may promote long-term failure due to debonding. Surgeons should be aware of this complication as it is most likely underreported, while manufacturers should consider more rigorous pre-clinical testing as suboptimal coating bonding may result in failures during long-term clinical use.

In-situ computed tomography and transient dynamic analysis – failure analysis of a single-lap tensile-shear test with clinch points

Clinching is a mechanical joining technology, in which a mainly form-fit joint is created by means of local cold forming. To characterize the load-bearing behavior of such joints, they are typically analyzed destructively, for example by tensile-shear tests in combination with metallographic sections. However, both the initiation and progress of failure can only be described to a limited extent by this method. Furthermore, these tests allow only limited conclusions about clinch points under in-service loading. More purposefully, clinch points can be analyzed nondestructively by combining in-situ computed tomography (CT) and transient dynamic analysis (TDA). The TDA continuously measures the dynamic behavior of the specimen and indicates failure events like crack initiation, which then can be evaluated thoroughly by stopping the test and performing a CT scan. To qualify the TDA for this task, it is necessary to link the observed damage behavior with specific dynamic characteristics. In this work, the complementation of in-situ CT and TDA is investigated by testing a clinched single-lap tensile-shear specimen made of aluminum. The testing procedure is stepwise: at certain displacement levels, the specimen is investigated by in-situ CT and TDA. While the in-situ CT provides the location, extent, and development of the failure phenomena, the TDA uses this information to evaluate the dynamic signal and detect relevant frequency ranges, which indicate damage events. The results demonstrate, that failure initiation and progression can be analyzed efficiently by combining both measuring systems. The TDA reliably detects relevant signal changes in the monitored frequency band. By means of in-situ computed tomography, the corresponding failure phenomena can be described in detail, enhancing the understanding of the load-bearing and deformation behavior of clinch points. The concatenation of characteristic signal changes and observed failure phenomena can henceforth be transferred to analyze complex structures during operation nondestructively by TDA.

Mechanical Properties of the AlCu4Mg1 Alloy Joint Manufactured by Underwater Friction Stir Welding.

The manuscript presents the results of butt joining of 3-millimeter-thick AlCu4Mg1 alloy sheets using the FSW (friction stir welding) and UWFSW (underwater friction stir welding) methods. The aim of the research is to verify the influence of the water environment on the FSW friction welding process. The article checked three sets of joint parameters. The parameters differed in tool rotation speed and feed rate. The same sets of parameters were used for the FSW and UWFSW fusion techniques. With the supplied devices, metallographic sections are cross-sectioned, and the power supplies are subjected to a light microscope. Microhardness tests and the influence of the heat-affected zone were carried out. A monotonic test was performed. A monotonic test is available, extended with a visual correlation test. The obtained cracked fracture surfaces were examined using a scanning microscope. An analysis of the microfractographic cracking process was carried out. The obtained results did not show any improvement in the strength properties of the obtained joints made using the UWFSW technique when using a scanning microscope.

Influence of Process Energy on the Formation of Imperfections in Body-Centered Cubic Cells with Struts in the Vertical Orientation Produced by Laser Powder Bed Fusion from the Magnesium Alloy WE43.

The low specific density and good strength-to-weight ratio make magnesium alloys a promising material for lightweight applications. The combination of the properties of magnesium alloys and Additive Manufacturing by the Laser Powder Bed Fusion (LPBF) process enables the production of complex geometries such as lattice or bionic structures. Magnesium structures are intended to drastically reduce the weight of components and enable a reduction in fuel consumption, particularly in the aerospace and automotive industries. However, the LPBF processing of magnesium structures is a challenge. In order to produce high-quality structures, the process parameters must be developed in such a way that imperfections such as porosity, high surface roughness and dimensional inaccuracy are suppressed. In this study, the contour scanning strategy is used to produce vertical and inclined struts with diameters ranging from 0.5 to 3 mm. The combination of process parameters such as laser power, laser speed and overlap depend on the inclination and diameter of the strut. The process parameters with an area energy of 1.15-1.46 J/mm2 for struts with a diameter of 0.5 mm and an area energy of 1.62-3.69 J/mm2 for diameters of 1, 2 and 3 mm achieve a relative material density of 99.2 to 99.6%, measured on the metallographic sections. The results are verified by CT analyses of BCCZ cells, which achieve a relative material density of over 99.3%. The influence of the process parameters on the quality of struts is described and discussed.

Investigation of Tool Degradation during Friction Stir Welding of Hybrid Aluminum-Steel Sheets in a Combined Butt and Overlap Joint.

Friction stir welding, as a solid-state welding technique, is especially suitable for effectively joining high-strength aluminum alloys, as well as for multi-material welds. This research investigates the friction stir welding of thin aluminum and steel sheets, an essential process in the production of hybrid tailor-welded blanks employed in deep drawing applications. Despite its proven advantages, the welding process exhibits variable outcomes concerning formability and joint strength when utilizing an H13 welding tool. To better understand these inconsistencies, multiple welds were performed in this study, joining 1 mm thick steel to 2 mm thick aluminum sheets, with a cumulative length of 7.65 m. The accumulation of material on the welding tool was documented through 3D scanning and weighing. The integrity of the resulting weld seam was analyzed through metallographic sections and X-ray imaging. It was found that the adhering material built up continuously around the tool pin over several welds totaling between 1.5 m and 2.5 m before ultimately detaching. This accretion of material notably affected the welding process, resulting in increased intermixing of steel particles within the aluminum matrix. This research provides detailed insights into the dynamics of friction stir welding in multi-material welds, particularly in the context of tool material interaction and its impact on weld quality.

Relation of nonmetallic inclusions to the cyclic properties of steel 42CrMo4 after steel melt cleaning by filtration and related processes

Nonmetallic inclusions (NMIs) detrimentally influence the steel properties. The application of metal melt filter systems promises to reduce NMIs in steel. In the current work, NMIs are analyzed from metallographic sections after metal melt filtration or cleaning by a related process of the steel 42CrMo4 using immersion filtration, flow-through filtration as well as filters floating on top of the melt. Analyses by automated scanning electron microscopy (ASPEX) as well as light optical microcopy (LOM) revealed the chemistry, size distribution, and morphology of NMIs. The filter systems had a significant effect on these characteristics of NMIs. The threshold value ΔKth against fatigue crack propagation was found to depend on the amount of NMIs within the steel. A higher amount of NMIs caused less crack deflection leading to less roughness-induced crack closure and in turn resulted in lower threshold values at a stress ratio of R = 0.1. The comparison of the present analysis of NMIs with fatigue data from previous work indicated that the analysis of NMIs from metallographic sections can be used to approximate the fatigue strength of a batch in the same way as the analysis of NMIs from fatigue fracture surfaces for single specimens, as suggested by Murakami.

Local laser heat treatment of AlSi10Mg as-built parts produced by Laser Powder Bed Fusion

Today, complex structural components for lightweight applications are frequently manufactured by laser powder bed fusion (PBF-LB), often using aluminum alloys such as AlSi10Mg. However, the application of cyclic load cases can be challenging as PBF-LB produced AlSi10Mg parts typically have low ductility and corresponding brittle failure behavior in the as-built condition.Therefore, this paper presents investigations on the feasibility of a laser heat treatment of PBF-LB produced AlSi10Mg parts to locally increase the ductility and decrease the hardness in critical areas. Potential heat treatment process parameters were derived theoretically based on the temperature fields in the material calculated assuming three-dimensional heat conduction and a moving heat source. PBF-LB produced specimens were then laser heat treated at varying laser power and scan speed. Hardness measurements on metallographic cross sections showed hardness reductions of over 35 % without inducing hydrogen pore growth.

Oxide scale microstructure and failure mechanism of alloy 601 under varying metal dusting conditions

Chemical plants which process highly carbonaceous gases at elevated temperatures are prone to catastrophic corrosion by metal dusting. Typically, commercial alloys with high amounts of protective oxide scale formers (Cr, Al, and Si) are used in these environments. However, scale failure is still frequently observed after an incubation time initiating pits. In this study, the microstructure and subsequent metal dusting-induced failure of the oxide scale on the commercial Ni-based alloy 601 was analyzed. Samples were exposed in different aggressive metal dusting gases and characterized using metallographic cross sections, electron beam microanalysis (EPMA), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and transmission electron microscopy (TEM). A thin and protective chromia scale formed in some regions with a continuous silica layer below. Across most of the alloy 601 surfaces, internal oxidation of Al could be linked to metallic particles in the outer scale. Additionally, MnCr2O4 was observed in the outer scale. Together with pores in the chromia, the spinel and metallic particles in the outer scale combined to provide pathways for carbon ingress. After exposure in a gas with a higher driving force for carbon deposition, a higher amount of carbon was incorporated in the growing oxide scale, resulting in earlier scale failure and metal dusting pit initiation.Graphical

Temporal power modulation in high power laser beam welding of round bars

Temporal power modulation bears an enormous potential for high power laser beam welding of round bars since all its specific challenges are faced. They can be summarised as deviating welding conditions towards the round bar‘s centre. Accordingly, a tailored amount of energy would be provided to that area. The investigations are conducted on 30 mm diameter bars of 1.4301 stainless steel with the use of a 16 kW disk laser. The modulation parameters comprise 6/12/50/100/200 Hz modulation frequency and 0.30/0.47/0.73 modulation depth or power modulation ratio. Post analysis focuses on metallographic longitudinal sections and calculations. The modulation‘s outstanding capability is creating deeper and narrower weld seams due to higher peak power and more intense evaporation of protrusions along the keyhole front wall. Therefore, more laser power is provided to the weld root and despite applying lower average power, the same weld depth is achieved. Finally, more ecological and economical welding as well as welding of more temperature sensitive materials is enabled.

Using ultrasonic atomization to recycle aluminium bronze chips for additive laser directed energy deposition

In the post-processing of large maritime components, a considerable amount of waste in the form of milling and grinding chips is produced. At the same time, additive manufacturing technologies have shown great potential in producing high-volume parts for maritime applications, allowing novel design approaches and short lead times. In this context, this study presents a sustainable approach to recycle and use aluminium bronze waste material, generated during post-processing of large cast ship propellers, as feedstock for laser-powder directed energy deposition. The recycling technology used to produce powder batches is inductive re-melting in combination with ultrasonic atomization. The derived metal powders are characterized using digital image analysis, powder flowability tests, scanning electron microscopy as well as energy dispersive X-ray spectroscopy. Compared to conventional metal powders produced by gas atomization, the recycled material shows excellent sphericity and a powder size distribution with a higher content of finer and coarser particles. Metallographic sections of deposited additively produced specimens show an increased hardness and reduced ductility, but also competitive densities and higher yield and ultimate tensile strength compared to cast material. The process chain shows high potential for the maritime sector to enable circular and sustainable manufacturing.

Process development and process adaption guidelines for the deposition of thin-walled structures with IN718 using extreme high-speed directed energy deposition (EHLA3D)

Extreme high-speed directed energy deposition (EHLA) is a modified variant of the laser based directed energy deposition (DED-LB) and is being applied as an efficient coating process for rotational symmetric components. Characteristics of EHLA processes are feed rates of up to 200 m/min, which result in smaller weld bead deposition and thinner layer thicknesses compared to conventional DED-LB. When transferred to additive manufacturing, this characteristic utilizes the potential of depositing thin-walled filigree structures at deposition rates, which are comparable to typical DED-LB processes (EHLA3D). The results of this work were achieved with an EHLA3D machine, which is a modified CNC-type machine capable of operating feed rates with vf = 30 m/min. In this work, process parameters were developed for the deposition of thin-walled filigree structures with the Ni-based superalloy IN718. Single tracks with constant feed rates and a variation in the beam diameter and powder mass flow were deposited and analyzed regarding the resulting weld bead dimension and dilution zone. Then, process parameters were selected and transferred to the deposition of thin walls, and guidelines of the parameter adaption toward thin-walled deposition were defined. Two parameter sets were developed to assess the feasible wall-thicknesses deposited by EHLA3D. Depending on the developed parameter sets, wall thicknesses between 300 and 500 μm are achieved. To characterize the resulting thin-walls, surface roughness measurements and metallographic cross sections were conducted.

Functionality and Mechanical Performance of Miniaturized Non-Assembly Pin-Joints Fabricated in Ti6Al4V by Laser Powder Bed Fusion.

In this work, additively manufactured pin-joint specimens are analyzed for their mechanical performance and functionality. The functionality of a pin-joint is its ability to freely rotate. The specimens were produced using laser powder bed fusion technology with the titanium alloy Ti6Al4V. The pin-joints were manufactured using previously optimized process parameters to successfully print miniaturized joints with an angle to the build plate. The focus of this work lies in the influence of joint clearance, and therefore all specimens were manufactured with a variety of clearance values, from 0 µm up to 150 µm, in 10 µm steps. The functionality and performance were analyzed using torsion testing and tensile testing. Furthermore, a metallographic section was conducted to visually inspect the clearances of the additively manufactured pin-joints with different joint clearance values. The results of the torsion and tensile tests complement each other and emphasize a correlation between the joint clearance and the maximal particle size of the powder utilized for manufacturing and the mechanical behavior and functionality of the pin-joints. Non-assembly multibody pin-joints with good functionality were obtained reliably using a joint clearance of 90 µm or higher. Our findings show how and with which properties miniaturized pin-joints that can be integrated into lattice structures can be successfully manufactured on standard laser powder bed fusion machines. The results also indicate the potential and limitations of further miniaturization.

Dezincification in cast and heat-treated alpha-beta brass samples

Abstract Two α-β brass alloys with varying Zn contents have been studied. The samples received for examination were heat-treated at 500 °C in order to conduct dezincification studies according to EN ISO 6509-1 and to measure the depth of dezincification from metallographic sections. According to the phase diagram, the α-phase content should increase as a result of heat-treatment at 500 °C. This phenomenon, however, is difficult to observe in the metallographic sections which were prepared from the heattreated samples. When analyzing the depth of dezincification, it was found that reduced dezincification occurred in the heat-treated samples. This is plausible since β brass is attacked by preferential corrosion. Not only was uniform layer dezincification observed in the brass alloy with the higher Zn content, but also the onset of plug dezincification. This is associated with the original microstructure of the brass which is characterized by a coarse primary grain size. In this alloy, it is clearly observed that larger areas containing alpha brass will impede the process of dezincification.

Development of an automated 3D metallography system and some first application examples in microstructural analysis

Abstract Traditional metallography relies on the imaging of individual section planes. However, conclusions as to spatial shapes and microstructural arrangements can only be drawn to a limited extent. The idea to reconstruct three-dimensional microstructures from metallographic serial sections is therefore obvious and not at all new. However, the manual process of preparing a great number of individual sections and assembling them into image stacks is time-consuming and laborious and therefore constitutes an obstacle to frequent use. This is why the Federal Institute for Materials Research and Testing, or BAM for short (Bundesanstalt für Materialforschung und -prüfung), is developing a robot-assisted 3D metallography system performing the tasks of preparation and image acquisition on a metallographic section fully automatically and repeatedly. Preparation includes grinding, polishing and optional etching of the section surface. Image acquisition is performed using a light optical microscope with autofocus at several magnification levels. The obtained image stack is then pre-processed, segmented and converted to a 3D model resembling a microtomographic image, but with a higher lateral resolution at large volumes. As opposed to tomographic techniques, it is possible to perform traditional chemical etching for contrasting. The integration of a scanning electron microscope is in the planning stages. Studies conducted so far have demonstrated the possibility of visualizing hot gas corrosion layers, gray cast irons and ceramic-based microelectronic structures (vias).

A Crystallographic Basis for Critically Evaluating the Mechanisms for Secondary Grain Formation During Directional Solidification

AbstractA crystallography-based method is presented for the critical appraisal of possible mechanisms that trigger the formation of secondary grains during directional solidification. The method permits an analysis of a large population of defects, while avoiding the pitfalls of the metallographic sectioning approach that is affected by dendrite stereology. Here, the nickel-base superalloy CMSX-4, an alloy commonly used for single crystal turbine blade applications, is studied. All secondary grains originate exclusively at the external surface and when the off-axial primary $$\langle 0\,0\,1\rangle$$ ⟨ 0 0 1 ⟩ crystal orientations are measured, are evident at both the converging and diverging dispositions of the single crystal primary dendrites without a noticeable bias. Almost all of the secondary grains have low misorientations, with an average misorientation between 5 to 15 deg. No systematic deviation between the individual $$\langle 0\,0\,1\rangle$$ ⟨ 0 0 1 ⟩ orientations of the secondary grain and the single crystal is observed. A significant twist contribution about an axis within ~ 30 deg from one of the secondary arms occurs when primary arms converge on the external surface, but both twist and tilt prevail for the diverging case. Both nucleation and buoyancy driven thermo-solutal convection can be eliminated as potential mechanisms. Thermo-mechanical deformation is deduced to be the most likely mechanism; deformation must originate in the vicinity of the primary dendrite tips. It is proposed that dendrite deflection arises primarily from the resistance encountered by the primary tips with the external surface during axial contraction in the presence of a dominant vertical thermal gradient.