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.     

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.     

Transparent polycrystalline MgO ceramic fabricated by low-temperature vacuum sintering with MgF2 additive

This study introduces transparent MgO ceramics produced via simply vacuum sintering at 1200–1500 °C by optimal incorporation of MgF₂ as a sintering additive. The effect of MgF₂ content and sintering temperature on the densification process, optical, and thermal properties of MgO ceramics is presented with emphasis on its function as a sintering aid and adverse effect of MgF₂ evaporation in the condition of high MgF₂ content or high sintering temperature. MgO ceramic with 1.0 mol% MgF₂ sintered at 1300 °C exhibits the highest relative density of 99.95% with average grain size of 17.46 μm. The in-line transmittance attains 60% at 1000 nm and >80% in the infrared range (3.8–6.8 μm), without absorption bands originated from the carbon contamination. The corresponding room-temperature thermal conductivity reaches 47.25 W/(m∙K). These results demonstrate that MgF₂ is an outstanding sintering additive for the preparation transparent MgO ceramics.     

Structural and optical properties of Tm:Y2O3 transparent ceramic with La2O3, ZrO2 as composite sintering aid

The paper reports the use of La₂O₃ and ZrO₂ co-doping as a composite sintering aid for the fabrication of Tm:Y₂O₃ transparent ceramics. Two groups of experiments were conducted for investigating the influences of composite sintering aids on the microstructures and the optical properties of Tm:Y₂O₃ transparent ceramics in contrast to single La³⁺ and single Zr⁴⁺ doped Tm:Y₂O₃. Samples with composite sintering aids could realize fine microstructures and good optical properties at relatively low sintering temperatures. Grain sizes around 10 μm and transmittances close to theoretical value at wavelength of 2 μm were achieved for the 9 at.% La³⁺, 3 at.% Zr⁴⁺ co-doped samples sintered at 1500-1600 °C. The influences of the composite sintering aids on the emission intensities and the phonon energies of Tm:Y₂O₃ ceramics were also investigated.     

Two-step pressure sintering of transparent lutetium oxide by spark plasma sintering

Transparent lutetium oxide (Lu₂O₃) body was prepared by spark plasma sintering using a two-step pressure profile combined with a low heating rate. The effects of pre-load pressures from 10 to 100 MPa and heating rates from 0.03 to 1.67 K s⁻¹ on the microstructures and optical properties were investigated. With increasing pre-load pressures from 10 to 100 MPa, the grains became smaller with a narrower distribution, whereas the transmittance showed maxima at 30 MPa. The average grain size slightly increased from 0.67 to 0.86 μm as the heating rate increased from 0.03 to 1.67 K s⁻¹, while the transmittance decreased. Transmittances of 60% at 550 nm and 79% at 2000 nm were obtained under a pre-load pressure of 30 MPa at a heating rate of 0.17 K s⁻¹.     

Corrosion mechanisms of Al2O3/MgAl2O4 by V2O5, NiO, Fe2O3 and vanadium slag

The effects of V₂O₅, NiO, Fe₂O₃ and vanadium slag on the corrosion of Al₂O₃ and MgAl₂O₄ have been investigated. The specimens of Al₂O₃ and MgAl₂O₄ with the respective oxides above mentioned were heated at 10 °C/min from room temperature up to three different temperatures: 1400, 1450 and 1500 °C. The corrosion mechanisms of each system were followed by XRD and SEM analyses. The results obtained showed that Al₂O₃ was less affected by the studied oxides than MgAl₂O₄. Alumina was only attacked by NiO forming NiAl₂O₄ spinel, while the MgAl₂O₄ spinel was attacked by V₂O₅ forming MgV₂O₆. It was also observed that Fe₂O₃ and Mg, Ni, V and Fe present in the vanadium slag diffused into Al₂O₃. On the other hand, the Fe₂O₃ and Ca, S, Si, Na, Mg, V and Fe diffused into the MgAl₂O₄ structure. Finally, the results obtained were compared with those predicted by the FactSage software.     

Transparent Er2O3 ceramics fabricated by high-pressure spark plasma sintering

Fabrication of transparent Er₂O₃ ceramics was carried out by high-pressure spark plasma sintering (HP-SPS). The color and in-line transmittance of these ceramics was highly sensitive to the sintering parameters. Samples exhibited a strong pink or wine color after sintering at 1150 °C under 600 MPa or 1250 °C under 250 MPa, respectively. This was confirmed to be a result of oxygen vacancies created during the sintering process and high sensitivity of Er₂O₃ to the strong reducing atmosphere in the SPS apparatus. Post-sintering annealing in an air furnace led to elimination of oxygen vacancies and increased transparency. Additionally, the photoluminescence intensity and phosphorescence lifetime of annealed (pink) samples was higher and shorter, respectively, compared to that of the reduced (wine-colored) samples.     

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.     

Effects of CaSiO3 addition on sintering behavior and microwave dielectric properties of Al2O3 ceramics

The effects of CaSiO₃ addition on the sintering behavior and microwave dielectric properties of Al₂O₃ ceramics have been investigated. The addition of CaSiO₃ into Al₂O₃ ceramics resulted in the emergence of Ca₂Al₂SiO₇ and CaAl₂Si₂O₈, which acting as liquid sintering aids can effectively lower the sintering temperature of Al₂O₃ ceramic. The Q × f value of Al₂O₃-CaSiO₃ ceramics decreased with the CaSiO₃ addition increasing because of the lower Q × f value of Ca₂Al₂SiO₇ and CaAl₂Si₂O₈. Compared with the pure CaSiO₃ ceramic, the Al₂O₃-CaSiO₃ ceramic with 20 wt% CaSiO₃ addition possessed good dielectric properties of ?_r = 9.36 and Q × f = 13,678 GHz at the similar sintering temperature.     

Fabrication of magnesium aluminate (MgAl2O4) spinel foams

This paper reports on a novel-processing route for fabricating magnesium aluminate (MgAl₂O₄) spinel (MAS) foams from aqueous suspensions containing 30–35 vol.% solids loading. A stoichiometric MAS powder formed from alumina (71.8%) and magnesia (28.2%) at 1400 °C was surface passivated against hydrolysis in an ethanol solution of H₃PO₄ and Al(H₂PO₄)₃ at 80 °C for 24 h. Stable aqueous suspensions with 30–35 vol.% solids loading were prepared using the surface passivated MAS powder with the help of tetra-methylammonium hydroxide (TMAH) and an ammonium salt of polyacrylic acid (Duramax D-3005) employed as dispersing agents. An aqueous solution of N-cetyl-N,N,N-trimethylammonium bromide (CTMAB) was utilized to create foam in aqueous MAS suspensions by mechanical frothing. Liquid foam was then consolidated in non-porous moulds by introducing a polymerization initiator and a catalyst under ambient conditions. Dried (at >90 °C for 24 h) MAS foams were then sintered for 1 h at 1650 °C. For comparison purposes, dense MAS bodies out of an un-passivated stoichiometric MAS powder, and, dense as well as foams out of alumina were also prepared in this study. The sintered properties of MAS and alumina ceramics were characterized by various means and thus obtained results are presented and discussed in this paper. The sintered MAS foams exhibited a porosity of about 74–76% and a compressive strength of about 4–7.2 MPa inline to values reported for other ceramic foams in the literature.     

Synthesis of mesoporous nanocrystalline MgAl2O4 spinel via surfactant assisted precipitation route

In this research, mesoporous nanocrystalline MgAl₂O₄ spinel powders were synthesized with a facile synthesis method by co-precipitation route using CTAB as surfactant. The prepared samples were characterized by X-ray diffraction, N₂ adsorption, thermal gravimetric and differential thermal analyses, Fourier transform infrared spectroscopy and transmission electron microscope. The effects of surfactant to metal molar ratio on the structural properties of the samples were investigated. The obtained results showed that the sample prepared without addition of surfactant presented a lower specific surface area and bigger crystallite size compared with those obtained for the samples prepared by CTAB/metal molar ratio of 0.3. The results showed that the sample prepared by CTAB/metal molar ratio of 0.3 has the highest specific surface area and the smallest crystallite size. Moreover, the CTAB/metal molar ratio higher than 0.3 led to a decrease in the specific surface area, due to destruction of the pore walls.     

Transparent yttria produced by spark plasma sintering at moderate temperature and pressure profiles

Transparent yttria (Y₂O₃) bodies were fabricated by spark plasma sintering, and the effects of the sintering temperature on relative density, microstructure, and the optical and mechanical properties of Y₂O₃ bodies were investigated. Fully dense Y₂O₃ bodies were obtained at sintering temperatures 1473-1873 K. The average grain size was 0.24-0.32 μm at 1473-1573 K, and steadily increased to 1.97 μm with an increase in temperature to 1823 K. The highest transmittance was obtained in the Y₂O₃ body sintered at 1573 K and annealed at 1323 K, showing 81.7% (99% of the theoretical value) at a wavelength of 2000 nm.     

Structural, thermal and mechanical properties of transparent Yb:(Y0.97Zr0.03)2O3 ceramic

Yb doped (Y_0.97Zr_0.03)₂O₃ transparent ceramics were fabricated by solid state reaction and vacuum sintering. The microstructure, thermal and mechanical properties of Y₂O₃ ceramic, as well as the effect of Yb doping concentration on these properties were investigated in detail. The lattice parameter and unit cell volume decrease with the increasing of Yb content, whereas thermal expansive coefficient increases. With Yb content increasing from 0 to 8 at.%, the mean grain size increases from 15.82 μm to 26.54 μm, and the thermal conductivity at room temperature (RT) decreases from 11.97 to 6.39 W/m/K. The microhardness decreases with Yb content, and the microhardness and fracture toughness of (Y_0.97Zr_0.03)₂O₃ transparent ceramic is 11.11 GPa and 1.29 MPa m^1/2, respectively.     

Effect of TiO2 on phase evolution and microstructure of MgAl2O4 spinel in different atmospheres

The effect of TiO₂ on the formation and microstructure of magnesium aluminate spinel (MgAl₂O₄) at 1600 °C in air and reducing conditions were investigated. Under reducing conditions, stoichiometric MgAl₂O₄ spinel shifted toward alumina-rich types owing to volatilization of MgO, resulting in an increase in the porosity of fired samples. Addition of graphite to mixtures of MgO and Al₂O₃ intensified the reducing conditions and accelerated the formation of non-stoichiometric MgAl₂O₄. For TiO₂-containing samples on addition of MgAl₂O₄, magnesium aluminum titanium oxide (Mg_xAl_2(1−x)Ti_(1+x)O₅, x = 0.2 or 0.3) was detected as a minor phase. Under reducing conditions, XRD peak shifts were smaller for TiO₂-containing samples than for samples without TiO₂ owing to the formation of a solid solution of TiO₂ in MgAl₂O₄ and establishment of alumina-rich spinel, which have opposite effects on increasing the lattice parameter. In bauxite-containing samples, MgAl₂O₄ spinel, corundum, magnesium orthotitanate spinel (Mg₂TiO₄) and amorphous phases were identified. Mg₂TiO₄ spinel formed a complete solid solution with MgAl₂O₄ spinel but Mg₂TiO₄ remained as a distinct phase owing to the heterogeneous microstructure of bauxite-containing samples. Also dense microstructure established in air fired TiO₂ containing samples. The results are discussed with emphasis on the application and design of alumina-magnesia-carbon refractory materials, which are used in the steel industry.     

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.     

Influence of green state processes on the sintering behaviour and the subsequent optical properties of spark plasma sintered alumina

The present investigation gives a quantitative correlation between different green microstructures, and their sintering behaviour during spark plasma sintering. The green microstructures were elaborated via various green shaping processes such as direct casting and direct coagulation casting compared to uniaxial compaction of the as-received sub-micron grained corundum powder. Narrowing pore size distribution and reducing pore size (≈40 nm) in the green compact could favour cold densification during initial uniaxial pressing by grain sliding and rearrangement. This is attributed to the soft homogeneous touching network in direct-cast green samples. Consequently, grain growth was impeded and the onset of shrinkage was delayed. Moreover, the small pores and the narrow pore size distribution in the homogeneous green bodies led to higher final densities, with better optical properties compared to the less homogeneous green samples.     

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.     

Processing and mechanical properties of B4C-SiCw ceramics densified by spark plasma sintering

Homogenous distribution of whiskers in the ceramic matrix is difficult to be achieved. To solve this problem, B₄C-SiC_w powder mixtures were freeze dried from a slurry dispersed by cellulose nanofibrils (CellNF) in this work. Dense B₄C ceramics reinforced with various amounts of SiC_w up to 12 wt% were consolidated by spark plasma sintering (SPS) at 1800 °C for 10 min under 50 MPa. During this process, CellNF was converted into carbon nanostructures. As iron impurities exist in the starting B₄C and SiC_w powders, both thermodynamic calculations and microstructure observations suggest the dissolution and precipitation of SiC_w in the liquids composed of Fe-Si-B-C occurred during sintering. Although not all the SiC_w grains were kept in the final ceramics, B₄C-9 wt% SiC_w ceramics sintered at 1800 °C still exhibit excellent Vickers hardness (35.5 ± 0.8 GPa), flexural strength (560 ± 9 MPa) and fracture toughness (5.1 ± 0.2 MPa·m^1/2), possibly contributed by the high-density stacking faults and twins in their SiC grains, no matter in whisker or particulate forms.     

Microstructure and magnetic properties of nickel-zinc ferrite ceramics fabricated by spark plasma sintering

Dense nickel-zinc (NiZn) ferrite ceramics were successfully fabricated within tens of seconds via spark plasma sintering. The phase composition and microstructure of the sintered samples were characterized by X-ray diffraction and scanning electron microscopy, respectively. The static magnetic properties at room temperature and Curie temperature of the samples were investigated by vibrating sample magnetometry. The results indicated that the main phase of the sintered samples was Ni_0.75Zn_0.25Fe₂O₄ with spinal structure, and the sintering temperature and heating rate observably affected the microstructure and density, then the magnetic properties of the sample. The Joule heat generated by NiZn ferrite during spark plasma sintering was very important for the rapid preparation of the sample with high density and small grain size. The low sintering temperature and heating rate would be helpful to obtain samples with small grain size, high density, and then good magnetic properties. The samples sintered at 900 °C with the heating rate of 5–10 °C/s were characterized of the relative density above 95%, 4πM_s value beyond 4000 Gs and coercivity below 27.7 Oe.