Microstructure and thermal conductivity of spark plasma sintering AlN ceramics

Abstract

Dense aluminium nitride ceramics were prepared by spark plasma sintering at a lower sintering temperature of 1700°C with Y₂O₃, Sm₂O₃ and Dy₂O₃ as sintering additives respectively. The effects of three kinds of sintering additives on the phase composition, microstructure and thermal conductivity of AlN ceramics were investigated. The results showed that those sintering additives not only facilitated the densification via the liquid phase sintering mechanism, but also improved thermal conductivity by decreasing oxygen impurity. Sm₂O₃ could effectively improve thermal conductivity of AlN ceramics compared with Y₂O₃ and Dy₂O₃. Observation by scanning electron microscopy showed that AlN ceramics prepared by spark plasma sintering method manifested quite homogeneous microstructures, but AlN grain sizes and shapes and location of secondary phases varied with the sintering additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of secondary phases.     

Microstructure and mechanical properties of spark plasma sintered austenitic ODS steel

In this work, austenitic oxide dispersion strengthened (AODS) steel of composition Fe–16Cr–16Ni–1.5 W–0.21Ti–0.3Y₂O₃ (wt. %) was fabricated using two–stage ball milling followed by consolidation through spark plasma sintering (SPS). In the first–stage, mechanical alloying (MA) of ferritic powder and nano sized Y₂O₃ was carried out. This was followed by the addition of Ni in second–stage milling. SPS of the milled powder was carried out at 900, 950, 1000 and 1050 °C to explore the role of SPS temperature on density, microstructure as well as mechanical properties of the consolidated samples. A relative density of ～ 99% was obtained for samples sintered at 950 and 1000 °C. The as–sintered samples were subsequently solution annealed at 1075 °C for 2 h and water quenched. X–ray diffraction studies confirmed the presence of austenite in the consolidated and solution annealed samples. Electron back scatter diffraction analysis of solution annealed samples sintered at all the temperatures revealed a bimodal microstructure. The average grain size of 1.07 ± 0.72 µm was obtained for solution annealed samples sintered at 1000 °C. Yield strength and elongation of the same was measured as 851 MPa and 18%, respectively at room temperature. These values are the best combination of strength to elongation achieved on AODS alloys processed using MA and SPS, which makes this AODS steel much promising for high temperature applications.     

放电等离子烧结制备透明AlN陶瓷

采用放电等离子烧结(spark plasma sintering,SPS)技术,添加不同含量CaF2为烧结助剂,成功制备了透明氮化铝(AlN)陶瓷.SPS技术具有烧结快速,烧结体致密度高的特点,是制备透明AlN的有效方法.CaF2的加入量的提高,有利于烧结体的致密度和透过率的提高.当CaF2加入量为3%(质量分数)时,烧结体致密度不再继续提高,但仍有利于透过率的提高,此时烧结体透过率最高为54.7%.SEM、XRD、TEM和EDX结果表明烧结体具有很高的致密度、纯度,均匀的晶粒形状和尺寸,晶界及三角晶界处观察不到第二相的存在,从而保证了烧结体良好的光学性能.     

Microstructure and wear properties of spark plasma sintered 316L-30W composites

ABSTRACT

316L-30W composites were successfully fabricated via spark plasma sintering at 1550°C to evaluate their potential as the interlayer between W and 316L stainless steel in fusion reactors. The effect of holding time on the microstructure and its subsequent effects on the fracture morphology and wear properties of the composites were investigated. The results show that more W particles melted and reacted with 316L steel as the holding time increased from 1 to 5 min. The generation of voids was mainly caused by the differences in diffusivity and the coefficient of thermal expansion between W and 316L. The 316L-30W composite held for 3 min had a smaller and more stable friction coefficient, indicating that its interface was firmly bonded and homogeneous.

This paper is part of a thematic issue on Nuclear Materials.     

Microstructure and mechanical properties of BAS/SiC composites sintered by spark plasma sintering

High-density BAS/SiC composites were obtained from β-SiC starting powder by the spark plasma sintering technique. Various physical properties of the BAS/SiC composites were investigated in detail, such as densification, phase analysis, microstructures and mechanical properties. The results demonstrated that the relative density of the BAS/SiC composites reached over 99.4% at 1900 °C. The SiC grains were uniformly distributed in the continuous BAS matrix which is probably because of complete infiltration of the SiC particles in BAS liquid-phase formed during sintering. The pull-out of SiC particles, crack deflection and bridging were observed as the major toughening mechanism. The flexural strength and fracture toughness of the BAS/SiC composites sintered at 1900 °C were up to 560 MPa and 7.0 MPa·m^1/2, respectively.     

Microstructure and mechanical properties of spark plasma sintered titanium‐added copper/reduced graphene oxide composites

Copper matrix composites were fabricated through mixing fixed amount of reduced graphene oxide and the different amounts of titanium. The dried copper/titanium/reduced graphene oxide mixture powders were firstly obtained by the wet‐mixing process, and then the spark plasma sintering process realized their faster densification. In the as‐sintered bulk composites, the layered reduced graphene oxide network, uniform titanium particles and copper‐titanium solid solution are observed in copper matrix. Investigations on mechanical properties show that the as‐prepared bulk composites exhibit the hardness and compressive yield strength compared with single reduced graphene oxide added composites. Increased titanium addition resulted into higher hardness and strength. The relevant formation and failure mechanisms of the composites and their influence on mechanical properties were discussed.     

Physicomechanical properties of spark plasma sintered carbon nanotube-reinforced metal matrix nanocomposites

The technological and industrial needs for development of fully dense nanocomposites have led to significant advances in spark plasma sintering (SPS) technique and its enhanced forms. This technique has opened up a new prospect over carbon nanotube (CNT)-metal matrix nanocomposites (MMNCs) with superior physical or mechanical characteristics. To date, a large number of authentic papers have been published over this ongoing field, but have not been comprehensively reviewed. The pertinent research works cover some significant aspects of CNT-MMNCs requiring a concise review on (i) the potential phase transformations of pure CNTs and microstructure evolution; (ii) the novel approaches for uniform dispersion of CNTs inside the metallic matrices including Cu, Al, Ag, Ni, Ti, Mg, and Fe; and (iii) recent improvements in mechanical, thermal, electrical, biological, and tribological properties of CNT-MMNCs. The present review paper strives to scrutinize the aforementioned topics and provide a broad overview of the unsolved challenges and suggested solutions for them.     

Functional properties of a spark plasma sintered ultrafine-grained 316L steel

A micrometric austenitic stainless steel 316L powder was densified by spark plasma sintering. The process parameters were varied over wide ranges and the impact of such variations on sintered materials was studied through the characterization of their microstructures, densities, hardness and corrosion resistance. For comparison with the properties of traditionally cast 316L, all these investigations were also systematically carried out on as cast samples. The sintered stainless steel produced this way was highly densified, with grains of a micrometric size and the forming process did not induce any residual strain gradients as shown by transmission electronic microscopy analysis. The investigation of the corresponding mechanical properties reveals an enhancement of hardness up to twice the value measured on one sample of as cast 316L. This result is in good agreement with the Hall–Petch formalism. Additionally, in the matter of corrosion behavior, fully dense samples display an enhanced passive state in chloride media compared to as cast material. Spark plasma sintering appears to be an interesting alternative elaboration way of ultrafine 316L stainless steel giving materials with high stress resistance, without strain gradients through the volume, and promising functional properties concerning corrosion behavior.     

Mechanical properties and microstructure of spark plasma sintered nanostructured p-type SiGe thermoelectric alloys

SiGe based thermoelectric (TE) materials have been employed for the past four decades for power generation in radio-isotope thermoelectric generators (RTG). Recently “nanostructuring” has resulted in significantly increasing the figure-of-merit (ZT) of both n and p-type of SiGe and thus nanostructured Si₈₀Ge₂₀ alloys are evolving as a potential replacement for their conventional bulk counterparts in designing efficient RTGs. However, apart from ZT, their mechanical properties are equally important for the long term reliability of their TE modules. Thus, we report the mechanical properties of p-type nanostructured Si₈₀Ge₂₀ alloys, which were synthesized employing spark plasma sintering of mechanically alloyed nanopowders of its constituent elements with 1.2% boron doping. Nanostructured p-type Si₈₀Ge₂₀ alloys exhibited a hardness of ~ 9 ± 0.1 GPa, an elastic modulus of ~ 135 ± 1.9 GPa, a compressive strength of 108 ± 0.2 MPa, and fracture toughness of ~ 1.66 ± 0.04 MPa√m with a thermal shock resistance value of 391 ± 21 Wm^− 1. This combination of good mechanical properties coupled with higher reported ZT of nanostructured p-type Si₈₀Ge₂₀ alloys are rendered to be a potential material for power generation applications, compared to its bulk counterpart.     

Excellent mechanical properties and large magnetocaloric effect of spark plasma sintered Ni-Mn-In-Co alloy

The Ni43.75Mn37.5In12.5Co6.25 alloy was obtained by using the spark plasma sintering (SPS) technique.The martensitic transformation,magnetic and mechanical properties of the SPS alloy were investigated.Key findings demonstrate that the martensitic transformation temperature of this alloy is about 10 K lower than that of the as-cast one.Both SPS and as-cast alloys show a 7 layered modulated martensite (7M) at room temperature.The compressive fracture strength and strain of the SPS alloy increase by 176.92％ and 33.33％ compared with the as-cast alloy,achieving 1440 MPa and 14％,respectively.The maximum magnetic entropy change △Sm is 17.1 J kg-1 K-1 for the SPS alloy at the magnetic field of 5 T.     

Microstructure and properties of Nd-Fe-B magnets prepared by spark plasma sintering

Abstract

Anisotropic Nd₁₅.₅Dy₁.₀Fe_BalCo₃.₀B₆.₈Al₁.₀ magnets were produced by the spark plasma sintering (SPS) technique. The effects of processing conditions on the microstructure, magnetic properties, dimensional precision and density of the magnets were studied. The magnetic properties, microstructure and constituents were investigated by means of a magnetic flux density - magnetic field strength (B-H) loopline instrument, scanning electron microscopy and energy dispersive X-ray analysis. The density of the magnets was determined by the Archimedes method, and the dimensional precision of the magnets was measured by micrometer. It was found that the microstructure of SPS processed Nd-Fe-B magnets is unique; the grain size is fine and uniform while distribution of the neodymium rich phase is heterogeneous. The optimal magnetic properties of SPS processed Nd-Fe-B magnets obtained so far are maximum energy product of 240 kJ m^-3 and coercive force of 1260 kA m^-1. The dimensional precision of the magnets is ~ 20 μm, and the density of the magnets reaches 7.58 g cm^-3.     

Effect of sintering temperature on microstructures and mechanical properties of spark plasma sintered nanocrystalline aluminum

Organic-coated aluminum nano-powders were consolidated by spark plasma sintering technique with low initial pressure of 1 MPa and high holding pressure of 300 MPa at different sintering temperature. The effect of sintering temperature on microstructures and mechanical properties of the compact bulks was investigated. The results indicate that both the density and the strain of the nanocrystalline aluminum increase with an increase in sintering temperature. However, the micro-hardness, compressive strength and tensile stress of the compact bulks increase initially and then decrease with increasing sintering temperature. The nanocrystalline aluminum sintered at 773 K has the highest micro-hardness of 3.06 GPa, the best compressive strength of 665 MPa and the supreme tensile stress of 282 MPa. A rapid grain growth of nanocrystalline aluminum sintered at 823 K leads to a decrease in micro-hardness, compressive strength and tensile stress. After annealing, a remarkable increase in strain and a slight rise in strength were obtained due to the relief of the residual stress in nanocrystalline Al and the formation of composite structure.     

Thermoelectric and mechanical properties of melt spun and spark plasma sintered n-type Yb- and Ba-filled skutterudites

Here we present thermoelectric and mechanical properties of n-type filled-skutterudites produced by a combination of melt spinning of pre-melted charges with subsequent consolidation by spark plasma sintering, a process we refer to as MS-SPS. This combination of processing steps leads to phase-pure n-type filled-skutterudites and obviates more energy and time intensive annealing steps. We show that both the thermoelectric properties and the tensile fracture strength compare favorably to materials made by traditional methods. The process is scalable to at least 80 g billets, such that the transport properties measured on test bars harvested from these larger billets compare favorably to those measured on lab-scale billets (5 g total billet mass). ZT values approaching 1.1 at 750 K were observed in materials made by MS-SPS. In addition, the tensile fracture strength of test bars cut from an 80 g billet is ∼128 MPa at room temperature and decreases with increasing temperature. Fractography of the test bars reveals that the majority failed due to surface and edge flaws with few failures due to volume type flaws. This indicates that the powder metallurgical methods employed to produce these samples is mature.     

放电等离子烧结(SPS)YAG陶瓷的初步研究

研究了采用放电等离子烧结(Spark Plasma Sintering SPS),利用高纯的氧化钇和氧化铝,在1500～1700℃,真空度优于10Pa,反应快速合成YAG陶瓷,但试样的致密度不高,而低气孔率是制备透明陶瓷的关键,实验表明,TEOS的掺加和粉料粒度的减小对烧结试样致密度的提高有一定的作用.     

Computational estimation of elastic properties of spark plasma sintered TaC by meshfree and finite element methods

In this study, the overall elastic modulus of spark plasma sintered TaC composite has been estimated using a novel engineering analysis technique, called Scan-and-Solve, that makes it possible to perform completely automated stress analysis directly from the segmented micrographs. The computed results have been compared with object oriented finite element technique (OOF), which also makes use of the microstructure. In contrast with the traditional mesh based engineering analysis methods, Scan-and-Solve uses spatial meshes that may or may not conform to the shape of the geometric model. This makes Scan-and-Solve computational technology essentially meshfree, and it makes it possible to eliminate error-prone and time consuming data conversion and spatial meshing. The presented method guarantees exact treatment of the prescribed boundary conditions. In the paper, we compare the stress simulation results in porous TaC ceramic obtained by the Scan-and-Solve and object oriented finite element methods. It is shown that the effective elastic modulus predicted from the microstructure by the two methods is very similar (266 vs. 270 GPa) provided the porosity coefficients are measured close to each other.     

Preparation and mechanical properties of laminated zirconium diboride/molybdenum composites sintered by spark plasma sintering

Laminated ZrB₂/Mo composites, alternately consisting of matrix layers of 80 vol.% ZrB₂ + 10 vol.% nano-SiC whiskers + 10 vol.% SiC particles and Mo interlayers, with the addition of Si and B as interlayer adjusting agent, were prepared by roll-compaction and spark plasma sintering (at 1600°C) process. XRD and SEM techniques were used to characterize the phases and microstructure of the obtained composites. The results showed that without the addition of Si and B in the interlayer, interfacial debonding between the matrix layer and interlayer often occurred due to the thermal mismatch between the two kinds of layers. However, the interfacial mismatch could be effectively inhibited by the addition of Si and B to the Mo interlayers. The laminated ZrB₂/Mo composites with 6 at.% Si and 4 at.% B in the interlayers showed the highest bending strength at (451±20) MPa and the highest fracture toughness at (7.52±0.12) MPa·m^?. MoB, ZrB and Mo5SiB2 were formed by the reactions among ZrB₂, Mo and the additions.     

Microstructure and mechanical properties of sintered glass

Glass microspheres have been sintered under argon in order to obtain sintered brittle bodies over a large range of density. During sintering, the microstructure evolves from a stacking of spheres to a body containing isolated pores. This evolution of the microstructure is described using image analysis and mathematical morphology. Mechanical properties are also investigated as a function of density. Special attention was paid to fracture toughness because, due to the isotropic behaviour of glass, internal stresses of the second order do not exist. A maximum ofG _IC is observed and it can be correlated with changes in the morphological parameters.     

Microstructure and elastic properties of sintered hydroxyapatite

The paper focuses on the dependence of microstructure and elastic properties of sintered hydroxyapatite on the processing parameters. Several specimens were sintered in conventional furnace at various temperatures. Elastic moduli were measured ultrasonically and information about the microstructure was recovered from these data and then verified by analysis of microphotographs. It was obtained that the average shape of pores becomes more round as the sintering temperature increases. That leads, in particular, to higher fracture toughness of the material since the stress concentration near pores is reduced.