Search results for: Intermetallic

Authors: Minoo Tavakoli, Alireza Kiani Rashid, Abbas Afrasiabi

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An aluminum coating deposited on mild steel substrate by electric arc spray and diffused to the base steel material by diffusion treatment at 800 and 900°C for 1 and 3 hours in a static air. Alloy layers formed by diffusion at both temperatures were investigated, and their features were compared with those of pack cementation aluminized steel. High-temperature oxidation tests were carried out in air at 600 °C for 145 hours. Results indicated that the aluminide coatings obtained from this process have significantly improved the high-temperature oxidation resistance in both methods due to the Al2O3 scale formation. Furthermore, it showed that the isothermal oxidation resistance of arc spray technique is better than pack cementation method. This can be attributed to voids that formed at the intermetallic layer /Al layer interface which is increased in the pack cementation method.

Keywords: electric arc spray, pack cementation, oxidation resistance, aluminized steel

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Authors: Ahmet Yonetken, Ayhan Erol

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The microstructure, mechanical properties and corrosion characteristics of Ni plated %10Al2O3-%40Co-%20Cr and %10Ti powders were investigated using specimens produced by tube furnace sintering at 800-1200°C temperature. A uniform nickel layer on Al2O3-Co-Cr and Ti powders was deposited prior to sintering using electroless plating technique. A composite consisting of quintet additions, a metallic phase, Ti,Cr and Co including a ceramic phase, alumina, within a matrix of Ni has been prepared under Ar shroud and then tube furnace sintered. XRD, SEM (Scanning Electron Microscope), corrosion behavior in acidic media were investigated to characterize the properties of the specimens. Experimental results carried out for composition (%10Al2O3-%40Co-%20Cr- %10Ti)20Ni at 1200°C suggest that the best properties as 312.18HV were obtained at 1200°C.

Keywords: sintering, intermetallic, Electroless nickel plating, composite

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Authors: Mahdi Amne Elahi, Marcus Koch, Peter Plapper

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Due to the demand of miniaturizing in automotive industry, the application of laser welding is quite promising. The current study focused on laser micro-welding of CuSn6 bronze and nickel wire for a miniature electromechanical hybrid component. Due to the advantages of laser welding, the welding can be tailored specifically for the requirements of the part. Scanning electron and optical microscopy were implemented to study the microstructure and tensile-shear test was selected to represent the mechanical properties. Different welding sides, beam oscillations, and speeds have been investigated to optimize the tensile-shear load and microstructure. The results show that the mechanical properties and microstructure of the joint is highly under the influence of the mentioned parameters. Due to the lack of intermetallic compounds, the soundness of the joint is achievable by manipulating the geometry of the weld seam and minimize weld defects.

Keywords: bronze, laser micro-welding, microstructure, nickel, tensile shear test

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Authors: Xiangfang Xu, Bintao Wu, Yugang Miao, Duanfeng Han

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Experiments were conducted on 5A06 aluminum alloy and Q235 steel using the laser-TIG hybrid heat source welding-brazing method to realize the reliable connection of Al/Fe dissimilar metals and the welding characteristics were analyzed. It was found that the joints with uniform seam and high tensile strength could be obtained using such a method, while the welding process demanded special welding parameters. Spectrum measurements showed that the Al and Fe atoms diffused more thoroughly at the brazing interface and formed a 3μm-thick intermetallic compound layer at the Al/Fe joints brazed connection interface. Shearing tests indicated that the shearing strength of the Al/Fe welding-brazed joint was 165MPa. The fracture occurred near the melting zone of aluminum alloy, which belonged to the mixed mode with the ductile fracture as the base and the brittle fracture as the supplement.

Keywords: Al/Fe dissimilar metals, laser-TIG hybrid heat source, shearing strength, welding-brazing method

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Authors: Yu-Ting Wang, Yun-Hsiang Cheng, Chien-Cheng Lin, Kun-Lin Lin

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Using a transient liquid phase method, Al was successfully bonded with Al₂O₃, which deposited Ni, Cu, Ge, and Si at the surface of the Al₂O₃ substrate after annealing at the relatively low melting point of Al. No reaction interlayer existed at the interface of any Al/Al₂O₃ specimens. Al−Fe intermetallic compounds, such as Al₉Fe₂ and Al₃Fe, formed in the Al substrate because of the precipitation of Fe, which was an impurity of the Al foil, and the reaction with Al at the grain boundaries of Al during annealing processing. According to the evaluation results of mechanical and thermal properties, the Al/Al₂O₃ specimen deposited on the Ni film possessed the highest shear strength, thermal conductivity, and bonding area percentage, followed by the Cu, Ge, and Si films. The properties of the Al/Al₂O₃ specimens deposited with Ge and Si were relatively unsatisfactory, which could be because the deposited amorphous layers easily formed oxide, resulting in inferior adhesion between Al and Al₂O₃. Therefore, the optimal choice for use in high-power devices is Al/Al₂O₃, with the deposition of Ni film.

Keywords: direct-bonded aluminum, transient liquid phase, thermal conductivity, microstructures, shear strength

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Authors: Ouafek Nora, Keghouche Nassira, Dehdouh Heider, Untidt Carlos

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A lot of knowledge has been accumulated on the metal clusters supported on oxide surfaces because of their multiple applications in microelectronics, heterogeneous catalysis, and magnetic devices. In this work, the surface state of Ni / MgO has been studied by XPS (X-ray Photoemission Spectroscopy). The samples were prepared by impregnation with ion exchange Ni²⁺ / MgO, followed by either a thermal treatment in air (T = 100 -350 ° C) or a gamma irradiation (dose 100 kGy, 25 kGy dose rate h -1). The obtained samples are named after impregnation NMI, NMR after irradiation, and finally NMC(T) after calcination at the temperature T (T = 100-600 °C). A structural study by XRD and HRTEM reveals the presence of nanoscaled Ni-Mg intermetallic phases (Mg₂Ni, MgNi₂, and Mg₆Ni) and magnesium hydroxide. Mg(OH)₂ in nanometric range (2- 4 nm). Mg-Ni compounds are of great interest in energy fields (hydrogen storage…). XPS spectra show two Ni2p peaks at energies of about 856.1 and 861.9 eV, indicating that the nickel is primarily in an oxidized state on the surface. The shift of the main peak relative to the pure NiO (856.1 instead of 854.0 eV) suggests that in addition to oxygen, nickel is engaged in another link with magnesium. This is in agreement with the O1s spectra which present an overlap of peaks corresponds to NiO and MgO, at a calcination temperature T ≤ 300 °C.

Keywords: XPS, XRD, nanoparticules, Ni-MgO

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Authors: Gauthier Lefevre, Holger Kohlmann, Sebastien Saitzek, Rachel Desfeux, Adlane Sayede

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Hydrogen is a promising energy carrier, compatible with the sustainable energy concept. In this context, solid-state hydrogen-storage is the key challenge in developing hydrogen economy. The capability of absorption of large quantities of hydrogen makes intermetallic systems of particular interest. In this study, efforts have been devoted to the theoretical investigation of binary systems with constraints consideration. On the one hand, besides considering hydrogen-storage, a reinvestigation of crystal structures of the palladium-arsenic system shows, with experimental validations, that binary systems could still currently present new or unknown relevant structures. On the other hand, various binary Mg-based systems were theoretically scrutinized in order to find new interesting alloys for hydrogen storage. Taking the effect of pressure into account reveals a wide range of alternative structures, changing radically the stable compounds of studied binary systems. Similar constraints, induced by Pulsed Laser Deposition, have been applied to binary systems, and results are presented.

Keywords: binary systems, evolutionary algorithm, first principles study, pulsed laser deposition

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Authors: Redrisse Djoumessi Fobasso, Baidyanath Sahu, Andre M. Strydom

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The R₂TX₃ (R = rare-earth, T = transition, and X = s and p block element) series of compounds are interesting owing to their fascinating structural and magnetic properties. In this present work, we have studied the magnetic and physical properties of the new Gd₂AgSi₃ polycrystalline compound. The sample was synthesized by the arc-melting method and confirmed to crystallize in the tetragonal α-ThSi₂-type crystal structure with space group I4/amd. Dc– and ac–magnetic susceptibility, specific heat, electrical resistivity, and magnetoresistance measurements were performed on the new compound. The structure provides a unique position in the unit cell for the magnetic trivalent Gd ion. Two magnetic phase transitions were consistently found in dc- and ac-magnetic susceptibility, heat capacity, and electrical resistivity at temperatures Tₙ₁ = 11 K and Tₙ₂ = 20 K, which is an indication of the complex magnetic behavior in this compound. The compound is found to be metamagnetic over a range of temperatures below and above Tₙ₁. From field-dependent electrical resistivity, it is confirmed that the compound shows unusual negative magnetoresistance in the antiferromagnetically ordered region. These results contribute to a better understanding of this class of materials.

Keywords: complex magnetic behavior, metamagnetic, negative magnetoresistance, two magnetic phase transitions

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Authors: Jinan B. Al-Dabbagh, Rozman Mohd Tahar, Mahadzir Ishak

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TiAl alloy nano-powder was successfully produced by a mechanical alloying (MA) technique in a planetary ball mill. The influence of milling parameters, such as the milling duration, rotation speed, and balls-to-powder mass ratio, on the characteristics of the Ti50%Al powder, including the microstructure, crystallite size refinement, and phase formation, were investigated. It was found that MA of elemental Ti and Al powders promotes the formation of TiAl alloys, as Ti (Al) solid solution was formed after 5h of milling. Milling without the addition of process control agents led to a dramatic decrease in the crystallite size to 17.8 nm after 2h of milling. Higher rotation energy and a higher ball-to-powder weight ratio also accelerated the reduction in crystallite size. Subsequent heating up to 850°C resulted in the formation of a new intermetallic phase with a dominant TiAl3 phase plus minor γ-TiAl or α2-Ti3Al phase or both. A longer milling duration also exhibited a better effect on the micro-hardness of Ti50%Al powders.

Keywords: TiAl alloys, nanocrystalline materials, mechanical alloying, materials science

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Authors: Bunty Tomar, Shiva S.

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Fabrication of steel and copper-based functionally graded material (FGM) through cold metal transfer-based wire arc additive manufacturing is a novel exploration. Components combining Cu and steel show significant usage in many industrial applications as they combine high corrosion resistance, ductility, thermal conductivity, and wear resistance to excellent mechanical properties. Joining steel and copper is challenging due to the mismatch in their thermo-mechanical properties. In this experiment, a functionally graded material (FGM) structure of pure copper (Cu) and 316L stainless steel (SS) was successfully developed using cold metal transfer-based wire arc additive manufacturing (CMT-WAAM). The interface of the fabricated samples was characterized under optical microscopy, field emission scanning electron microscopy, and X-ray diffraction techniques. Detailed EBSD and TEM analysis was performed to analyze the grain orientation, strain distribution, grain boundary misorientations, and formation of metastable and intermetallic phases. Mechanical characteristics of deposits was also analyzed using tensile and wear testing. This works paves the way to use CMT-WAAM to fabricate steel/copper FGMs.

Keywords: wire arc additive manufacturing (waam), cold metal transfer (cmt), metals and alloys, mechanical properties, characterization

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Authors: Forrest Kaatz, Adhemar Bultheel

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Au-Cu and Pt-M (M = Fe, Co, and Ni) nanocluster alloys are currently being investigated worldwide by many researchers for their interesting catalytic and nanophase properties. The low-temperature behavior of the phase diagrams is not well understood for alloys with nanometer sizes and shapes. These systems have similar bulk phase diagrams with the L12 (Au3Cu, Pt3M, AuCu3, and PtM3) structurally ordered intermetallics and the L10 structure for the AuCu and PtM intermetallics. We consider three models for low temperature ordering in the phase diagrams of Au–Cu and Pt–M nanocluster alloys. These models are valid for sizes ~ 5 nm and approach bulk values for sizes ~ 20 nm. We study the phase transition in nanoclusters with cubic, octahedral, and cuboctahedral shapes, covering the compositions of interest. These models are based on studying the melting temperatures in nanoclusters using the regular solution, mixing model for alloys. Experimentally, it is extremely challenging to determine thermodynamic data on nano–sized alloys. Reasonable agreement is found between these models and recent experimental data on nanometer clusters in the Au–Cu and Pt–M nanophase systems. From our data, experiments on nanocubes about 5 nm in size, of stoichiometric AuCu and PtM composition, could help differentiate between the models. Some available evidence indicates that ordered intermetallic nanoclusters have better catalytic properties than disordered ones. We conclude with a discussion of physical mechanisms whereby ordering could improve the catalytic properties of nanocluster alloys.

Keywords: catalytic reactions, gold nanoalloys, phase transitions, platinum nanoalloys

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Authors: Maruf Yinka Kolawole, Jacob Olayiwola Aweda, Farasat Iqbal, Asif Ali, Sulaiman Abdulkareem

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Zinc is a non-ferrous metal with potential application in orthopaedic implant materials. However, its poor mechanical properties were major challenge to its application. Therefore, this paper studies the mechanical properties of biodegradable Zn-based alloy for biomedical application. Pure zinc powder with varying (0, 1, 2, 3 & 6) wt% of magnesium powders were ball milled using ball-to-powder ratio (B:P) of 10:1 at 350 rpm for 4 hours. The resulting milled powders were compacted and sintered at 300 MPa and 350 °C respectively. Microstructural, phase and mechanical properties analyses were performed following American standard of testing and measurement. The results show that magnesium has influence on the mechanical properties of zinc. The compressive strength, hardness and elastic modulus of 210 ± 8.878 MPa, 76 ± 5.707 HV and 45 ± 11.616 GPa respectively as obtained in Zn-2Mg alloy were optimum and meet the minimum requirement of biodegradable metal for orthopaedics application. These results indicate an increase of 111, 93 and 93% in compressive strength, hardness and elastic modulus respectively as compared to pure zinc. The increase in mechanical properties was adduced to effectiveness of compaction pressure and intermetallic phase formation within the matrix resulting in high dislocation density for improving strength. The study concluded that, Zn-2Mg alloy with optimum mechanical properties can therefore be considered a potential candidate for orthopaedic application.

Keywords: Biodegradable metal, Biomedical application, Mechanical properties, Powder Metallurgy, Zinc

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Authors: Sagar Pandit

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The present work focuses on the effect of various process parameters on the mechanical properties and microstructure of joints produced by continuous drive friction welding and linear friction welding. An attempt is made to investigate the feasibility of obtaining an acceptable weld joint between similar as well as dissimilar components and the microstructural changes have also been assessed once the good weld joints were considered (using Optical Microscopy and Scanning Electron Microscopy techniques). The impact of forging pressure in the microstructure of the weld joint has been studied and the variation in joint strength with varying forge pressure is analyzed. The weld joints were obtained two pair of dissimilar materials and one pair of similar materials, which are listed respectively as: Al-AA5083 & Cu-C101 (dissimilar), Aluminium alloy-3000 series & Mild Steel (dissimilar) and High Nitrogen Austenitic Stainless Steel pair (similar). Intermetallic phase formation was observed at the weld joints in the Al-Cu joint, which consequently harmed the properties of the joint (less tensile strength). It was also concluded that the increase in forging pressure led to both increment and decrement in the tensile strength of the joint depending on the similarity or dissimilarity of the components. The hardness was also observed to possess maximum as well as minimum values at the weld joint depending on the similarity or dissimilarity of workpieces. It was also suggested that a higher forging pressure is needed to obtain complete joining for the formation of the weld joint.

Keywords: forging pressure, friction welding, mechanical properties, microstructure

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Authors: Emrah Yaliniz, Ali Kalkanli

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ZE41A magnesium alloy has been extensively used in aerospace industry, especially for use in rotorcraft transmission casings. Due to the improved mechanical properties, the latest generation of magnesium casting alloy EV31A-T6 (Elektron 21® specified in AMS 4429) is seen as a potential replacement for ZE41A in terms of strength. Therefore, the necessity of enhancement has been arisen for ZE41A in order to avoid fully replacement. The main element affecting the strength of ZE41A is Zirconium (Zr), which acts as a grain refiner. The specified range of Zr element for ZE41A alloy is between 0.4 wt % and 1.0 wt % (unless otherwise stated by weight percentage after this point) as stated in AMS 4439. This paper investigates the effects of Zr amount on tensile and metallurgical properties of ZE41A magnesium alloy. The Zr alloying amount for the research has been chosen as 0.5 % and 1 %, which are standard amounts in a commercial alloy (average of 0.4-0.6%) and maximum percent in the standard, separately. 1 % Zr amount has been achieved via Zirmax (66.7 Mg-33.3 Zr) master alloy addition. The ultimate tensile strength of ZE41A with 1% Zr has been increased up to about 220-225 MPa in comparison to 200 MPa given in AMS 4439. The reason for the increase in strength with the addition of Zirmax is based on the decrease in grain size, which was measured about 30 µm. Optical microscope, scanning electron microscopy (SEM) and X-ray Diffraction (XRD) were used to detect the change in the microstructural futures via alloying. The zirconium rich coring at the center of the grains was observed in addition to the grain boundary intermetallic phases and bulk Mg-rich matrix. The solidification characteristics were also identified by using the cooling curve obtained from the sand casting mold during cooling of the alloys.

Keywords: aerospace, grain refinement, magnesium, sand casting, ZE41A

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Authors: Saumya R. Jha, Krishanu Biswas, Nilesh P. Gurao

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Several recent investigations have revealed medium entropy alloys exhibiting better mechanical properties than their high entropy counterparts. This clearly establishes that although a higher entropy plays a vital role in stabilization of particular phase over complex intermetallic phases, configurational entropy is not the primary factor responsible for the high inherent strengthening in these systems. Above and beyond a high contribution from friction stresses and solid solution strengthening, strain hardening is an important contributor to the strengthening in these systems. In this regard, researchers have developed severe plastic deformation (SPD) techniques like High Pressure Torsion (HPT) to incorporate very high shear strain in the material, thereby leading to ultrafine grained (UFG) microstructures, which cause manifold increase in the strength. The presented work demonstrates a meticulous study of the variation in mechanical properties at different radial displacements from the center of HPT tested equiatomic ternary FeMnNi synthesized by casting route, which is a low stacking fault energy FCC alloy that shows significantly higher toughness than its high entropy counterparts like Cantor alloy. The gradient in grain sizes along the radial direction of these specimens has been modeled using microstructure entropy for predicting the mechanical properties, which has also been validated by indentation tests. The dislocation density is computed by FEM simulations for varying strains and validated by analyzing synchrotron diffraction data. Thus, the proposed model can be utilized to predict the strengthening behavior of similar systems deformed by HPT subjected to varying loading conditions.

Keywords: high pressure torsion, severe plastic deformation, configurational entropy, dislocation density, FEM simulation

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Authors: Andras Dezső, Peter Baumli, George Kaptay

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The phosphorous is the important components in the steels, because it makes the changing of the mechanical properties and possibly modifying the structure. The phosphorous can be create the Fe3P compounds, what is segregated in the ferrite grain boundary in the intervals of the nano-, or microscale. This intermetallic compound is decreasing the mechanical properties, for example it makes the blue brittleness which means that the brittle created by the segregated particles at 200 ... 300°C. This work describes the phosphide solubility by the other components effect. We make calculations for the Ni, Mo, Cu, S, V, C, Si, Mn, and the Cr elements by the Thermo-Calc software. We predict the effects by approximate functions. The binary Fe-P system has a solubility line, which has a determinating equation. The result is below: lnwo = -3,439 – 1.903/T where the w0 means the weight percent of the maximum soluted concentration of the phosphorous, and the T is the temperature in Kelvin. The equation show that the P more soluble element when the temperature increasing. The nickel, molybdenum, vanadium, silicon, manganese, and the chromium make dependence to the maximum soluted concentration. These functions are more dependent by the elements concentration, which are lower when we put these elements in our steels. The copper, sulphur and carbon do not make effect to the phosphorous solubility. We predict that all of cases the maximum solubility concentration increases when the temperature more and more high. Between 473K and 673 K, in the phase diagram, these systems contain mostly two or three phase eutectoid, and the singe phase, ferritic intervals. In the eutectoid areas the ferrite, the iron-phosphide, and the metal (III)-phospide are in the equilibrium. In these modelling we predicted that which elements are good for avoid the phosphide segregation or not. These datas are important when we make or choose the steels, where the phosphide segregation stopping our possibilities.

Keywords: phosphorous, steel, segregation, thermo-calc software

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Authors: Matthew Ferguson, Tatyana Konkova, Ioannis Violatos

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Microstructure analysis of additively manufactured (AM) materials is an important step in understanding the interrelationship between mechanical properties and materials performance. Literature on the effect of laser-based AM process parameters on the microstructure in the substrate-deposit interface is limited. The interface region, the adjoining area of substrate and deposit, is characterized by the presence of the fusion zone (FZ) and heat-affected zone (HAZ), experiencing rapid thermal gyrations resulting in thermal-induced transformations. Inconel 718 was utilized as work material for both the substrate and deposit. Three blocks of Inconel 718 material were deposited by Direct Energy Deposition (DED) using three different laser powers, 550W, 750W and 950W, respectively. A coupled thermo-mechanical transient approach was utilized to correlate temperature history to the evolution of microstructure. The thermal history of the deposition process was monitored with the thermocouples installed inside the substrate material. The interface region of the blocks was analyzed with Optical Microscopy (OM) and Scanning Electron Microscopy (SEM), including the electron back-scattered diffraction (EBSD) technique. Laser power was found to influence the dissolution of intermetallic precipitated phases in the substrate and grain growth in the interface region. Microstructure and thermal history data were utilized to draw conclusive comparisons between the investigated process parameters.

Keywords: additive manufacturing, direct energy deposition, electron back-scattered diffraction, finite element analysis, inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region

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Authors: Vaibhav Pandey, K. Chattopadhyay, N. C. Santhi Srinivas, Vakil Singh

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Aluminium alloy 7075 consist of different intermetallic precipitate particles MgZn2, CuAl2, which result in heterogeneity of micro structure and influence the corrosion properties of the alloy. Artificial ageing was found to enhance the strength properties, but highly susceptible to stress-corrosion cracking. Various conventional surface modification techniques are developed for improving corrosion properties of aluminum alloys. This led to development of novel surface mechanical attrition treatment (SMAT) technique the so called ultrasonic shot peening which gives nano-grain structure at surface. In the present investigation the influence of surface mechanical attrition treatment on corrosion behavior of aluminum alloy 7075 was studied in 3.5wt% NaCl solution. Two different size of 1 mm and 3 mm steel balls are used as peening media and SMAT was carried out for different time intervals 5, 15 and 30 minutes. Surface nano-grains/nano-crystallization was observed after SMAT. The formation of nano-grain structure was observed for larger size balls with time of treatment and consequent increase in micro strain. As-SMATed sample with 1 mm balls exhibits better corrosion resistance as compared to that of un-SMATed sample. The enhancement in corrosion resistance may be due to formation of surface nano-grain structure which reduced the electron release rate. In contrast the samples treated with 3 mm balls showed very poor corrosion resistance. A decrease in corrosion resistance was observed with increase in the time of peening. The decrease in corrosion resistance in the shotpeened samples with larger diameter balls may due to increase in microstrain and defect density.

Keywords: aluminum alloy 7075, corrosion, SMAT, ultrasonic shot peening, surface nano-grains

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Authors: Saeedeh Imani Moqadam, Ilya Bobrov, Jérémy Epp, Nils Ellendt, Lutz Mädler

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High entropy alloys (HEAs), having adjustable properties and enhanced stability compared with intermetallic compounds, are solid solution alloys that contain more than five principal elements with almost equal atomic percentage. The concept of producing such alloys pave the way for developing advanced materials with unique properties. However, the synthesis of such alloys may require advanced processes with high cooling rates depending on which alloy elements are used. In this study, the micro spheres of different diameters of HEAs were generated via a drop-on-demand droplet generator and subsequently solidified during free-fall in an argon atmosphere. Such droplet generators can generate individual droplets with high reproducibility regarding droplet diameter, trajectory and cooling while avoiding any interparticle momentum or thermal coupling. Metallography as well as X-ray diffraction investigations for each diameter of the generated metallic droplets where then carried out to obtain information about the microstructural state. To calculate the cooling rate of the droplets, a droplet cooling model was developed and validated using model alloys such as CuSn%6 and AlCu%4.5 for which a correlation of secondary dendrite arm spacing (SDAS) and cooling rate is well-known. Droplets were generated from these alloys and their SDAS was determined using quantitative metallography. The cooling rate was then determined from the SDAS and used to validate the cooling rates obtained from the droplet cooling model. The application of that model on the HEA then leads to the cooling rate dependency and hence to the identification of process windows for the synthesis of these alloys. These process windows were then compared with cooling rates obtained in processes such as powder production, spray forming, selective laser melting and casting to predict if a synthesis is possible with these processes.

Keywords: cooling rate, drop-on-demand, high entropy alloys, microstructure, single droplet generation, X-ray Diffractometry

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Authors: Varun A Baheti, Sanjay Kashyap, Kamanio Chattopadhyay, Praveen Kumar, Aloke Paul

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Ni–Sn system finds applications in the microelectronics industry, especially with respect to flip–chip or direct chip, attach technology. Here the region of interest is under bump metallization (UBM), and solder bump (Sn) interface due to the formation of brittle intermetallic phases there. Understanding the growth of these phases at UBM/Sn interface is important, as in many cases it controls the electro–mechanical properties of the product. Cu and Ni are the commonly used UBM materials. Cu is used for good bonding because of fast reaction with solder and Ni often acts as a diffusion barrier layer due to its inherently slower reaction kinetics with Sn–based solders. Investigation on the growth kinetics of phases in Ni–Sn system is reported in this study. Just for simplicity, Sn being major solder constituent is chosen. Ni–Sn electroplated diffusion couples are prepared by electroplating pure Sn on Ni substrate. Bulk diffusion couples prepared by the conventional method are also studied along with Ni–Sn electroplated diffusion couples. Diffusion couples are annealed for 25–1000 h at 50–215°C to study the phase evolutions and growth kinetics of various phases. The interdiffusion zone was analysed using field emission gun equipped scanning electron microscope (FE–SEM) for imaging. Indexing of selected area diffraction (SAD) patterns obtained from transmission electron microscope (TEM) and composition measurements done in electron probe micro−analyser (FE–EPMA) confirms the presence of various product phases grown across the interdiffusion zone. Time-dependent experiments indicate diffusion controlled growth of the product phase. The estimated activation energy in the temperature range 125–215°C for parabolic growth constants (and hence integrated interdiffusion coefficients) of the Ni₃Sn₄ phase shed light on the growth mechanism of the phase; whether its grain boundary controlled or lattice controlled diffusion. The location of the Kirkendall marker plane indicates that the Ni₃Sn₄ phase grows mainly by diffusion of Sn in the binary Ni–Sn system.

Keywords: diffusion, equilibrium phase, metastable phase, the Ni-Sn system

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Authors: L. Vivet, L. Benabou, O. Simon

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With highly demanding applications in the field of power electronics, there is an increasing need to have interconnection materials with properties that can ensure both good mechanical assembly and high thermal/electrical conductivities. So far, lead-free solders have been considered an attractive solution, but recently, sintered joints based on nano-silver paste have been used for die attach and have proved to be a promising solution offering increased performances in high-temperature applications. In this work, the main parameters of the bonding process using silver oxalates are studied, i.e., the heating rate and the bonding pressure mainly. Their effects on both the mechanical and thermal properties of the sintered layer are evaluated following an experimental design. Pairs of copper substrates with gold metallization are assembled through the sintering process to realize the samples that are tested using a micro-traction machine. In addition, the obtained joints are examined through microscopy to identify the important microstructural features in relation to the measured properties. The formation of an intermetallic compound at the junction between the sintered silver layer and the gold metallization deposited on copper is also analyzed. Microscopy analysis exhibits a nanoporous structure of the sintered material. It is found that higher temperature and bonding pressure result in higher densification of the sintered material, with higher thermal conductivity of the joint but less mechanical flexibility to accommodate the thermo-mechanical stresses arising during service. The experimental design allows hence the determination of the optimal process parameters to reach sufficient thermal/mechanical properties for a given application. It is also found that the interphase formed between silver and gold metallization is the location where the fracture occurred after the mechanical testing, suggesting that the inter-diffusion mechanism between the different elements of the assembly leads to the formation of a relatively brittle compound.

Keywords: nanoporous structure, silver oxalate, sintering, mechanical strength, thermal conductivity, microelectronic packaging

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Authors: Anatoly A. Kuznetsov, Pavel G. Berezhko, Sergey M. Kunavin, Eugeny V. Zhilkin, Maxim V. Tsarev, Vyacheslav V. Yaroshenko, Valery V. Mokrushin, Olga Y. Yunchina, Sergey A. Mityashin

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The acoustic emission is caused by short-time propagation of elastic waves that are generated as a result of quick energy release from sources localized inside some material. In particular, the acoustic emission phenomenon lies in the generation of acoustic waves resulted from the reconstruction of material internal structures. This phenomenon is observed at various physicochemical transformations, in particular, at those accompanying hydrogenation processes of metals or intermetallic compounds that make it possible to study parameters of these transformations through recording and analyzing the acoustic signals. It has been known that at the interaction between metals or inter metallides with hydrogen the most intensive acoustic signals are generated as a result of cracking or crumbling of an initial compact powder sample as a result of the change of material crystal structure under hydrogenation. This work is dedicated to the study into changes occurring in metallic titanium samples at their interaction with hydrogen and followed by acoustic emission signals. In this work the subjects for investigation were specimens of metallic titanium in two various initial forms: titanium sponge and fine titanium powder made of this sponge. The kinetic of the interaction of these materials with hydrogen, the acoustic emission signals accompanying hydrogenation processes and the structure of the materials before and after hydrogenation were investigated. It was determined that in both cases interaction of metallic titanium and hydrogen is followed by acoustic emission signals of high amplitude generated on reaching some certain value of the atomic ratio [H]/[Ti] in a solid phase because of metal cracking at a macrolevel. The typical sizes of the cracks are comparable with particle sizes of hydrogenated specimens. The reasons for cracking are internal stresses initiated in a sample due to the increasing volume of a solid phase as a result of changes in a material crystal lattice under hydrogenation. When the titanium powder is used, the atomic ratio [H]/[Ti] in a solid phase corresponding to the maximum amplitude of an acoustic emission signal are, as a rule, higher than when titanium sponge is used.

Keywords: acoustic emission signal, cracking, hydrogenation, titanium specimen

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Authors: Olawale S. Fatoba, Stephen A. Akinlabi, Esther T. Akinlabi, Rezvan Gharehbaghi

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The performance of material surface under wear and corrosion environments cannot be fulfilled by the conventional surface modifications and coatings. Therefore, different industrial sectors need an alternative technique for enhanced surface properties. Titanium and its alloys possess poor tribological properties which limit their use in certain industries. This paper focuses on the effect of hybrid coatings Al-Cu-Fe on a grade five titanium alloy using laser metal deposition (LMD) process. Icosahedral Al-Cu-Fe as quasicrystals is a relatively new class of materials which exhibit unusual atomic structure and useful physical and chemical properties. A 3kW continuous wave ytterbium laser system (YLS) attached to a KUKA robot which controls the movement of the cladding process was utilized for the fabrication of the coatings. The titanium cladded surfaces were investigated for its hardness, corrosion and tribological behaviour at different laser processing conditions. The samples were cut to corrosion coupons, and immersed into 3.65% NaCl solution at 28oC using Electrochemical Impedance Spectroscopy (EIS) and Linear Polarization (LP) techniques. The cross-sectional view of the samples was analysed. It was found that the geometrical properties of the deposits such as width, height and the Heat Affected Zone (HAZ) of each sample remarkably increased with increasing laser power due to the laser-material interaction. It was observed that there are higher number of aluminum and titanium presented in the formation of the composite. The indentation testing reveals that for both scanning speed of 0.8 m/min and 1m/min, the mean hardness value decreases with increasing laser power. The low coefficient of friction, excellent wear resistance and high microhardness were attributed to the formation of hard intermetallic compounds (TiCu, Ti2Cu, Ti3Al, Al3Ti) produced through the in situ metallurgical reactions during the LMD process. The load-bearing capability of the substrate was improved due to the excellent wear resistance of the coatings. The cladded layer showed a uniform crack free surface due to optimized laser process parameters which led to the refinement of the coatings.

Keywords: Al-Cu-Fe coating, corrosion, intermetallics, laser metal deposition, Ti-6Al-4V alloy, wear resistance

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Authors: Zbigniew Szklarz, Aldona Garbacz-Klempka, Magdalena Bisztyga-Szklarz

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Typical metallic alloys bases on one major alloying component, where the addition of other elements is intended to improve or modify certain properties, most of all the mechanical properties. However, in 1995 a new concept of metallic alloys was described and defined. High Entropy Alloys (HEA) contains at least five alloying elements in an amount from 5 to 20 at.%. A common feature this type of alloys is an absence of intermetallic phases, high homogeneity of the microstructure and unique chemical composition, what leads to obtaining materials with very high strength indicators, stable structures (also at high temperatures) and excellent corrosion resistance. Hence, HEA can be successfully used as a substitutes for typical metallic alloys in various applications where a sufficiently high properties are desirable. For fabricating HEA, a few ways are applied: 1/ from liquid phase i.e. casting (usually arc melting); 2/ from solid phase i.e. powder metallurgy (sintering methods preceded by mechanical synthesis) and 3/ from gas phase e.g. sputtering or 4/ other deposition methods like electrodeposition from liquids. Application of different production methods creates different microstructures of HEA, which can entail differences in their properties. The last two methods also allows to obtain coatings with HEA structures, hereinafter referred to as High Entropy Films (HEF). With reference to above, the crucial aim of this work was the optimization of the manufacturing process of the multi-component metallic layers (HEF) by the low- and high temperature electrochemical deposition ( ED). The low-temperature deposition process was crried out at ambient or elevated temperature (up to 100 ᵒC) in organic electrolyte. The high-temperature electrodeposition (several hundred Celcius degrees), in turn, allowed to form the HEF layer by electrochemical reduction of metals from molten salts. The basic chemical composition of the coatings was CoCrFeMnNi (known as Cantor’s alloy). However, it was modified by other, selected elements like Al or Cu. The optimization of the parameters that allow to obtain as far as it possible homogeneous and equimolar composition of HEF is the main result of presented studies. In order to analyse and compare the microstructure, SEM/EBSD, TEM and XRD techniques were employed. Morover, the determination of corrosion resistance of the CoCrFeMnNi(Cu or Al) layers in selected electrolytes (i.e. organic and non-organic liquids) was no less important than the above mentioned objectives.

Keywords: high entropy alloys, electrodeposition, corrosion behavior, microstructure

Procedia PDF Downloads 53

Authors: Kirill M. Dubovikov, Ekaterina S. Marchenko, Gulsharat A. Baigonakova

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NiTi alloys are widely used as implants in medicine due to their unique properties such as superelasticity, shape memory effect and biocompatibility. However, despite these properties, one of the major problems is the release of nickel after prolonged use in the human body under dynamic stress. This occurs due to oxidation and cracking of NiTi implants, which provokes nickel segregation from the matrix to the surface and release into living tissues. As we know, nickel is a toxic element and can cause cancer, allergies, etc. One of the most popular ways to solve this problem is to create a corrosion resistant coating on NiTi. There are many coatings of this type, but not all of them have good biocompatibility, which is very important for medical implants. Coatings based on calcium phosphate phases have excellent biocompatibility because Ca and P are the main constituents of the mineral part of human bone. This fact suggests that a Ca-P coating on NiTi can enhance osteogenesis and accelerate the healing process. Therefore, the aim of this study is to investigate the structure of Ca-P coating on NiTi substrate. Plasma assisted radio frequency (RF) sputtering was used to obtain this film. This method was chosen because it allows the crystallinity and morphology of the Ca-P coating to be controlled by the sputtering parameters. It allows us to obtain three different NiTi samples with Ca-P coating. XRD, AFM, SEM and EDS were used to study the composition, structure and morphology of the coating phase. Scratch tests were carried out to evaluate the adhesion of the coating to the substrate. Wettability tests were used to investigate the hydrophilicity of the different coatings and to suggest which of them had better biocompatibility. XRD showed that the coatings of all samples were hydroxyapatite, but the matrix was represented by TiNi intermetallic compounds such as B2, Ti2Ni and Ni3Ti. The SEM shows that the densest and defect-free coating has only one sample after three hours of sputtering. Wettability tests show that the sample with the densest coating has the lowest contact angle of 40.2° and the largest free surface area of 57.17 mJ/m2, which is mostly disperse. A scratch test was carried out to investigate the adhesion of the coating to the surface and it was shown that all coatings were removed by a cohesive mechanism. However, at a load of 30N, the indenter reached the substrate in two out of three samples, except for the sample with the densest coating. It was concluded that the most promising sputtering mode was the third, which consisted of three hours of deposition. This mode produced a defect-free Ca-P coating with good wettability and adhesion.

Keywords: biocompatibility, calcium phosphate coating, NiTi alloy, radio frequency sputtering.

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Authors: Siri Marthe Arbo, Afaf Saai, Sture Sørli, Mette Nedreberg

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This work aims to establish a reliable approach for optimizing a Laser Metal Deposition (LMD) process for a critical maritime component, based on the material properties and structural performance required by the maritime industry. The component of interest is a water jet impeller, for which specific requirements for material properties are defined. The developed approach is based on the assessment of the effects of LMD process parameters on microstructure and material performance of standard AM 2205 duplex stainless steel powder. Duplex stainless steel offers attractive properties for maritime applications, combining high strength, enhanced ductility and excellent corrosion resistance due to the specific amounts of ferrite and austenite. These properties are strongly affected by the microstructural characteristics in addition to microstructural defects such as porosity and welding defects, all strongly influenced by the chosen LMD process parameters. In this study, the influence of deposition speed and heat input was evaluated. First, the influences of deposition speed and heat input on the microstructure characteristics, including ferrite/austenite fraction, amount of porosity and welding defects, were evaluated. Then, the achieved mechanical properties were evaluated by standard testing methods, measuring the hardness, tensile strength and elongation, bending force and impact energy. The measured properties were compared to the requirements of the water jet impeller. The results show that the required amounts of ferrite and austenite can be achieved directly by the LMD process without post-weld heat treatments. No intermetallic phases were observed in the material produced by the investigated process parameters. A high deposition speed was found to reduce the ductility due to the formation of welding defects. An increased heat input was associated with reduced strength due to the coarsening of the ferrite/austenite microstructure. The microstructure characterizations and measured mechanical performance demonstrate the great potential of the LMD process and generate a valuable database for the optimization of the LMD process for duplex stainless steels.

Keywords: duplex stainless steel, laser metal deposition, process optimization, microstructure, mechanical properties

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Authors: H. M. Nanjundaswamy, S. K. Nath, S. Ray

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TiO₂ particles have been added in molten aluminium to result in aluminium based cast Al/Al₃Ti-Al₂O₃ composite, which has been added then to molten magnesium to synthesize magnesium based cast Mg-Al/Al₃Ti-Al₂O₃ composite. The nominal compositions in terms of Mg, Al, and TiO₂ contents in the magnesium based composites are Mg-9Al-0.6TiO₂, Mg-9Al-0.8TiO₂, Mg-9Al-1.0TiO₂ and Mg-9Al-1.2TiO₂ designated respectively as MA6T, MA8T, MA10T and MA12T. The microstructure of the cast magnesium based composite shows grayish rods of intermetallics Al₃Ti, inherited from aluminium based composite but these rods, on hot forging, breaks into smaller lengths decreasing the average aspect ratio (length to diameter) from 7.5 to 3.0. There are also cavities in between the broken segments of rods. β-phase in cast microstructure, Mg₁₇Al₁₂, dissolves during heating prior to forging and re-precipitates as relatively finer particles on cooling. The amount of β-phase also decreases on forging as segregation is removed. In both the cast and forged composite, the Brinell hardness increases rapidly with increasing addition of TiO₂ but the hardness is higher in forged composites by about 80 BHN. With addition of higher level of TiO₂ in magnesium based cast composite, yield strength decreases progressively but there is marginal increase in yield strength over that of the cast Mg-9 wt. pct. Al, designated as MA alloy. But the ultimate tensile strength (UTS) in the cast composites decreases with the increasing particle content indicating possibly an early initiation of crack in the brittle inter-dendritic region and their easy propagation through the interfaces of the particles. In forged composites, there is a significant improvement in both yield strength and UTS with increasing TiO₂ addition and also, over those observed in their cast counterpart, but at higher addition it decreases. It may also be noted that as in forged MA alloy, incomplete recovery of forging strain increases the strength of the matrix in the composites and the ductility decreases both in the forged alloy and the composites. Initiation fracture toughness, J_IC, decreases drastically in cast composites compared to that in MA alloy due to the presence of intermetallic Al₃Ti and Al₂O₃ particles in the composite. There is drastic reduction of J_IC on forging both in the alloy and the composites, possibly due to incomplete recovery of forging strain in both as well as breaking of Al₃Ti rods and the voids between the broken segments of Al₃Ti rods in composites. The ratio of tearing modulus to elastic modulus in cast composites show higher ratio, which increases with the increasing TiO₂ addition. The ratio decreases comparatively more on forging of cast MA alloy than those in forged composites.

Keywords: composite, fracture toughness, forging, tensile properties

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Authors: Bharatkumar Doshi

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Electro-Magnetic Pulse Welding (EMPW) is a solid state welding process carried out at almost room temperature, in which joining is enabled by high impact velocity deformation. In this process, high voltage capacitor’s stored energy is discharged in an EM coil resulting in a damped, sinusoidal current with an amplitude of several hundred kiloamperes. Due to these transient magnetic fields of few tens of Tesla near the coil is generated. As the conductive (tube) part is positioned in this area, an opposing eddy current is induced in this part. Consequently, high Lorentz forces act on the part, leading to acceleration away from the coil. In case of a tube, it gets compressed under forming velocities of more than 300 meters per second. After passing the joining gap it collides with the second metallic joining rod, leading to the formation of a jet under appropriate collision conditions. Due to the prevailing high pressure, metallurgical bonding takes place. A characteristic feature is the wavy interface resulting from the heavy plastic deformations. In the process, the formation of intermetallic compounds which might deteriorate the weld strength can be avoided, even for metals with dissimilar thermal properties. In order to optimize the process parameters like current, voltage, inductance, coil dimensions, workpiece dimensions, air gap, impact velocity, effective plastic strain, shear stress acting in the welding zone/impact zone etc. are very critical and important to establish. These process parameters could be determined by simulation using Finite Element Methods (FEM) in which electromagnetic –structural couple field analysis is performed. The feasibility of welding could thus be investigated by varying the parameters in the simulation using COMSOL. Simulation results shall be applied in performing the preliminary experiments of welding the different alloy steel tubes and/or alloy steel to other materials. The single turn coil (S.S.304) with field shaper (copper) has been designed and manufactured. The preliminary experiments are performed using existing EMPW facility available Institute for Plasma Research, Gandhinagar, India. The experiments are performed at 22kV charged into 64µF capacitor bank and the energy is discharged into single turn EM coil. Welding of axi-symetric components such as aluminum tube and rod has been proven experimentally using EMPW techniques. In this paper EM coil design, manufacturing, Electromagnetic-structural FEM simulation of Magnetic Pulse Welding and preliminary experiment results is reported.

Keywords: COMSOL, EMPW, FEM, Lorentz force

Procedia PDF Downloads 154

Authors: Elvis Medina, Alejandro Karelovic, Romel Jiménez

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Catalytic ammonia decomposition represents an attractive alternative due to its high H₂ content (17.8% w/w), a product stream free of COₓ, among others; however, challenges need to be addressed for its consolidation as an H₂ chemical storage technology, especially, those focused on the synthesis of efficient bimetallic catalytic systems, as an alternative to the price and scarcity of ruthenium, the most active catalyst reported. In this sense, from the perspective of rational catalyst design, adjusting the main catalytic activity descriptor, a screening of supported catalysts with different compositional settings of cobalt-molybdenum metals is presented to evaluate their effect on the catalytic decomposition rate of ammonia. Subsequently, a kinetic study on the supported monometallic Co and Mo catalysts, as well as on the bimetallic CoMo catalyst with the highest activity is shown. The synthesis of catalysts supported on γ-alumina was carried out using the Charge Enhanced Dry Impregnation (CEDI) method, all with a 5% w/w loading metal. Seeking to maintain uniform dispersion, the catalysts were oxidized and activated (In-situ activation) using a flow of anhydrous air and hydrogen, respectively, under the same conditions: 40 ml min⁻¹ and 5 °C min⁻¹ from room temperature to 600 °C. Catalytic tests were carried out in a fixed-bed reactor, confirming the absence of transport limitations, as well as an Approach to equilibrium (< 1 x 10⁻⁴). The reaction rate on all catalysts was measured between 400 and 500 ºC at 53.09 kPa NH3. The synergy theoretically (DFT) reported for bimetallic catalysts was confirmed experimentally. Specifically, it was observed that the catalyst composed mainly of 75 mol% cobalt proved to be the most active in the experiments, followed by the monometallic cobalt and molybdenum catalysts, in this order of activity as referred to in the literature. A kinetic study was performed at 10.13 – 101.32 kPa NH3 and at four equidistant temperatures between 437 and 475 °C the data were adjusted to an LHHW-type model, which considered the desorption of nitrogen atoms from the active phase surface as the rate determining step (RDS). The regression analysis were carried out under an integral regime, using a minimization algorithm based on SLSQP. The physical meaning of the parameters adjusted in the kinetic model, such as the RDS rate constant (k₅) and the lumped adsorption constant of the quasi-equilibrated steps (α) was confirmed through their Arrhenius and Van't Hoff-type behavior (R² > 0.98), respectively. From an energetic perspective, the activation energy for cobalt, cobalt-molybdenum, and molybdenum was 115.2, 106.8, and 177.5 kJ mol⁻¹, respectively. With this evidence and considering the volcano shape described by the ammonia decomposition rate in relation to the metal composition ratio, the synergistic behavior of the system is clearly observed. However, since characterizations by XRD and TEM were inconclusive, the formation of intermetallic compounds should be still verified using HRTEM-EDS. From this point onwards, our objective is to incorporate parameters into the kinetic expressions that consider both compositional and structural elements and explore how these can maximize or influence H₂ production.

Keywords: CEDI, hydrogen carrier, LHHW, RDS

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Authors: A. V. Samokhin, A. A. Fadeev, M. A. Sinaiskii, N. V. Alekseev, A. V. Kolesnikov

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Composite materials where metal matrix is reinforced by ceramic or metal particles are of great interest for use in the manufacturing of electrical contacts. Significant improvement of the composite physical and mechanical properties as well as increase of the performance parameters of composite-based products can be achieved if the nanoscale structure in the composite materials is obtained by using nanosized powders as starting components. The results of nanosized composite powders synthesis (Ag-SnO2, W-Cu and Cu-C) in the DC thermal plasma flows are presented in this paper. The investigations included the following processes: - Recondensation of micron powder mixture Ag + SnO2 in a nitrogen plasma; - The reduction of the oxide powders mixture (WO3 + CuO) in a hydrogen-nitrogen plasma; - Decomposition of the copper formate and copper acetate powders in nitrogen plasma. The calculations of equilibrium compositions of multicomponent systems Ag-Sn-O-N, W-Cu-O-H-N and Cu-O-C-H-N in the temperature range of 400-5000 K were carried to estimate basic process characteristics. Experimental studies of the processes were performed using a plasma reactor with a confined jet flow. The plasma jet net power was in the range of 2 - 13 kW, and the feedstock flow rate was up to 0.35 kg/h. The obtained powders were characterized by TEM, HR-TEM, SEM, EDS, ED-XRF, XRD, BET and QEA methods. Nanocomposite Ag-SnO2 (12 wt. %). Processing of the initial powder mixture (Ag-SnO2) in nitrogen thermal plasma stream allowed to produce nanopowders with a specific surface area up to 24 m2/g, consisting predominantly of particles with size less than 100 nm. According to XRD results, tin was present in the obtained products as SnO2 phase, and also as intermetallic phases AgxSn. Nanocomposite W-Cu (20 wt .%). Reduction of (WO3+CuO) mixture in the hydrogen-nitrogen plasma provides W-Cu nanopowder with particle sizes in the range of 10-150 nm. The particles have mainly spherical shape and structure tungsten core - copper shell. The thickness of the shell is about several nanometers, the shell is composed of copper and its oxides (Cu2O, CuO). The nanopowders had 1.5 wt. % oxygen impurity. Heat treatment in a hydrogen atmosphere allows to reduce the oxygen content to less than 0.1 wt. %. Nanocomposite Cu-C. Copper nanopowders were found as products of the starting copper compounds decomposition. The nanopowders primarily had a spherical shape with a particle size of less than 100 nm. The main phase was copper, with small amount of Cu2O and CuO oxides. Copper formate decomposition products had a specific surface area 2.5-7 m2/g and contained 0.15 - 4 wt. % carbon; and copper acetate decomposition products had the specific surface area 5-35 m2/g, and carbon content of 0.3 - 5 wt. %. Compacting of nanocomposites (sintering in hydrogen for Ag-SnO2 and electric spark sintering (SPS) for W-Cu) showed that the samples having a relative density of 97-98 % can be obtained with a submicron structure. The studies indicate the possibility of using high-intensity plasma processes to create new technologies to produce nanocomposite materials for electric contacts.

Keywords: electrical contact, material, nanocomposite, plasma, synthesis

Procedia PDF Downloads 214