Study of color change and microstructure development of Al2O3–Cr2O3/Cr3C2 nanocomposites prepared by spark plasma sintering

The densification behaviors of Al₂O₃–Cr₂O₃/Cr₃C₂ nanocomposites prepared by a Spark Plasma Sintering (SPS) were investigated in this work. The initial powders used for sintering were Al₂O₃–Cr₂O₃, which were prepared by metal organic chemical vapor deposition (MOCVD) in a spout bed. Different colors of the compacts such as green, purple and black were observed after densification process at different SPS temperatures from 1200 °C to 1350 °C. These changes of color were relevant to the existence of secondary phase of green Cr₂O₃, pink solid solution of Cr₂O₃–Al₂O₃ and black Cr₃C₂, which were formed under the different SPS temperature. The secondary phase of Cr₂O₃ retarded the processing of densification for spark plasma sintering at 1200 °C. The Cr₂O₃ reacted with Al₂O₃ to form solid solution of Cr₂O₃–Al₂O₃ and with carbon to form Cr₃C₂ as sintering temperature increased to 1350 °C. The characteristics of high heating rate, shorter sintering time for SPS and the formation of secondary phase of Cr₃C₂ effectively reduced the substrate's grain growth, making Al₂O₃–Cr₂O₃/Cr₃C₂ nanocomposites with small grain size.     

Toughening of MgAl2O4 spinel/ Si3N4 nanocomposite fabricated by spark plasma sintering

The main objective of this work is to compare the hardness, fracture toughness, and optical transparency of MgAl₂O₄ spinel (magnesium aluminate), MgAl₂O₄ spinel/ Si₃N₄ nanocomposite, and the heat-treated spinel/Si₃N₄ nanocomposite. For this purpose, the commercial spinel nanopowder and the laboratory-made spinel/ Si₃N₄ nanocomposite powder were sintered using spark plasma sintering (SPS). A heat treatment at 1000?°C for 4?h was carried out on the as-sintered nanocomposite. The field emission scanning electron microscopy (FESEM), Energy dispersive X-ray (EDX) mapping, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Nanoindentation, and Vickers microhardness analyses were used to determine microstructure, elemental analysis, functional group, hardness, and indentation toughness of the samples. The results showed that the hardness and toughness of the heat-treated sample are more than those of the as-SPSed nanocomposite as much as 15.7% and 25.7%, respectively. Also, the values of optical transmission of the nanocomposite sample in the visible range (400–800?nm) and infrared region (800–2000?nm) were lower than those of pure spinel.     

Fine-grained transparent MgAl2O4 spinel obtained by spark plasma sintering of commercially available nanopowders

A high transmittance/small grain size combination for pure spinel ceramics from commercially available nanopowders without sintering aids can be obtained by SPS sintering. By using a low heating rate ≤10 °C/min and a sintering temperature ≤1300 °C, a transparent polycrystalline MgAl₂O₄ spinel was fabricated by SPS with an in-line transmission of 74% and 84% for 550 nm (visible) and 2000 nm (NIR) wavelengths respectively. A small average grain size of about 250 nm was obtained and the pores located at the multiple grain junctions have a mean size of about 20 nm. The high in-line transmission is linked not only to the low residual porosity but particularly to the very small size of pores.     

Mechanical properties of Al2O3-Cr2O3/Cr3C2 nanocomposite fabricated by spark plasma sintering

The fine grains of Al₂O₃-Cr₂O₃/Cr-carbide nanocomposites were prepared by employing recently developed spark plasma sintering (SPS) technique. The initial materials were fabricated by a metal organic chemical vapor deposition (MOCVD) process, in which Cr(CO)₆ was used as a precursor and Al₂O₃ powders as matrix in a spouted chamber. The basic mechanical properties like hardness, fracture strength and toughness, and the nanoindentation characterization of nanocomposites such as Elastics modulus (E), elastic work (W_e) and plastic work (W_p) were analyzed. The microstructure of dislocation, transgranular and step-wise fracture surface were observed in the nanocomposites. The nanocomposites show fracture toughness of (4.8 MPa m^1/2) and facture strength (780 MPa), which is higher than monolithic alumina. The strengthening mechanism from the secondary phase and solid solution are also discussed in the present work. Nanoindentation characterization further illustrates the strengthening of nanocomposites.     

Preparation mullite/Si3N4 composites by reaction spark plasma sintering and their characterization

In the present study, in-situ mullite/Si₃N₄ composites were prepared successfully by reaction spark plasma sintering. For this purpose, 5, 10 and 15?wt% of Si₃N₄ were added to stoichiometric mullite made of mechanically milled mixture of alumina and kaolin clay to investigate the effect of reinforcement content on the final properties of the prepared composites. The sintering processes were performed at 1400?°C under the initial and final applied pressures of 10 and 30?MPa and the vacuum condition of 17?Pa. The XRD patterns revealed the mullite and Si₃N₄ peaks as the dominant crystalline phases. Microstructural investigations demonstrated a uniform distribution of Si₃N₄ inside mullite matrix for the composites containing 5 and 10?wt% of the reinforcement particles. Meanwhile, some agglomerates of Si₃N₄ were observed in the microstructure of the mullite-15?wt%Si₃N₄ composite. Moreover, no evidence of reaction between the starting materials was detected through XRD and FESEM analyses. The highest values of hardness, bending strength, and fracture toughness obtained for the composite containing 15?wt% of Si₃N₄ were 19.14?GPa, 481?MPa and 3.85?MPa?m^?1/2, respectively. The fracture toughness mechanisms were detected as crack branching, breaking and deflection, as well as particles pulling-out, all of which were observed in the mullite-15?wt%Si₃N₄ composite.     

The effect of Al2O3-MgO additives on the microstructure of spark plasma sintered silicon nitride

It was shown that spark plasma sintered silicon nitride with a high content of Al₂O₃ and MgO consists of α and β silicon nitride, the main phase being α silicon nitride. The increase in the sintering temperature did not lead to significant changes in the phase composition as occurs in silicon nitride added with Al₂O₃-Y₂O₃. It was found that increasing in SPS temperature above 1650 °C leads to an insignificant increase in the density. A complex shaped equiaxed grain microstructure was shown in both cases. However, doping with aluminum and yttrium oxides allows obtaining an elongated grain microstructure. The Hall-Petch effect was observed for the microhardness of the investigated SPSed silicon nitride. The microhardness of the described ceramics was rather high and more than 1900 HV compared to the pressureless sintered at 1800 °C silicon nitride with the microhardness equal to 1511 HV.     

Synthesis, spark plasma sintering and electrical conduction mechanism in BaTiO3-Cu composites

BaTiO₃-Cu composite powders were prepared via an alkoxide-mediated synthesis approach. As-synthesized BaTiO₃ nanoparticles were as small as 40 nm and coated partially larger Cu particles of approximately 1 μm in size. Thermogravimetric analysis (TGA) and dilatometry revealed a gradual increase in weight loss and retarded shrinkage with the increase of Cu addition. BaTiO₃-Cu composites were successfully densified by spark plasma sintering (SPS). The microstructures show an average grain-size for BaTiO₃ of around 100 nm and a crystallite size of about 1 μm for the Cu inclusions. The AC conductivity of the BaTiO₃-Cu composites increased with increasing Cu content or with temperature. The dominant electrical conduction mechanism in SPSed BaTiO₃-Cu composites changed from migration of oxygen vacancies to band conduction of trapped electrons in oxygen vacancies with the increase of Cu content.     

Joining of C/SiC composites by spark plasma sintering technique

CVD–SiC coated C/SiC composites (C/SiC) were joined by spark plasma sintering (SPS) by direct bonding with and without the aid of joining materials. A calcia-alumina based glass–ceramic (CA), a SiC + 5 wt% B₄C mixture and pure Ti foils were used as joining materials in the non-direct bonding processes. Morphological and compositional analyses were performed on each joined sample. The shear strength of joined C/SiC was measured by a single lap test and found comparable to that of C/SiC.     

Microstructure and properties of Al2O3-TiC-Ti3SiC2 composites fabricated by spark plasma sintering

Abstract

Abstract

Highly densified Al₂O₃-TiC-Ti₃SiC₂ composites were fabricated by spark plasma sintering technique and subsequently characterised. From fracture surface observation, it is found that Al₂O₃ is 0·2-0·4?μm, TiC is 1-1·5?μm and Ti₃SiC₂ is 1·5-5?μm in grain size. With the increase in Ti₃SiC₂ volume contents, Vickers hardness of the composites decreases because of the low hardness of monolithic Ti₃SiC₂. The fracture toughness rises remarkably when the contents of Ti₃SiC₂ increase, which is attributed to the pullout and microplastic deformation of Ti₃SiC₂ grains. At the same time, the flexural strength of the composites shows a considerable improvement as well. The electrical conductivity rises significantly as the Ti₃SiC₂ contents increase because of the formation of Ti₃SiC₂ network and the increase in conductive phase contents.     

Effects of ball milling and post-annealing on the transparency of spark plasma sintered Lu2O3

The effects of ball milling of starting powder and post-annealing of spark plasma sintered (SPSed) Lu₂O₃ on its microstructure and optical property were investigated. When ball-milled powder was used, the SPSed Lu₂O₃ was found to have a larger grain size with wider distribution and lower transparency than in the case using powder without ball milling. After annealing at 1323 K in air, the Lu₂O₃ that was SPSed using ball-milled powder became colorless, had a higher transmittance in the visible spectrum than the case where as-received powder was used, and exhibited transmittances of 71.4% and 81.6% for wavelengths of 550 and 2000 nm, respectively.     

LZS/Al2O3 nanostructured composites obtained by colloidal processing and spark plasma sintering

Li₂O-SiO₂-ZrO₂ (LZS) glass-ceramics have high mechanical strength, hardness, resistance to abrasion and chemical attack, but also a high coefficient of thermal expansion (CTE), which can be reduced adding alumina nanoparticles. The conventional glass-ceramic production is relatively complex and energy consuming, since it requires the melting of the raw materials to form a glass frit and a two-step milling process to obtain particle sizes adequate for compaction. This study describes the preparation of LZS glass-ceramics through a colloidal processing approach from mixtures of SiO₂ and ZrO₂ nanopowders and a Li precursor (lithium acetate obtained by reaction of the carbonate with acetic acid). Concentrated suspensions were freeze-dried to obtain homogeneous mixtures of powders that were pressed (100 MPa) and sintered conventionally and by spark plasma sintering. The effect of the alumina nanoparticles additions on suspensions rheology, sintering behavior and properties such as thermal expansion, thermal conductivity, hardness and Young’s modulus were evaluated.     

Mechanical properties and microstructures of TiCN/nano-TiB2/TiN cermets prepared by spark plasma sintering

The effects of TiN and nano-TiB₂ additions to titanium carbonitride (TiCN-WC-Cr₃C₂-Co)-based cermets processed by spark plasma sintering (SPS) are identified. The TiN and nano-TiB₂ additions were varied from 0 to 15?wt% to ascertain their combined effects on the mechanical properties. Scanning electron microscopy (SEM) revealed the combined chemical composition of the new phases formed during sintering. The hardness and fracture toughness values were recorded. Increase in the fracture toughness value with TiN addition was more compared with the nano-TiB₂ addition. In contrast, the hardness values were higher for the cermets formed with the nano-TiB₂ addition. Sintered bodies were made as tool inserts that meet SNGN120408 standard tool configuration. Using these tools, EN24 work-piece was turned at different cutting speeds of 11.87, 29.68, 71.46, 163.88?m/min under conditions of dry cutting. The performance was evaluated. Cutting force as well as surface roughness of the work-piece after machining was measured. For all cutting tools, initially the cutting force was high but it tended to decrease at higher cutting speeds. In addition, for all the tools, at higher cutting tools the surface roughness values were uniformly minimal. The cermet with a composition 55TiCN-15WC-10Co-5Cr₃C₂–15nanoTiB₂ (all in wt%), in particular, showed a balanced enhancement in both fracture toughness (6.8?MPa?m^1/2) and Vickers hardness (18?GPa) values. The surface finish of the work-piece was also the best after machining when a tool of the above composition was used.     

Synthesis,microstructure and property characterization of Mo4Y2Al3B6 ceramic fabricated by spark plasma sintering

Polycrystalline Mo₄Y₂Al₃B₆ ceramic (92.84 wt% Mo₄Y₂Al₃B₆ and 7.16 wt% MoB) was prepared by spark plasma sintering at 1250 ℃ under 30 MPa using Mo, Y, Al, and B as starting materials. The dense sample obtained has a high relative density of 96.6 %. The average thermal expansion coefficient is 8.38 × 10^?6 K^?1 in the range of 25–1000 ℃. The thermal diffusivity decreases from 6.50 mm²/s at 25 °C to 4.33 mm²/s at 800 °C. The heat capacity, thermal conductivity, and electrical conductivity are 0.30 J·g^?1·K^?1, 11.73 W·m^?1·K^?1, and 0.66 × 10⁶ Ω^?1·m^?1 at 25 °C, respectively. Vickers hardness with increasing load in the range of 10–300 N at room temperature decreases from 10.82 to 9.49 GPa, and the fracture toughness, compressive strength, and flexural strength are 5.14 MPa·m^1/2, 1255.14 MPa, and 384.82 MPa, respectively, showing the promising applications as structural-functional ceramics.     

The effect of slip casting and spark plasma sintering (SPS) temperature on the transparency of MgAl2O4 spinel

MgAl₂O₄ bulk samples were fabricated by two different approaches to investigate the effect of slip casting and sintering temperature on their transparency. Three MgAl₂O₄ samples containing 1 wt% LiF, as the sintering aid, were prepared by the spark plasma sintering process (SPS) at 1400 °C and 1500 °C, under 100 MPa, for 15 min. Also, another MgAl₂O₄ sample was prepared by slip casting followed by SPS under similar conditions. It was observed that utilizing slip casting led to more transparency (10% in the visible region and 20% in the IR region) due to the more homogeneous structure. It was also observed that by reducing the SPS temperature from 1500 °C to 1400 °C, the transparency increased (20% in the IR region) because of the lower grain growth rate at the lower temperature.     

Densification,microstructure and properties of ultra-high temperature HfB2 ceramics by the spark plasma sintering without any additives

Ultra-high temperature HfB₂ ceramic with nearly full densification is achieved by using gradient sintering process of SPS without any additives. The effect of the sintering temperature on the densification behavior, relative density, microstructure, mechanical and thermionic properties is systematically investigated. The results show that the fast densification of HfB₂ ceramic occurs at the heating stage, and the highest relative density of 96.75% is obtained at T =1950 °C, P = 60 MPa and t =10min. As the temperature is increased from 1800 to 1950 °C, the grain size of HfB₂ increases from 6.12 ±1.33 to 10.99 ± 2.25 μm, and refined microstructure gives the excellently mechanical properties. The highest hardness of 26.34 ±2.1GPa, fracture toughness of 7.12 ± 1.33 MPa m^1/2 and bending strength of 501 ±10MPa belong to the HfB₂ ceramic obtained at T =1950°C. Moreover, both the Vickers hardness and fracture toughness obey the normal indentation size effect. HfB₂ ceramic also exhibits the thermionic emission characterization with the highest current density of 6.12 A/cm² and the lowest work function of 2.92 eV.     

Improvement of Vickers hardness measurement on SWNT/Al2O3 composites consolidated by spark plasma sintering

Dense alumina composites with different carbon nanotube content were prepared by colloidal processing and consolidated by Spark Plasma Sintering (SPS). Single-wall carbon nanotubes (SWNTs) were distributed at grain boundaries and also into agglomerates homogeneously dispersed. Carrying out Vickers hardness tests on the cross-section surfaces instead of top (or bottom) surfaces has shown a noticeable increase in the reliability of the hardness measurements. This improvement has been mainly attributed to the different morphology of carbon nanotube agglomerates, which however does not seem to affect the Vickers hardness value. Composites with lower SWNT content maintain the Vickers hardness of monolithic alumina, whereas it significantly decreases for the rest of compositions. The decreasing trend with increasing SWNT content has been explained by the presence of higher SWNT quantities at grain boundaries. Based on the results obtained, a method for optimizing Vickers hardness tests performance on SWNT/Al₂O₃ composites sintered by SPS is proposed.     

Graphene nanosheets toughened TiB2-based ceramic tool material by spark plasma sintering

One kind of TiB₂/TiC composite ceramic tool material toughened by graphene nanosheets was fabricated by spark plasma sintering. Effects of graphene nanosheets on microstructure, mechanical properties and toughening mechanisms were investigated. The results indicated that TiB₂/TiC with 0.1?wt% graphene nanosheets sintered at 1800?°C with the holding time of 5?min obtained full densification and optimal mechanical properties. Its fracture toughness and Vickers hardness were 7.9?±?1.2?MPa?m^1/2 and 20.0?±?0.7?GPa, respectively. Excess graphene nanosheets had no effects to toughness improvement. Fracture toughness was increased by 31.7% in comparison with the TiB₂/TiC without graphene nanosheets. Toughness enhancement mainly benefited from crack bridging, also slip-stick effect of graphene made it hard to detach and effectively restrained crack extension.     

Interface reaction of U3Si2-UO2 composite pellets during spark plasma sintering

U₃Si₂-UO₂ composite fuel combines the advantages of high uranium density and thermal conductivity of U₃Si₂ and excellent stability of UO₂ under light water reactor (LWR) condition. Since commercialized pressureless sintering of UO₂ is usually performed above the melting point of U₃Si₂, spark plasma sintering (SPS) is considered as a convenient method to produce U₃Si₂-UO₂ composite fuel. However, the potential interaction between U₃Si₂ and UO₂, an important aspect for composite materials, has not been sufficiently investigated. In this report, U₃Si₂-UO₂ pellets with 1:1 wt ratio were fabricated by SPS. Next, the interaction between U₃Si₂ and UO₂ during the sintering process was examined with X-ray diffraction (XRD), optical microscopy (OM), scanning electron microscope (SEM), and transmission electron microscope (TEM). The results show that U₃Si₂ and UO₂ reacted to yield USi as the main product. The reaction occurred at a relatively low temperature of 1100 °C, at which the composite fuel was less than 90% theoretical density (TD).     

Densification, microstructure and mechanical properties of SiO2-cBN composites by spark plasma sintering

SiO₂-cBN composites were consolidated by spark plasma sintering at 1473-1973 K. The effects of cBN content and sintering temperature on the relative density, phase transformation, microstructure and mechanical properties of the SiO₂-cBN composites were investigated. The relative density of the SiO₂-cBN composites increased with increasing SiO₂ content. The phase transformation of cBN to hBN in SiO₂-cBN composites was identified at 1973 K, showing the highest transformation temperature in cBN-containing composites. The SiO₂-20 vol% cBN composites sintered at 1673 K showed the highest hardness and fracture toughness of 12.5 GPa and 1.5 MPa m^1/2, respectively.     

Spark plasma sintering of Al2O3-cBN composites facilitated by Ni nanoparticle precipitation on cBN powder by rotary chemical vapor deposition

Al₂O₃-cBN/Ni composites were consolidated by spark plasma sintering (SPS) using α-Al₂O₃ and Ni nanoparticle precipitated cBN (cBN/Ni) powders. The Ni nanoparticles, 10-100 nm in diameter and 0.5-2.2 mass% in content, were precipitated on cBN powder by rotary chemical vapor deposition. The effect of sintering temperature (T_SPS) and Ni content (C_Ni) on the densification, phase transformation, microstructure and hardness of the Al₂O₃-cBN/Ni composites were investigated. The highest relative density of Al₂O₃-30 vol% cBN composite was 99% at T_SPS = 1573 K and C_Ni = 1.7 mass%. At T_SPS = 1673 K, the relative density decreased due to the phase transformation of cBN to hBN. The Vickers hardness of Al₂O₃-30 vol% cBN/Ni at T_SPS = 1573 K and C_Ni = 1.7 mass% showed the highest value of 27 GPa.