Self-propagating high-temperature synthesis of ceramic materials based on the M<Subscript><Emphasis Type="Italic">n</Emphasis> + 1</Subscript>AX<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> phases in the Ti-Cr-Al-C system

Compact ceramic materials based on the M_{n + 1}AX _n phases in the Ti-Cr-Al-C system are produced by forced self-propagating high-temperature synthesis (SHS) compaction. The mechanisms of the structure and phase formation in synthetic products, as well as the combustion macrokinetics of the SHS mixture, are studied. Complex investigations of the structure, phase composition, and physical and mechanical properties of new Ti_{2 ? x} Cr _x AlC ceramic materials synthesized at different charging parameters (x = 0, 0.5, 1, 1.5, and 2) are performed. The highest content (96–98%) of the M_{n + 1}AX _n phase in the composition of synthetic products is found to be in samples where just one of the host elements (titanium (x = 0) or chromium (x = 2)) is present. The produced materials have a high heat resistance, and the increase in the chromium concentration is favorable to an appreciable growth in resistance to high-temperature oxidation.     

Estimation of the Ultimate Tensile Strength of Steel from Its <Emphasis Type="Italic">HB</Emphasis> and <Emphasis Type="Italic">HV</Emphasis> Hardness Numbers and Coercive Force

A formula is derived to accurately describe the tabulated relation between the Brinell (HB) and Vickers (HV) hardnesses of steel over the entire range of their possible variation. This formula and the formulas describing the relation between the HB hardness of chromium–molybdenum and chromium–nickel steels and their ultimate tensile strength σ_u are used to analyze the change in σ_u of 38KhNM steel upon quenching and tempering. The data that reveal a relation between σ_u of 38KhNM steel and its coercive force are obtained.     

Microstructure and Properties of Fe<Subscript>3</Subscript>Al-Fe<Subscript>3</Subscript>AlC<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> Composite Prepared by Reactive Liquid Processing

A Fe₃Al-Fe₃AlC _x composite was prepared using reactive liquid processing (RLP) through controlled mixture of carbon steel and aluminum in the liquid state. The microstructure and phases of the composite were assessed using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, optical microscopy, and differential scanning calorimetry. In addition, the density, hardness, microhardness, and elastic modulus were evaluated. The Fe₃Al-Fe₃AlC _x composite consisted of 65 vol pct Fe₃Al and 35 vol pct Fe₃AlC _x (κ). The κ phase contained 10.62 at. pct C, resulting in the stoichiometry Fe₃AlC_0.475. The elastic modulus of the Fe₃Al-Fe₃AlC_0.475 composite followed the rule of mixtures. The RLP technique was shown to be capable of producing Fe₃Al-Fe₃AlC_0.475 with a microstructure and properties similar to those achieved using other processing techniques reported in the literature.     

Rare-earth metals (REMs) in nickel aluminide-based alloys: II. Effect of a REM on the phase composition of a multicomponent Ni<Subscript>3</Subscript>Al-based alloy

The hardening mechanisms are studied in the cast high-temperature next-generation materials that are based on the intermetallic compound Ni₃Al and are low alloyed with refractory (W, Re, Mo, Cr) and reaction- and surface-active (REM, Ti, etc.) metals. The interaction of the main impurities (C, O, Si, S) with three characteristic representatives of the REM group (namely, Y, La, Ce), which can be used for alloying, is analyzed. The reported data on the behavior of some REMs in the alloys based on nickel monoaluminide NiAl are considered. The effect of the REMs on the phase compositions of real multicomponent semicommercial Ni₃Al-based VKNA alloys produced by directional solidification is investigated, and the excess phases precipitating upon alloying are revealed. Alloying with refractory metals and REMs is shown to lead to the formation of nanophases that stabilize the dendritic or single-crystal structure of VKNA-type cast alloys and strengthen the interface boundaries in them.     

Mechanical Behavior of Three-Dimensional Braided Nickel-Based Superalloys Synthesized <Emphasis Type="Italic">via</Emphasis> Pack Cementation

Braided tubes of Ni-based superalloys are fabricated via three-dimensional (3-D) braiding of ductile Ni-20Cr (wt pct) wires followed by post-textile gas-phase alloying with Al and Ti to create, after homogenization and aging, γ/γ′ strengthened lightweight, porous structures. Tensile tests reveal an increase in strength by 100 MPa compared to as-braided Ni-20Cr (wt pct). An interrupted tensile test, combined with X-ray tomographic scans between each step, sheds light on the failure behavior of the braided superalloy tubes.     

<Emphasis Type="Italic">R</Emphasis>-Curve Approach to Describe the Fracture Resistance of Tool Steels

This work addresses the events involved in the fracture of tool steels, aiming to understand the effect of primary carbides, inclusions, and the metallic matrix on their effective fracture toughness and strength. Microstructurally different steels were investigated. It is found that cracks nucleate on carbides or inclusions at stress values lower than the fracture resistance. It is experimentally evidenced that such cracks exhibit an increasing growth resistance as they progressively extend, i.e., R-curve behavior. Ingot cast steels present a rising R-curve, which implies that the effective toughness developed by small cracks is lower than that determined with long artificial cracks. On the other hand, cracks grow steadily in the powder metallurgy tool steel, yielding as a result a flat R-curve. Accordingly, effective toughness for this material is mostly independent of the crack size. Thus, differences in fracture toughness values measured using short and long cracks must be considered when assessing fracture resistance of tool steels, especially when tool performance is controlled by short cracks. Hence, material selection for tools or development of new steel grades should take into consideration R-curve concepts, in order to avoid unexpected tool failures or to optimize microstructural design of tool steels, respectively.     

Functionally Graded Al Alloy Matrix <Emphasis Type="Italic">In-Situ</Emphasis> Composites

In the present work, functionally graded (FG) aluminum alloy matrix in-situ composites (FG-AMCs) with TiB₂ and TiC reinforcements were synthesized using the horizontal centrifugal casting process. A commercial Al-Si alloy (A356) and an Al-Cu alloy were used as matrices in the present study. The material parameters (such as matrix and reinforcement type) and process parameters (such as mold temperature, mold speed, and melt stirring) were found to influence the gradient in the FG-AMCs. Detailed microstructural analysis of the composites in different processing conditions revealed that the gradients in the reinforcement modify the microstructure and hardness of the Al alloy. The segregated in-situ formed TiB₂ and TiC particles change the morphology of Si particles during the solidification of Al-Si alloy. A maximum of 20 vol pct of reinforcement at the surface was achieved by this process in the Al-4Cu-TiB₂ system. The stirring of the melt before pouring causes the reinforcement particles to segregate at the periphery of the casting, while in the absence of such stirring, the particles are segregated at the interior of the casting.     

Infrared Brazing of Ti<Subscript>50</Subscript>Ni<Subscript>50</Subscript> Shape Memory Alloy and Inconel 600 Alloy with Two Ag-Cu-Ti Active Braze Alloys

Infrared brazing of Ti₅₀Ni₅₀ SMA and Inconel 600 alloy using Cusil-ABA and Ticusil filler metals has been investigated. The joints were dominated by Ag-Cu eutectic with proeutectic Cu in the Cusil-ABA brazed joint and with proeutectic Ag in the Ticusil one. A continuous curved belt composed of a Ni₃Ti layer and a (Cu _x Ni_1?x )₂Ti layer formed in the brazed Ti₅₀Ni₅₀/Ticusil/Inconel 600 joint. On the Ti₅₀Ni₅₀ SMA side, an intermetallic layer of (Cu _x Ni_1?x )₂Ti formed in all joints, with x values around 0.81 and 0.47. Layers of (Cu _x Ni_1?x )₂Ti, Ni₃Ti, and mixed Ni₃Ti and Ni₂Cr intermetallics were observed next to the Inconel 600 substrate in the brazed Ti₅₀Ni₅₀/Cusil-ABA/Inconel 600 joint. The maximum shear strengths of the joints using the Cusil-ABA filler metal and the Ticusil filler metal were 324 and 300 MPa, respectively. In the Cusil-ABA brazed joint, cracks with cleavage-dominated fracture propagated along the (Cu _x Ni_1?x )₂Ti interfacial layer next to the Ti₅₀Ni₅₀ SMA substrate. In the Ticusil brazed joint, ductile dimple fracture occurred in the Ag-rich matrix near the Inconel 600 alloy substrate. The absence of a detrimental Ti-Fe-(Cu) layer on the Inconel 600 substrate side can effectively improve the shear strength of the joint.     

Inclusion Detection in Aluminum Alloys <Emphasis Type="Italic">Via</Emphasis> Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy (LIBS) has shown promise as a technique to quickly determine molten metal chemistry in real time. Because of its characteristics, LIBS could also be used as a technique to sense for unwanted inclusions and impurities. Simulated Al₂O₃ inclusions were added to molten aluminum via a metal-matrix composite. LIBS was performed in situ to determine whether particles could be detected. Outlier analysis on oxygen signal was performed on LIBS data and compared to oxide volume fraction measured through metallography. It was determined that LIBS could differentiate between melts with different amounts of inclusions by monitoring the fluctuations in signal for elements of interest. LIBS shows promise as an enabling tool for monitoring metal cleanliness.     

Morphology-Dependent Hardness of Cr<Subscript>7</Subscript>C<Subscript>3</Subscript>-Ni-Rich Alloy Composite <Emphasis Type="Italic">vs</Emphasis> Orientation Independent Hardness of Cr<Subscript>7</Subscript>C<Subscript>3</Subscript> Primary Phase in a Laser Clad Microstructure

Microstructural evolution with superheating was studied in chromium carbide-nickel coatings deposited by laser cladding. At lower superheating, selective growth of 〈0001〉 direction from the high density of Cr₇C₃ grains nucleated resulted in a columnar structure with (0001) texture. Increased superheating lead to the loss of columnar structure as well as the (0001) texture. The hexagonal Cr₇C₃ showed an unusual isotropic nanoindentation hardness evidently correlated with its low c/a ratio. However, the rod-like morphology of the carbide dendrites resulted in significant anisotropy in the hardness of the composite.     

Physicochemical laws of the interaction of nickel aluminides with alloying elements: II. Interaction of nickel aluminides with alloying elements and/or interstitial phases

The Ni-Al-X (X is an interstitial element or phase) phase diagrams are analyzed to reveal systems that can be used as the basis for designing promising alloys and natural composites based on nickel aluminides reinforced by interstitial phases (natural composites I). The most thermally stable materials are shown to be heterophase alloys and composite materials (CMs) located in the eutectic-type (including degenerate eutectic) pseudobinary sections of ternary or multicomponent phase diagrams. They exhibit insignificant (or zero) dissolution of interstitial phases at operating temperatures and the absence of an intense interaction between CM components (natural composites II). Natural composites I based on the NiAl-or Ni₃Al-interstitial phase alloys produced upon cooling from a melt can be reinforced by the refractory thermally stable rigid interstitial phases, namely, borides and carbides, that are present in pseudobinary sections in equilibrium with these nickel aluminides, since the elements forming these phases dissolve completely in matrix melts and the mutual solubility of these phases in the solid state is low. Such borides are TiB₂ and HfB₂ in equilibrium with β-NiAl, and such carbides are, e.g., TiC and HfC in equilibrium with β-NiAl and La₂C₃, NbC, and TaC in equilibrium with γ′-Ni₃Al. Natural composites II should be produced using solid-phase methods (NiAl with AlN, Y₂O₃, Al₂O₃) or a combination of methods, where a refractory interstitial phase of the Al₂O₃ or Y₂O₃ type is solid and the intermetallic NiAl or Ni₃Al matrix is liquid. NiAl-TiB₂ (HfB₂), NiAl-Al₂O₃ (Y₂O₃), and Ni₃Al-La₂C₃ (NbC, TaC) composites are considered as examples.     

<Emphasis Type="Italic">In Situ</Emphasis> Investigation of the Evolution of Lattice Strain and Stresses in Austenite and Martensite During Quenching and Tempering of Steel

Energy dispersive synchrotron X-ray diffraction was applied to investigate in situ the evolution of lattice strains and stresses in austenite and martensite during quenching and tempering of a soft martensitic stainless steel. In one experiment, lattice strains in austenite and martensite were measured in situ in the direction perpendicular to the sample surface during an austenitization, quenching, and tempering cycle. In a second experiment, the sin² ψ method was applied in situ during the austenite-to-martensite transformation to distinguish between macro- and phase-specific micro-stresses and to follow the evolution of these stresses during transformation. Martensite formation evokes compressive stress in austenite that is balanced by tensile stress in martensite. Tempering to 748 K (475 °C) leads to partial relaxation of these stresses. Additionally, data reveal that (elastic) lattice strain in austenite is not hydrostatic but hkl dependent, which is ascribed to plastic deformation of this phase during martensite formation and is considered responsible for anomalous behavior of the 200 _γ reflection.     

Effects of Powder Carrier on the Morphology and Compressive Strength of Iron Foams: Water <Emphasis Type="Italic">vs</Emphasis> Camphene

With its well-known popularity in structural applications, considerable attention has recently been paid to iron (Fe) and its oxides for its promising functional applications such as biodegradable implants, water-splitting electrodes, and the anode of lithium-ion batteries. For these applications, iron and its oxides can be even further utilized in the form of porous structures. In order to control the pore size, shape, and amount, we synthesized Fe foams using suspensions of micrometric Fe₂O₃ powder reduced to Fe via freeze casting in water or liquid camphene as a solvent through sublimation of either ice or camphene under 5 pct H₂/Ar gas and sintering. We then compared them and found that the resulting Fe foam using water as a solvent (p?=?71.7 pct) showed aligned lamellar macropores replicating ice dendrite colonies, while Fe foam using camphene as a solvent (p?=?68.0 pct) exhibited interconnected equiaxed macropores replicating camphene dendrites. For all directions with respect to the loading axis, the compressive behavior of the water-based Fe foam with a directional elongated wall pore structure was anisotropic (11.6?±?0.9 MPa vs 7.8?±?0.8 MPa), whereas that of the camphene-based Fe foam with a random round pore structure was nearly isotropic (12.0?±?1.1 MPa vs 11.6?±?0.4 MPa).     

<Emphasis Type="Italic">In situ</Emphasis> Observation of Calcium Oxide Treatment of Inclusions in Molten Steel by Confocal Microscopy

Calcium treatment of aluminum killed steel was observed in situ using high-temperature confocal scanning laser microscope (HT-CSLM). This technique along with a novel experimental design enables continuous observation of clustering behavior of inclusions before and after the calcium treatment. Results show that the increase in average inclusion size in non-calcium-treated condition was much faster compared to calcium-treated condition. Results also show that the magnitude of attractive capillary force between inclusion particles in non-treated condition was about 10^?15 N for larger particles (10 µm) and 10^?16 N for smaller particles (5 µm) and acting length of force was about 30 µm. In the case of calcium-treated condition, the magnitude and acting length of force was reduced to 10^?16 N and 10 µm, respectively, for particles of all sizes. This change in attractive capillary attractive force is due to change in inclusion morphology from solid alumina disks to liquid lens particles during calcium treatment.     

Mechanochemical preparation of Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Al<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposites

The mechanochemical preparation of nickel aluminide/corundum (Ni _x Al _y /Al₂O₃) powder nanocomposites is shown to be possible during the mechanochemical aluminum reduction of nickel oxide at various weight proportions of the components.     

Synthesis and Non-isothermal Carbothermic Reduction of FeTiO<Subscript>3</Subscript>-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> Solid Solution Systems

To investigate the carbothermic reduction behaviors of xFeTiO₃·(1 ? x)Fe₂O₃ solid solutions, the solid solutions with different x values were synthesized and used in the corresponding reactions. With an increase in x, the temperature pertaining to the onset of carbothermic reduction increased, while the rate of reduction of the solid solutions, α, decreased. The lattice parameters calculated from XRD patterns indicated that the solid solution with a higher x led to a larger lattice distortion. The non-isothermal kinetics were calculated, and an average activation energy E value of 3.0 × 10² kJ/mol was obtained.     

Physical and Mechanical Behaviour of <Emphasis Type="Italic">Sida acuta</Emphasis> Fibre Reinforced Epoxy Composite at Different Fibre Loading

Sida acuta is the botanical name of the plant belonging to Malvaceae family. Sida acuta fibres are available in nature, relatively low cost and abundantly available in India. The present work has been carried out to make use of Sida acuta fibres in the fibre reinforced polymer composites. In this study the composites are made using untreated bidirectional Sida acuta stem fibre as reinforcement and commercially available epoxy resin as matrix material using hand lay-up technique. The composites are made of different fibre fabric orientation (0°/90° and ±?45°) and each fabric orientation composite with different fibre loading (0, 24, 28 and 32 wt%) are characterized for their physical and mechanical properties. The test results show the significant effect of fibre loading on the physical and mechanical properties of these composites. Also the fracture behaviour and fibre pull-out at the fracture of the composite samples have been analysed using scanning electron microscope.     

History Dependence of the Microstructure on Time-Dependent Deformation During <Emphasis Type="Italic">In-Situ</Emphasis> Cooling of a Nickel-Based Single-Crystal Superalloy

Time-dependent plastic deformation through stress relaxation and creep deformation during in-situ cooling of the as-cast single-crystal superalloy CMSX-4^® has been studied via neutron diffraction, transmission electron microscopy, electro-thermal miniature testing, and analytical modeling across two temperature regimes. Between 1000 °C and 900 °C, stress relaxation prevails and gives rise to softening as evidenced by a decreased dislocation density and the presence of long segment stacking faults in γ phase. Lattice strains decrease in both the γ matrix and γ′ precipitate phases. A constitutive viscoplastic law derived from in-situ isothermal relaxation test under-estimates the equivalent plastic strain in the prediction of the stress and strain evolution during cooling in this case. It is thereby shown that the history dependence of the microstructure needs to be taken into account while deriving a constitutive law and which becomes even more relevant at high temperatures approaching the solvus. Higher temperature cooling experiments have also been carried out between 1300 °C and 1150 °C to measure the evolution of stress and plastic strain close to the γ′ solvus temperature. In-situ cooling of samples using ETMT shows that creep dominates during high-temperature deformation between 1300 °C and 1220 °C, but below a threshold temperature, typically 1220 °C work hardening begins to prevail from increasing γ′ fraction and resulting in a rapid increase in stress. The history dependence of prior accumulated deformation is also confirmed in the flow stress measurements using a single sample while cooling. The saturation stresses in the flow stress experiments show very good agreement with the stresses measured in the cooling experiments when viscoplastic deformation is dominant. This study demonstrates that experimentation during high-temperature deformation as well as the history dependence of the microstructure during cooling plays a key role in deriving an accurate viscoplastic constitutive law for the thermo-mechanical process during cooling from solidification.     

Synthesis of Al-Zr Alloys <Emphasis Type="Italic">Via</Emphasis> ZrO<Subscript>2</Subscript> Aluminum-Thermal Reduction in KF-AlF<Subscript>3</Subscript>-Based Melts

Physical–chemical investigations of KF-AlF₃ melts were carried out in order to develop the scientific basis of the technology for Al-Zr alloy synthesis. The possibility of Al-Zr alloy synthesis via the aluminum-thermal method was shown. The liquidus temperatures of KF-AlF₃ and KF-NaF-AlF₃ melts with additions of Al₂O₃ and ZrO₂ were determined using the thermal analysis method in the temperature range from 873 K to 1173 K (600 °C to 900 °C). The dependency of the solubility of ZrO₂ in KF-AlF₃ and KF-NaF-AlF₃ melts on Al₂O₃ concentration was measured.     

Orientation-Dependent Tensile Behavior of Nanolaminated Graphene-Al Composites: An <Emphasis Type="Italic">In Situ</Emphasis> Study

We conducted in situ microtension experiments in a scanning electron microscope (SEM) to study the orientation-dependent mechanical behavior of nanolaminated graphene-Al composite. We found a transition from a weak-and-brittle behavior in the isostress composite configuration to a strong-yet-ductile tensile response in the composite under isostrain condition. This is explained by the excellent load-bearing capacity of the graphene nanosheets and a crack deflection mechanism rendered by the laminate structure. These in situ measurements enabled direct observation of the deformation procedure and the exact failure mode, which highlight the importance of microstructural control in tailoring the mechanical properties of advanced metal matrix composites (MMCs).