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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Use of Refractory-Volatile Element Deep Eutectic Regions to Grow Single Crystalline Intermetallic Compounds

Compounds containing both refractory and volatile elements present a unique challenge for crystal growth, given the conflicting realities of high melting temperatures and high vapor pressures. Nevertheless, the discovery of superconductivity in FeAs and FeSe based materials and a Weyl semimetal state in TaP are motivations to explore compounds containing such pairs. Here, we discuss use of the low-melting single phase liquid regions above deep M-X eutectics (M=transition metal, X=P, S) as the basis for high temperature solutions for growing intermetallic compounds containing volatile-refractory pairs. We show that Ni-P, Pd-P, Pt-P, and Pd-S compositions form single phase melts at moderate temperatures below 1000 °C and with minimal vapor pressure. We first present the simple case of growing Ni 2 P from Ni-P and next discuss the more complicated growth of RPd 3 S 4 (R=La, Ce, Nd, Eu) from a Pd-S melt. We show how frit-disc alumina crucible sets allow for contamination-free capture of decanted liquid and its reuse in subsequent experiments, demonstrating a fractionation of the CePd 3 S 4 growth to determine the optimal conditions for crystal growth. We conclude by using the single phase liquid regions above the Pt-P and Pd-P eutectics to grow single crystals of MPt 5 P (M=Mn, Fe) and MnPd 5 P. As these materials have primarily been studied in polycrystalline form, we give an overview of the magnetic and transport properties of our single crystals. The examples outlined here illustrate the utility of using the single phase liquid above deep metal-X eutectics for solution growth and materials discovery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Microstructure-based prediction of thermal aging strength reduction factors for grade 91 ferritic-martensitic steel

This study aimed to develop a microstructure-based mechanistic approach to address the long-term thermal aging effect on yield stress and ultimate tensile strength and to provide a physical basis for developing thermal aging factors for G91 for a design life of 60 years. Several heats of G91 steel were examined. Controlled aging experiments were conducted on two heats at temperatures of 550, 600, and 650 °C for times up to ~64,000 h. Specimens were also taken from archived creep-tested specimens of G91 and from a tube removed from the Kingston coal-fired power plant to obtain data that cover a wide range of temperatures and for aging times up to 155,000 h. Thermal aging caused significant subgrain recovery, coarsening of M 23 C 6 carbides at subgrain boundaries and MX carbonitrides within subgrains. The intermetallic Laves phase forms during aging and grows rapidly. The growth rate of the subgrain width and MX mean size during thermal aging were described by kinetic models. Thermal aging results in the reductions in the yield stress and the ultimate tensile strength of G91. The effects of thermal aging on the reductions in yield stress and ultimate tensile strength were well described by the microstructure-strength model that considers three superimposed strengthening mechanisms, namely, sub-boundary strengthening, MX precipitation hardening, and Mo solid solution strengthening. Furthermore, the model was independently validated by the ASME Code values and is being used by the ASME to develop the aging-induced strength reduction factors for G91 steel for a design life of 60 years.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Phase-Field Modeling of Materials Interfaces and Nanostructures

Nanostructured materials offer unique properties for a wide range of energy applications. Among various known processing methods, liquid metal dealloying (LMD)—the selective dissolution of a base alloy element into a metallic melt—has emerged as a powerful technique to produce a new class of nano-/meso-scale open porous and bicontinuous composite structures with ultra-high interfacial area. LMD has recently been complemented by the advent of vapor phase dealloying (VPD), a novel technique that exploits the selective evaporation of one element from a parent alloy containing elements with very different vapor pressures, thereby enabling to fabricate open nanoporous structures of various elements from less-noble metals to inorganic elements regardless of their chemical activity without requiring high LMD temperatures and chemical etching. Together LMD and VPD have greatly expanded the scope of dealloying techniques, limited by traditional electrochemical means to noble metals, and boosted the design of new functional and structural materials that combine a wide variety of elements. Topologically-connected open porous structures with ultra-high surface area allow mass transport within the structure while preserving structural integrity, enabling them to serve as catalysts, fuel cells, supercapacitors, or high-capacity battery materials. Bicontinuous composite structures in turn can display high strength and high ductility or superior radiation-damage resistance due to the ultra-high interface area between interpenetrating solid phases. This research program makes use of state-of-the-art computational methods to understand at a basic level the self-organizing dealloying process with main focus on dealloying kinetics and interfacial pattern formation at the dealloying front controlling initial structure size, topology, and phase compositions. Phase-field simulation studies of LMD focus on solid solutions, line compounds, and intermetallic systems that can form ternary composites by nucleation and growth of a new phase. Studies of VPD employ phase-field modeling and a hybrid method combining a kinetic Monte Carlo (KMC) model of evaporation and surface diffusion with molecular dynamics for vapor-phase transport inside nanopores. Simulations explore mechanisms of interface- and diffusion-controlled dealloying kinetics, both observed in VPD but not fundamentally understood. In addition, our newly developed multi-physics phase-field approach of large-volume-change phase transformations is being used to model novel 3D anode geometries based on dealloyed nanoporous structures including novel sandwiched graphene/Si/silica for highrate Li ion battery. Those studies are aimed at elucidating geometric design principles that improve mechanical stability. We expect this research to enhance the capability to tailor nano-/mesoscale structures for a wide range of energy-related materials applications and to yield further advances in computational methodologies that benefit a broad materials research community.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Structurally Frustrated Remeika Phases: Tolerance Factor and Non-Kramers’ Ion Effects

Quantum materials that are found on the verge of structural, magnetic, and electronic instabilities are deep reservoirs for exotic phenomena. Our criteria to study the reported Ln 5 Ru 6 Sn 18 (Ln = Gd, Tb) are guided by the tolerance factor for Remeika phases─a class of intermetallic compounds with the general formula A 3 M 4 X 13 (where A = rare-earth element, M = transition metal, and X = tetrel), which can be viewed as structural analogues of pseudoperovskites (4 × ABX 3 ), with one of the tetrel atoms occupying the A-site. We have grown single crystals, up to 0.5 cm on the largest facet, of Gd 5 Ru 6 Sn 18 (a = 13.8052(12) Å) and Tb 5 Ru 6 Sn 18 (a = 13.7825(9) Å), which we expect to be on the verge of a formation instability. Bulk magnetic, heat capacity, and electrical transport measurements reveal unusual behavior that originates from the trivalent Gd and Tb ions, with deviations from typical metallic behavior and magnetic ordering that is short-range or disrupted in some other way. Furthermore, to better understand these phenomena, single-crystal neutron diffraction is investigated, which reveals short-range correlations among the partially occupied Tb and Sn sublattices, with 3D-ΔPDF analysis supporting direction-dependent local order. Taken together, these measurements show the utility of using tolerance factors in identifying materials that are likely to exhibit complex phenomena and uncover environments where a formation instability may strongly impact emergent bulk magnetic and electronic phenomena.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Metallurgical alloy approach to two-dimensional supramolecular materials

Alloys are normally mixtures of metallic elements used to search for superior functional properties compared with their individual components. Although a quintessential approach to better materials in metallurgy, the concept of alloying has been expanded to other inorganic materials and covalent polymers. In this work, we report on alloy formation of small organic molecules structured as amphiphilic chromophores in water. Using X-ray scattering, microscopy, and optical spectroscopy, we unambiguously demonstrate the formation of supramolecular alloys with changes in physical, photophysical, and mechanical properties. Additionally, we identify single-crystalline, two-dimensional supramolecular polymers containing multiple molecular species, analogous to intermetallic compounds. The mechanism of alloy formation suggests the possibility of controlled growth in these supramolecular assemblies to create emergent functional structures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Understanding the Electronic Behavior of f-Element Intermetallics

Due to their partially filled f-orbitals, lanthanide and actinide intermetallic materials exhibit intriguing electronic, structural, and magnetic properties. These materials provide a unique platform to explore exotic magnetic and quantum phenomena that arise from their strongly correlated f-electrons, offering insights into f-electron behavior. Incorporating light elements such as boron and carbon can significantly impact the electronic, chemical, and physical properties of these materials, with varying influence between lanthanides and actinides due to the more localized f-electrons in lanthanides. In this work, lanthanide-based intermetallic single crystals containing light atoms were synthesized using the molten metal flux growth method. In this method, one or more low-melting metals such as aluminum, gallium, tin, and bismuth are used in excess as the reaction medium. This solution-state approach allows for lower reaction temperatures compared to solid-state reactions and enables the isolation of kinetic products rather than thermodynamically stable compounds. The synthesized crystals were analyzed using an extensive array of analytical and computational characterization techniques, including single crystal X-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, magnetization measurements, and density functional theory calculations. These analyses provided detailed insights into the structural and magnetic properties of the synthesized materials.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
DOE OSTI2022

Intermetallic particle heterogeneity controls shear localization in high-strength nanostructured Al alloys

The mechanical behavior of two nanocrystalline Al alloys, Al-Mg-Y and Al-Fe-Y, is investigated with in-situ micropillar compression testing. Both alloys were strengthened by a hierarchical microstructure including grain boundary segregation, nanometer-thick amorphous complexions, carbide nanorod precipitates with sizes of a few nanometers, and submicron-scale intermetallic particles. The maximum yield strength of the Al-Mg-Y system is measured to be 950 MPa, exceeding that of the Al-Fe-Y system (680 MPa), primarily due to a combination of more carbide nanorods and more amorphous complexions. Both alloys exhibited yield strengths much higher than those of commercial Al alloys, and therefore have great potential for structural applications. However, some micropillar specimens were observed to plastically soften through shear banding. Post-mortem investigation revealed that intermetallic-free deformation pathways of a few micrometers in length were responsible for this failure. Further characterization showed significant grain growth within the shear band. The coarsened grains maintained the same orientation with each other, pointing to grain boundary mechanisms for plastic flow, specifically grain rotation and/or grain boundary migration. Here, the presence of intermetallic particles makes it difficult for both matrix and intermetallic grains to rotate into the same orientation due to the different lattice parameters and slip systems. Therefore, we are able to conclude that a uniform distribution of intermetallic particles with an average spacing less than the percolation length of shear localization can effectively prevent the maturation of shear bands, offering a design strategy for high-strength nanocrystalline Al alloys with both high strength and stable plastic flow.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Probing the solidification of quasicrystals via joint experiment and simulation (Final Report)

Quasicrystals (QCs) possess long-range positional order but non-crystallographic orientational order. Their classically ‘forbidden’ symmetry has long attracted the interest of scientists worldwide. Despite their frequent observation in both metal alloys and soft matter structures in the 35 years since their discovery, little is known about how QCs evolve from a liquid, amorphous, or crystalline precursor. In this project, we sought to resolve the enigma of QC self-assembly through a combined experimental and computational program. The Shahani group employed in situ electron and synchrotron X ray imaging to peer into the growth dynamics of QCs in a liquid, covering a broad range of length scales and solidification pathways. Glotzer's team developed new simulation models incorporating phasonic defects — which are unique to quasicrystals — and used this model to investigate two grains growing together, closely mimicking the experimental conditions. While QCs remain exceptional structures, most compounds in the realm of intermetallics adopt non-trivial geometries. In fact, only around 6% of phases are comprised of the simplest sphere packings that researchers so readily associate with metals. State-of-the-art knowledge of phase transformations at the outset of this collaborative project did not encompass the remaining 94% of intermetallic compounds that possess complex and aperiodic structure types. Therefore, we expect that outcomes from this project will have immediate and profound impact on synthesis and processing science: our efforts will be used to not only explain the growth dynamics of QCs but also complex intermetallics more broadly.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Creep Properties of NiAl-1Hf Single Crystals Re-Investigated

NiAl-1Hf single crystals have been shown to be quite strong at 1027 C, with strength levels approaching those of advanced Ni-based superalloys. Initial testing, however, indicated that the properties might not be reproducible. Study of the 1027 C creep behavior of four different NiAl-1Hf single-crystal ingots subjected to several different heat treatments indicated that strength lies in a narrow band. Thus, we concluded that the mechanical properties are reproducible. Recent investigations of the intermetallic NiAl have confirmed that minor alloying additions combined with single-crystal growth technology can produce elevated temperature strength levels approaching those of Ni-based superalloys. For example, General Electric alloy AFN 12 {Ni-48.5(at.%) Al-0.5Hf-1Ti-0.05Ga} has a creep rupture strength equivalent to Rene 80 combined with a approximately 30-percent lower density, a fourfold improvement in thermal conductivity, and the ability to form a self-protective alumina scale in aggressive environments. Although the compositions of strong NiAl single crystals are relatively simple, the microstructures are complex and vary with the heat treatment and with small ingot-toingot variations in the alloy chemistry. In addition, initial testing suggested a strong dependence between microstructure and creep strength. If these observations were true, the ability to utilize NiAl single-crystal rotating components in turbine machinery could be severely limited. To investigate the possible limitations in the creep response of high-strength NiAl single crystals, the NASA Glenn Research Center at Lewis Field initiated an in depth investigation of the effect of heat treatment on the microstructure and subsequent 1027 C creep behavior of [001]-oriented NiAl-1Hf with a nominal chemistry of Ni-47.5Al-1Hf-0.5Si. This alloy was selected since four ingots, grown over a number of years and possessing slightly different compositions, were available for study. Specimens taken from the ingots were subjected to several heat treatment schedules, examined by transmission electron microscopy, and tested in both compression and tension. An example of the microstructure found in a [001]-oriented NiAl-1Hf specimen after a solution treatment at 1317 C for 50 hr followed by air cooling is illustrated in the image on the left, where the NiAl matrix contains a uniform distribution of nanometer-scale Gphase (Ni16Hf6Si7) precipitates. Other heat treating schedules produced microstructures with nanometer-sized G-phase cubes and plates or, in an extreme case, produced a microstructure with all the G-phase converted to Heusler (Ni2AlHf) particles. The results of 1027 C creep strength and strain rate testing are illustrated which summarizes data from tensile and compressive testing of samples cut from all four NiAl-1Hf ingots and subjected to a variety of heat treatment schedules. With one exception, all the strength values lie in a narrow band that spans six orders of magnitude in strain rate. The only factor that produced results outside of this band was the heat treatment schedule that dissolved all the G-phase and replaced it with Heusler precipitates. The results portrayed in this figure lead to the important practical conclusion that the elevated-temperature creep properties of NiAl-1Hf single crystals are reproducible and are not affected by small variations in alloy chemistry from ingot to ingot or by different initial distributions of G-phase in the heat-treated alloy. The only variable in this study that produced a significant and delerious effect on mechanical strength was a post-solution heat treatment that lead to the complete disappearance of the G-phase in favor of Heusler precipitates.

Whittenberger, J. Daniel↗
DOE OSTI2022

Review on crystal structures and magnetic properties of RTX 3 materials

The structural and compositional diversity of the RTX 3 family of materials offers various magnetic and thermodynamic properties such as complex magnetic structure, vibronic bound states, heavy-fermions, valence fluctuations, metamagnetism, spin glass behavior, quantum criticality, and unconventional superconductivity. In this study we present an overview of the crystal structures, crystal growth and magnetic properties of RTX 3 compounds as well as a discussion of the relevant physics. The magnetic properties of several compounds of the RTX 3 family still remain unexplored. The compounds with a complex magnetic structure could potentially host exotic topological phases. This review article may help explore exotic magnetic properties such as the vibron state and topological spin textures.

quantum materials↗
DOE OSTI2026

Growth Strategy of a Hybrid Yb3Rh4Sn13/LaRuSn3 Structure Type: Integrating Thermal Analysis, In Situ Diffraction, and Geometric Descriptors

Remeika phases form a versatile family of cage like intermetallics built from transition metal–centered trigonal prisms linked into three dimensional frameworks that generate two characteristic voids: a large [AX₁₂] cuboctahedral cage hosting the rare earth ion and an [XX′₁₂] icosahedral cage accommodating the tetrel atom. In this work, we present a tool driven approach for targeted solid state synthesis of Remeika phases, integrating differential scanning calorimetry, in situ neutron diffraction, and a geometric tolerance factor that quantifies rare earth size compatibility within these polyhedral cages. When combined with arc melting and metallic flux crystal growth, this framework enables prediction, verification, and isolation of specific Remeika phases. Applying this strategy, we obtain single crystals of the predicted pseudo-perovskite Fe based Remeika compound Yb0.9FeGe3.1. More broadly, this perspective highlights how coupling real time structural probes with simple geometric descriptors provides a general pathway for designing synthesis conditions and accessing potentially metastable structure types in complex intermetallic systems.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Constructing Highly Durable Fuel Cell Catalysts Through Integrating Graphitic Shell‐Protected Composite Carbon Support with Gaseous Co Deposition‐Driven PtCo Intermetallics

Metal dissolution, nanoparticle agglomeration, and carbon support corrosion cause significant performance degradation of current PtCo catalysts under acidic and oxidative oxygen reduction reaction. Here, in this study, an integrated strategy is presented to design high-performance Pt 3 Co intermetallic catalysts by regulating gaseous Co deposition-driven diffusion into Pt nanoparticles supported on a composite carbon. The composite carbon is derived from ZIF-8/polyaniline, consisting of a high-surface-area (HSC) core and a protective graphitic shell (GS), which is employed to design 40 wt.% Pt/HSC@GS catalyst. The corresponding membrane electrode assemblies (MEAs) can maintain 1.09 A cm −2 at 0.7 V (20. 7% loss) after 10 000 cycles (1.0–1.5 V for carbon stability) and 1.15 A cm −2 (16.1% loss) after 150 000 cycles (0.60–0.95 V for catalyst stability). A ordered Pt 3 Co intermetallic is synthesized via a gaseous Co-deposition process, which yields a homogeneous Co-rich layer onto the Pt nanoparticles on the composite support, thereby facilitating Co diffusion into Pt crystal during subsequent ordering annealing to form the ordered intermetallic structure. This gaseous deposition leads to a thin carbon layer on PtCo nanoparticles, inhibiting particle growth during the annealing and mitigating Co dissolution under dynamic electrochemical conditions. The PtCo catalyst achieves impressive MEA performance and long-term durability (1.45 A cm −2 at 0.7 V after 120 000 cycles) under heavy-duty conditions.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2022

Preface for the special collection commemorating the career of Pat Thiel

This Special Collection in the Journal of Vacuum Science and Technology A (JVST A) has been compiled to commemorate the career of Professor Patricia (Pat) Thiel as a scientific leader in the international surface science community. Pat passed away in September 2020 due to breast cancer. This Collection includes 26 articles from colleagues, collaborators, and former Thiel group members. The topics overlap Pat’s scientific interests and advances in areas that include chemisorption, reconstruction, and complex formation on metal surfaces; submonolayer nucleation and growth and kinetic roughening of epitaxial thin films; coarsening of surface nanostructures; intercalation; surface phenomena for intermetallics including quasicrystals; and atomic-scale friction. We wish to thank the authors for their contributions towards producing this impressive Special Collection.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2021

Disorder trapping and formation of antiphase nanodomains in Ni 3 Sn: in situ observation and high resolution characterization

Rapid solidification of the intermetallic Ni 3 Sn compound from an undercooled liquid was investigated using time-resolved synchrotron X-ray diffraction. Primary growth of an ordered and a disordered cubic solid was observed in situ at a low and a high undercooling, respectively. The disordered cubic solid was reordered after rapid solidification and experienced a solid-state transformation in cooling. A HRTEM study revealed high density of crystal defects and nanodomains in the transformed matrix. A HAADFSTEM study determined that the nanodomains are antiphase domains with chemical disorder. These observations indicated a possibility of online control of mechanical properties in additively manufactured intermetallics.

36 MATERIALS SCIENCE↗
DOE OSTI2024

La 4 Co 4 X ( X = Pb , Bi , Sb ) : A demonstration of antagonistic pairs as a route to quasi-low-dimensional ternary compounds

We outline how pairs of strongly immiscible elements, referred to here as antagonistic pairs, can be used to synthesize ternary compounds with low or quasi-reduced-dimensional motifs intrinsically built into their crystal structures. By identifying third elements that are mutually compatible with a given antagonistic pair, ternary compounds can be formed in which the third element segregates the immiscible atoms into spatially separated substructures. Quasi-low-dimensional structural units, such as sheets, chains, or clusters are a natural consequence of the immiscible atoms seeking to avoid close contact in the solid state. Further, as proof of principle, we present the discovery, crystal growth, and basic physical properties of La 4 ⁢Co 4 ⁢$\mathrm{X}$ (X = Pb, Bi, Sb), a family of intermetallic compounds based on the antagonistic pairs Co-Pb and Co-Bi. La 4 ⁢Co 4 ⁢$\mathrm{X}$ adopts an orthorhombic crystal structure (space group Pbam) containing quasi-two-dimensional Co slabs and La-X polyhedra that stack in an alternating manner along the α axis. Consistent with our proposal, the La atoms separate the Co and X substructures, ensuring there are no direct contacts between the members of the immiscible (antagonistic) pair. Within the Co slabs, the atoms occupy the vertices of corner sharing tetrahedra and triangles, and this bonding motif produces narrow electronic bands near the Fermi level that favor magnetism. The Co is moment bearing in each La 4 ⁢Co 4 $\mathrm{X}$ compound studied, and we show that whereas La 4 ⁢Co 4 ⁢Pb behaves as a three-dimensional antiferromagnet with T N =220K, La 4 ⁢Co 4 ⁢Bi and La 4⁢ Co 4 ⁢Sb have behavior consistent with low-dimensional magnetic coupling and ordering, with T N =153K and 143 K, respectively. In addition to the Pb-, Bi-, and Sb-based La 4 ⁢Co 4 ⁢$\mathrm{X}$ compounds, we also were likely able to produce an analogous La 4 ⁢Co 4 ⁢Sn in polycrystalline form, although we were unable to isolate single crystals. We anticipate that identifying and using mutually compatible third elements together with an antagonistic pair represents a generalizable design principle for discovering new materials and new structure types containing low-dimensional substructures.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Template Assisted Lithium Superoxide Growth for Lithium-Oxygen Batteries

Developing batteries with energy densities comparable to internal combustion technology is essential for a worldwide transition to electrified transportation. Li-O2 batteries are seen as the ‘holy grail’ of battery technologies since they have the highest theoretical energy density of all battery technologies. Current lithium-oxygen (Li-O2) batteries suffer from large charge overpotentials related to electronic resistivity of the insulating lithium peroxide (Li2O2) discharge product. One potential solution is the formation and stabilization of a lithium superoxide (LiO2) discharge intermediate that exhibits good electronic conductivity. However, LiO2 is reported to be unstable at ambient temperature despite its favorable formation energy at -1.0 eV/atom. In this paper, based on our recent work on the development of cathode materials for aprotic lithium oxygen batteries including two intermetallic compounds, LiIr3 and LiIr, that are found to form good template interfaces with LiO2, a simple goodness of fit R factor to gauge how well a template surface structure can support LiO2 growth is developed. The R factor is a quantitative measurement to calculate the geometric difference in the unit cells of specific Miller Index 2D planes of the template surface and LiO2. Using this as a guide, the R factors for LiIr3, LiIr, and La2NiO4+, are found to be good. This guide is attested by simple extension to other noble metal intermetallics with electrochemical cycling data including LiRh3, LiRh, and Li2Pd. Finally, the template concept is extended to main group elements and the R factors for LiO2 (111) and Li2Ca suggest that Li2Ca is a possible candidate for the template assisted LiO2 growth strategy.

Intermetallics↗
DOE OSTI2022

Interdiffusion and Formation of Intermetallic Compounds in High-Temperature Power Electronics Substrate Joints Fabricated by Transient Liquid Phase Bonding

Power electronics packages typically comprise a dielectric substrate bonded to a metal layer and attached to heat sinks using a low-thermal-conductivity solder. These multiple layers increase the effective thermal resistance of the package and are responsible for package failures under cyclic thermal loads. Bonding the aluminum nitride dielectric layer (AlN) directly to a low coefficient of thermal expansion (CTE) aluminum silicon carbide (AlSiC) cold plate using copper-aluminum (Cu-Al) transient liquid phase (TLP) bonding has been shown to improve the mechanical reliability of the power electronic packages while making the package more compact by bringing the cooling solutions closer to the devices. This study aims to characterize the Cu-Al bonds formed during the TLP bonding of AlSiC with three different power electronics substrates: pure aluminum nitride (AlN), aluminum (DBA), and copper (DBC). The material compositions and microstructures of the bonds were analyzed using scanning electron microscopy (SEM), x-ray spectroscopy (EDS), confocal scanning acoustic microscopy (C-SAM), and x-ray diffraction (XRD). ..alpha..-Al solid compound was identified as the dominant phase in AlN-AlSiC and Al-AlSiC, with a notable presence of SiC particles. In contrast, three intermetallic phases - ..theta..-CuAl2, ..eta..-CuAl, and ..gamma..'- Cu9Al4 - were observed in the Cu-AlSiC bond. A computational solid-state diffusion model was developed to predict the intermetallic compounds (IMCs) formed during Cu-Al TLP bonding in each system, which supported the observation that an initial Cu volume fraction of 20 % in the material layers produced a final bond composition of >95 % Al with minimal IMC growth. However, increased Cu concentrations produced higher concentration gradients, leading to increased growth of IMCs, Kirkendall voids, and interstitial cracks.

DIRECT ENERGY CONVERSION↗