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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Sinter formation during directed energy deposition of titanium alloy powders

During directed energy deposition (DED) additive manufacturing, powder agglomeration and sintering can occur outside of the melt pool when using titanium alloy powders. Using in situ synchrotron radiography we investigate the mechanisms by which sintering of Ti6242 powder occurs around the pool, performing a parametric study to determine the influence of laser power and stage traverse speed on sinter build-up. The results reveal that detrimental sinter can be reduced using a high laser power or increased stage traverse speed, although the latter also reduces deposition layer thickness. The mechanism of sinter formation during DED was determined to be in-flight heating of the powder particles in the laser beam. Calculations of particle heating under the processing conditions explored in this study confirm that powder particles can reasonably exceed 700 °C, the threshold for Ti surface oxide dissolution, and thus the powder is prone to sintering if not incorporated into the melt pool. The build-up of sinter powder layer on deposit surfaces led to lack of fusion pores. To mitigate sinter formation and its detrimental effects on DED component quality, it is essential that the powder delivery spot area is smaller than the melt pool, ensuring most powder lands in the melt pool.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In-situ synchrotron X-ray diffraction of hydroxyapatite-zirconia composite during conventional and flash sintering

Here, we conducted in-situ X-ray diffraction to study the crystalline phase evolution in hydroxyapatite-zirconia composites during both conventional and flash sintering processes. Additionally, we examined the thermal history and microstructure of the composite under these sintering conditions. Despite both sintering methods reaching similar average temperatures, they yielded distinct results in terms of crystalline phase composition and microstructure. In the flash sintered samples, we observed a complete transformation of hydroxyapatite into α- tricalcium phosphate and a complete tetragonal to cubic phase transition in zirconia. Conversely, the conventionally sintered samples remained practically stable. Notably, the flash sintered samples exhibited needle-like microstructures, which were absent in their conventionally sintered counterparts. This divergence suggests that the application of an electric field plays a role in generating athermal effects during the sintering of hydroxyapatite-zirconia composites.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of sintering time on structural, microstructural and chemical composition of Ni-doped lanthanum gallate perovskites

This work reports the effect of two different sintering times, 6 and 48 h on the structural, microstructural, and chemical features of Ni-doped La{sub 0.90}Sr{sub 0.10}GaO{sub 3.00−δ}. Independently of the sintering time, La{sub 0.90}Sr{sub 0.10}Ga{sub 1−x}Ni{sub x}O{sub 3.00−δ} (where x=0.10, and 0.20 (mol)) presents a rhombohedral symmetry with a lattice volume that decreases when NiO dopant increases. Besides the perovskite, LaSrGa{sub 3.00}O{sub 7.00} (nominal composition) is present as second phase in all cases. When the samples are doped with NiO, the peaks of this second phase are shifted with respect to the peaks of the pure phase. These shifts suggest that this second phase could admit some Ni ions in its structure. According to the XRD patterns, the amount of the latter phase is larger when sintering time is increased. Electron probe microanalysis (EPMA) indicated that the matrix of the samples sintered for 6 h is constituted by a perovskite with an experimental composition very close to the nominal one. However, when the samples are sintered for 48 h the matrix of each sample is constituted by two perovskites; both with compositional deviations with respect to their nominal one. In particular, a significant Sr depletion compensated by a La increment in the A site is observed. Those compositional deviations could be mainly due to the diffusion of the cations in the bulk and/or from the bulk to the surface of the samples. That diffusion can favour the formation, not only, of a second perovskite with a different composition in relation with the first one formed, but also, the formation of second phases. In addition, a very slight broadening of Bragg peaks of the perovskites sintered for 48 h is observed by XRD and can be related to the presence of two different perovskites in each sample according to EPMA results. By BSEM and EPMA analyses La{sub 4.00}Ga{sub 2.00}O{sub 9.00} (nominal composition) is also observed as second phase when samples are treated for 48 h. - Graphical abstract: Typical microstructures, observed by FEG-SEM, of La{sub 0.90}Sr{sub 0.10}Ga{sub 1−x}Ni{sub x}O{sub 3.00−δ} materials with x=0.00 and 0.10 (nominal compositions) and sintered at 1450 °C for 48 h after polishing and thermal etching are shown. Lighter grey grains with a bimodal grain size are observed and according to XEDS analysis correspond to two perovskites with different experimental compositions (labelled as 1 and 2 for x=0.00 and labelled as 4 and 5 for x=0.10, respectively), meanwhile the darker grey phases correspond to LaSrGa{sub 3.00}O{sub 7.00} (labelled as 3 for x=0.00) and LaSr(Ga{sub 1−y′},Ni{sub y′}){sub 3.00}O{sub 7.00} (labelled as 6 for x=0.10), respectively. - Highlights: • When NiO is introduced into La{sub 0.90}Sr{sub 0.10}GaO{sub 3.00−δ} a change in symmetry is produced. • A significant Sr depletion in the A-site of perovskites treated for 48 h is observed. • Compositional deviations could be due to a thermally-activated diffusional process. • The phase purity of these materials is deteriorated when the sintering time is extended.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Development of nano-structured duplex and ferritic stainless steels by pulverisette planetary milling followed by pressureless sintering

Nano-structured duplex and ferritic stainless steel powders are prepared by planetary milling of elemental Fe, Cr and Ni powder for 40 h and then consolidated by conventional pressureless sintering. The progress of milling and the continuous refinement of stainless steel powders have been confirmed by means of X-ray diffraction and scanning electron microscopy. Activation energy for the formation of duplex and ferritic stainless steels is calculated by Kissinger method using differential scanning calorimetry and is found to be 159.24 and 90.17 KJ/mol respectively. Both duplex and ferritic stainless steel powders are consolidated at 1000, 1200 and 1400 °C in argon atmosphere to study microstructure, density and hardness. Maximum sintered density of 90% and Vickers microhardness of 550 HV are achieved for duplex stainless steel sintered at 1400 °C for 1 h. Similarly, 92% sintered density and 263 HV microhardness are achieved for ferritic stainless steel sintered at 1400 °C. - Highlights: • Synthesized duplex and ferritic stainless steels by pulverisette planetary milling • Calculated activation energy for the formation of duplex and ferritic stainless steels • Studied the effect of sintering temperature on density, hardness and microstructure • Duplex stainless steel exhibits 90% sintered density and microhardness of 550 HV. • Ferritic stainless steel shows 92% sintered density and 263 HV microhardness.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis and characterization of aluminium–alumina micro- and nano-composites by spark plasma sintering

Graphical abstract: The evolution of microstructure by varying the particle size of reinforcement in the matrix employing spark plasma sintering has been demonstrated here in Al–Al{sub 2}O{sub 3} system. An emphasis has been laid on varying the reinforcement particle size and evaluating the microstructural morphologies and their implications on mechanical performance of the composites. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) reinforced in aluminium matrix were fabricated by powder metallurgy route using spark plasma sintering technique technique at a temperature of 773 K and pressure of 50 MPa. Another set of specimens having composition 1, 5, 20 vol.% of alumina (average size ∼ 10 μm) had been fabricated to compare the physical as well as mechanical attributes of the microcomposite as well as the nanocomposites. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation measurements. The alumina nanoparticles revealed an interface showing appreciable physical intimacy with the aluminium matrix compared to that of the alumina microparticles. The interfacial integrity in case of nanocomposites is better than in the microcomposite which has been studied using microscopic techniques. Spark plasma sintering imparts enhanced densification as well as matrix-reinforcement proximity which has been corroborated with the experimental results. - Highlights: • The Al–Al{sub 2}O{sub 3} micro- and nano-composites fabricated by spark plasma sintering. • Better matrix-reinforcement integrity in nanocomposites than microcomposites. • Spark plasma sintering method results in higher density and hardness values. • High density and hardness values of nanocomposites than microcomposites. • High dislocation density in spark plasma sintered Al–Al{sub 2}O{sub 3} composites. - Abstract: In the present study, an emphasis has been laid on evaluation of the microstructural morphologies and their implications on mechanical performance of the composites by varying the reinforcement particle size. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) and microcomposites of 1, 5, 20 volume % of alumina (average size ∼ 10 μm) reinforced in aluminium matrix were fabricated by spark plasma sintering technique at a temperature of 773 K and pressure of 50 MPa. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation hardness measurements. The alumina nanoparticles revealed appreciable physical intimacy with the aluminium matrix than that of alumina microparticles. The highest nanohardness recorded 0.85 GPa and 99% densification for 7 and 1 vol.% Al–Al{sub 2}O{sub 3} nancomposites respectively. Spark plasma sintering imparts enhanced densification and matrix-reinforcement proximity which have been corroborated with the experimental results.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Tunning of microstructure and thermoelectric properties of Ca{sub 3}Co{sub 4}O{sub 9} ceramics by high-magnetic-field sintering

The structural, magnetic, electrical, and thermal transport properties of Ca{sub 3}Co{sub 4}O{sub 9} ceramics sintered under high magnetic field were investigated. Crystal grain texturing and densification were achieved through cold-pressing and high-magnetic-field sintering techniques. The c-axis of the layered crystal grain was partly oriented along the c-axis of the pressed samples via a cold-pressing technique, and the degree of orientation was further increased while applying the magnetic field in the sample sintering progress. The easy magnetization axis of Ca{sub 3}Co{sub 4}O{sub 9} polycrystalline ceramics was found to be the c-axis. The room-temperature resistivity along the ab-plane of the sample sintered under 8 T magnetic field was about 30% smaller than that of the sample sintered without magnetic field, and the Seebeck coefficient of the former reached 177.7 {mu}V/K at the room temperature, which is about 50% larger than that of the latter. Consequently, for the sample sintered at 8 T magnetic field, the power factor along the ab-plane was enhanced by about 1.8 times compared to the sample without magnetic field sintering. The obtained result is suggested to originate from the variations of the carrier mobility and spin-orbital degeneracy due to high-magnetic-field sintering in the progress of the sample preparation.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Selective light sintering of Aerosol-Jet printed silver nanoparticle inks on polymer substrates

Printing silver nanoparticle inks to generate conductive structures for electronics on polymer substrates has gained increasing relevance in recent years. In this context, the Aerosol-Jet Technology is well suited to print silver ink on 3D-Molded Interconnect Devices (MID). The deposited ink requires thermal post-treatment to obtain sufficient electrical conductivity and adhesion. However, commonly used oven sintering cannot be applied for many thermoplastic substrates due to low melting temperatures. In this study a new sintering technology, selective light sintering, is presented, based on the focused, continuous light beam of a xenon lamp. Sintering experiments were conducted with Aerosol-Jet printed structures on various polycarbonate (PC) substrates. Especially on neat, light transparent PC, silver tracks were evenly sintered with marginal impact to the substrate. Electrical conductivities significantly exceed the values obtained with conventional oven sintering. Adhesive strength is sufficient for conductive tracks. Experiments with non-transparent PC substrates led to substrate damage due to increased light absorption. Therefore a concept for a variation of light sintering was developed, using optical filters. First experiments showed significant reduction of substrate damage and good sintering qualities. The highly promising results of the conducted experiments provide a base for further investigations to increase adhesion and qualifying the technology for MID applications and a broad spectrum of thermoplastic substrates.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of sintering temperature on feature resolution and flexural strength of ceramics fabricated through vat photopolymerization additive manufacturing

Although ceramic additive manufacturing (AM) could be used to fabricate complex, high-resolution parts for diverse, functional applications, one ongoing challenge is optimizing the post-process, particularly sintering, conditions to consistently produce geometrically accurate and mechanically robust parts. This study aims to investigate how sintering temperature affects feature resolution and flexural properties of silica-based parts formed by vat photopolymerization (VPP) AM. Test artifacts were designed to evaluate features of different sizes, shapes and orientations, and three-point bend specimens printed in multiple orientations were used to evaluate mechanical properties. Sintering temperatures were varied between 1000°C and 1300°C. Deviations from designed dimensions often increased with higher sintering temperatures and/or larger features. Higher sintering temperatures yielded parts with higher strength and lower strain at break. Many features exhibited defects, often dependent on geometry and sintering temperature, highlighting the need for further analysis of debinding and sintering parameters. To the best of the authors’ knowledge, this is the first time test artifacts have been designed for ceramic VPP. This work also offers insights into the effect of sintering temperature and print orientation on flexural properties. These results provide design guidelines for a particular material, while the methodology outlined for assessing feature resolution and flexural strength is broadly applicable to other ceramics, enabling more predictable part performance when considering the future design and manufacture of complex ceramic parts.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Synthesis of BaTiO[subscript 3]-20wt%CoFe[subscript 2]O[subscript 4] Nanocomposites via Spark Plasma Sintering

Barium titanate-20wt% cobalt ferrite (BaTiO{sub 3}-20wt%CoFe{sub 2}O{sub 4}) nanocomposites were sintered from nanocrystalline BaTiO{sub 3} and CoFe{sub 2}O{sub 4} powders using spark plasma sintering (SPS) and pressureless sintering (PS) techniques. Using SPS, dense polycrystalline composites were obtained at a sintering temperature as low as 860 C and a time of 5 min whereas PS required a higher sintering temperature (1150 C) and time (120 min) to obtain similarly dense composites. Microstructural analysis of the composites showed that both the techniques retained nanocrystalline grain sizes after sintering. High resolution X-ray diffraction measurements revealed that the BaTiO{sub 3}-20wt%CoFe{sub 2}O{sub 4} composites sintered by the SPS technique did not exhibit formation of any new phase(s) due to reaction between the BaTiO{sub 3} and CoFe{sub 2}O{sub 4} phases during sintering. However, the PS technique resulted in the formation of additional phases (other than the BaTiO{sub 3} and CoFe{sub 2}O{sub 4} phases) in the composites. While the composites synthesized by SPS were of superior phase-purity, evidence of Fe diffusion from the spinel to the perovskite phase was found from X-ray diffraction and permittivity measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Properties of Bulk Sintered Silver As a Function of Porosity

This report summarizes a study where various properties of bulk-sintered silver were investigated over a range of porosity. This work was conducted within the National Transportation Research Center's Power Device Packaging project that is part of the DOE Vehicle Technologies Advanced Power Electronics and Electric Motors Program. Sintered silver, as an interconnect material in power electronics, inherently has porosity in its produced structure because of the way it is made. Therefore, interest existed in this study to examine if that porosity affected electrical properties, thermal properties, and mechanical properties because any dependencies could affect the intended function (e.g., thermal transfer, mechanical stress relief, etc.) or reliability of that interconnect layer and alter how its performance is modeled. Disks of bulk-sintered silver were fabricated using different starting silver pastes and different sintering conditions to promote different amounts of porosity. Test coupons were harvested out of the disks to measure electrical resistivity and electrical conductivity, thermal conductivity, coefficient of thermal expansion, elastic modulus, Poisson's ratio, and yield stress. The authors fully recognize that the microstructure of processed bulk silver coupons may indeed not be identical to the microstructure produced in thin (20-50 microns) layers of sintered silver. However, measuring these same properties with such a thin actual structure is very difficult, requires very specialized specimen preparation and unique testing instrumentation, is expensive, and has experimental shortfalls of its own, so the authors concluded that the herein measured responses using processed bulk sintered silver coupons would be sufficient to determine acceptable values of those properties. Almost all the investigated properties of bulk sintered silver changed with porosity content within a range of 3-38% porosity. Electrical resistivity, electrical conductivity, thermal conductivity, elastic modulus, Poisson's ratio, and yield stress all depended on the porosity content in bulk-sintered silver. The only investigated property that was independent of porosity in that range was coefficient of thermal expansion.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical Characterization Study of Sintered Silver Pastes: Preprint

Sintered silver-based bonded interfaces are a critical enabling technology for high-temperature, compact, high-performance, and reliable wide-bandgap packages and components. High-pressure (about 40 MPa) sintered silver interfaces have been implemented commercially, most notably the commercial products offered by Semikron. To reduce manufacturing complexity, there is significant industry interest in pressure-less sintered silver interfaces. To this end, current formulations of sintered silver paste are comprised of purely nano-sized silver particles or a combination of nano- and micro-sized silver particles/flakes. It is essential to quantify the mechanical properties and determine the reliability of these interfaces prior to use in automotive power electronics applications. In this paper, research efforts at the National Renewable Energy Laboratory, in collaboration with Virginia Polytechnic Institute and State University and an industry partner, in optimizing the synthesis procedure and mechanical characterization of sintered silver double-lap samples are described. These double-lap samples were synthesized using pressure-less sintering techniques. Shear testing was conducted at multiple temperatures and displacement rates on these samples sintered using two types of sintered silver pastes, one of them consisting of nano-silver particles and the other a hybrid paste or a combination of nano- and micron-sized silver flakes, employed in a double-lap configuration. Maximum values of shear stress obtained from the characterization study are reported.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2021

Controlled current-rate AC flash sintering of uranium dioxide

Uranium dioxide (UO2) pellets with controlled microstructures were densified up to 93.4% of their theoretical density in less than 25 minutes at a furnace temperature of 873 K, utilizing controlled current-rate alternating current (AC) flash sintering (FS). Using this AC-FS method it was possible to control the sintering rate and thermal gradients, resulting in dense pellets with no appreciable hourglassing and good mechanical integrity. Moreover, the apparent sintering activation energy for FS and for conventionally sintered samples was estimated to be 108 kJ mol -1 and 380 kJ mol -1 , respectively using the master sintering curve method. The apparent activation energy for FS was remarkably close to those reported in the literature for spark plasma sintering of UO 2 . Furthermore, both these field assisted sintering methods utilize fast heating rates and electrical effects that are likely enhancing the grain boundary diffusion mechanism. Finally controlled current-rate AC-FS has been demonstrated as a technological advancement, capable of producing ceramic nuclear fuels in a fraction of the conventional processing time.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidation of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In-operando synchrotron experiments of flash sintering carried out in current rate mode

Here, we report first-time results for in-operando flash sintering synchrotron experiments carried out in current rate mode where the specimen, held at a constant temperature, is fed current that is increased at a constant rate. These experiments are unique because the time dependence of the sintering behavior can be stretched out over a longer period (by changing the current rate) than in voltage-to-current experiments in which sintering occurs in a burst at the onset of the flash. Two results are presented: (i) A comparison of temperatures measured with the platinum standard to those predicted by the black body radiation model leading to estimates of the emissivity as a function of porosity whereby emissivity increases from 0.65 to 0.9 as the sample sinters from its green state to full density, and (ii) measurements of the excess lattice expansion as a function of density as the sample sinters continuously while the current is increased. The present work highlights the promise of current rate experiments to obtain results while the sample sinters gradually from its green density to full density (somewhat akin to conventional sintering) for gaining further insights into the mechanisms of flash sintering.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Development of Binder Jet Compatible Silicon Carbide Mixtures for Increased Sintered Density

Binder jet additive manufacturing can process a variety of ceramic powder feedstocks to manufacture near net shape green parts that are subsequently sintered to achieve densification. In particular, silicon carbide (SiC) is a promising ceramic material for heat exchangers in energy storage applications and binder jet is a well-suited process for manufacturing these heat exchangers due to the often geometrically complex designs. However, the need for good powder flowability in binder jet printing often limits the feedstock powder to be larger particles rather than that of ultra fine submicron powders used in conventional ceramic processing, which are more readily densified during sintering. The present work explores the use of various powder mixtures and sintering settings to identify strategies for achieving high density sintered parts in binder jet compatible systems without the use of infiltration. Liquid-phase sintering additives and bimodal powder mixtures are explored alongside different sintering temperatures, rates, atmospheres, and hold times. Two mixtures were found to be good candidates for further exploration: 1) 90 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 mixture achieved the highest sintered relative density of 91.2%; and 2) a bimodal mixture comprised of 45 wt% 10 µm SiC + 45 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 had the best powder flowability of the powders measured and a 75.1% sintered relative density.

25 ENERGY STORAGE↗
DOE OSTI2023

Rapid Laser Reactive Sintering of Garnet Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 and Li 6.1 La 3 Zr 2 Al 0.3 O 12 and Solid-State Electrolytes

All solid-state lithium-ion batteries (ASSLIBs) have gained significant interest in recent years due to their wide range of applications, including mobile devices, electric vehicles, and grid storage. Garnet-type Li 7 La 3 Zr 2 O 12 (LLZO) solid-state electrolyte (SSE) continues to be a significant player in the fabrication of ASSLIBs with excellent ionic conductivity on the order of 10 -3 S•cm -1 with the integration of dopants and sintering aids to assist conductivity and structural evolution during the sintering procedure. Traditional sintering techniques, such as solid-state sintering (SSS), have been proven to yield desirable crystal structures. However, the low ionic conductivity results from inferior microstructure, and lithium loss is a significant challenge. Recently, a relatively novel sintering process called rapid laser sintering (RLS) has shown great potential for achieving fully dense solid oxide electrolytes with less lithium loss, resulting in high ionic conductivity [1] [2] [3] [4]. Here, we applied a modified RLS method using precursor powders instead of pre-synthesized LLZO powders to fabricate Al-doped LLZO (Li 6.1 La 3 Zr 2 Al 0.3 O 12 + 13 wt% Li 2 CO 3 ) and Ta-doped LLZO (Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 + 5 wt% LiOH•H 2 O) dense electrolytes. This rapid laser reactive sintering (RLRS) could potentially reduce the number of processing steps and therefore lower the manufacturing cost. We hope the rapid high-temperature sintering can densify the electrolyte and avoid the lithium loss for achieving high lithium-ion conductivity. In this work, we optimized a combination of laser parameters (speed and power), initial precursor composition, and controlled atmospheres to discover the optimal conditions for reaching the efficacious crystal structure, microstructure, and ionic conductivity.

25 ENERGY STORAGE↗
DOE OSTI2019

Development of Multilayer Sinter Cladding of Cold Work Tool Steel on Hadfield Steel Plates for Wear-Resistant Applications

Machinery components used for mining and mineral processing activities are often subjected to high impact loads and wear which have placed demands for the development of materials with high resistance to dynamic loads and aggressive wear conditions. In this study, a multilayered cladding of high alloyed cold work tool steel (X245VCrMo9-4), interlayered with Hadfield steel (X120Mn12) plates, which was also used as substrate using super-solidus liquid-phase sintering technique was investigated. A stack of the cold work tool steel powder was prepared with interlayered X120Mn12 steel plates in an alumina crucible at tap density with the substrate placed on it and was sintered in a vacuum furnace at 1250 °C at a heating rate of 10 K/min, held for 30 min under a nitrogen atmosphere at 0.08 MPa and furnace-cooled. Sample from the as-sintered cladding was subjected to austenization at 1000 °C, quenched in oil and tempered at 150 °C for 2 h. Samples were subjected to microstructural examination using optical and scanning electron microscopy. The microstructural investigations were supplemented by hardness and impact wear tests. Computational thermodynamics was used to support experimental findings. The results revealed that a near-net densification of the sintered X245 was achieved with 99.93 ± 0.01% density. The sintered X245 was characterized by a dispersion of vanadium carbonitride precipitates, especially at the grain boundaries. The heat-treated X245 sample had the highest hardness of 680 ± 7 HV30 due to the matrix of tempered martensitic microstructure when compared to as-sintered with hardness of 554 ± 2 HV30. The X245/X120 interface was characterized by diffusion of Cr, Mo, Mn and C, which resulted in metallurgical bonding between the cladded materials. The impact wear resistance of the sintered X245 was eight times that of the X120; hence, a tough and wear-resistant tool is anticipated when the X120 work hardened in service.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of processing conditions on microstructural features in Mn–Si sintered steels

Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain boundaries by oxide inclusions • Reducing agents efficient at low temperatures critical for avoiding oxide inclusions.

36 MATERIALS SCIENCE↗