Formation of Mn-Co-Ni-O Nanoceramic Microspheres Using In Situ Ink-Jet Printing: Sintering Process Effect on the Microstructure and Electrical Properties.

Mn-Co-Ni-O nanoceramic microspheres with high density, uniformity, and size tunability are successfully fabricated using in situ ink-jet printing and two step sintering (TSS) techniques. The microspheres, synthesized by an effective and facile reverse microemulsion method, consist of uncalcined Mn-Co-Ni-O nanocrystallines that show a well formed single tetragonal spinel phase and an average particle size distribution of ≈20 nm. The sintering behavior, microstructure, and electrical properties of the Mn-Co-Ni-O nanoceramic microspheres are systematically investigated and characterized. The results indicate that the sintered Mn-Co-Ni-O nanoceramic microspheres show high density and improved electrical properties. The highest R25 , B25/50 , Ea , and α25 values achieved at sintering temperature of 1150 °C are 4846.7 KΩ, 4320 K, 0.401 eV, and -5.24% K-1 , respectively for these Mn-Co-Ni-O nanoceramic microspheres. Furthermore, the formation mechanism of uncalcined Mn-Co-Ni-O nanocrystallines and an analysis of the TSS procedure of the nanoceramic microspheres are discussed.

Effect of Two-Step Sintering on the Mechanical and Electrical Properties of 5YSZ and 8YSZ Ceramics.

Yttria-stabilized zirconia (YSZ) has been widely used in structural and functional ceramics because of its excellent physicochemical properties. In this paper, the density, average gain size, phase structure, and mechanical and electrical properties of conventionally sintered (CS) and two-step sintered (TSS) 5YSZ and 8YSZ are investigated in detail. As the grain size of YSZ ceramics became smaller, dense YSZ materials with a submicron grain size and low sintering temperature were optimized in terms of their mechanical and electrical properties. 5YSZ and 8YSZ in the TSS process significantly improved the plasticity, toughness, and electrical conductivity of the samples and significantly suppressed the rapid grain growth. The experimental results showed that the hardness of the samples was mainly affected by the volume density, that the maximum fracture toughness of 5YSZ increased from 3.514 MPa·m1/2 to 4.034 MPa·m1/2 in the TSS process, an increase of 14.8%, and that the maximum fracture toughness of 8YSZ increased from 1.491 MPa·m1/2 to 2.126 MPa·m1/2, an increase of 42.58%. The maximum total conductivity of the 5YSZ and 8YSZ samples under 680 °C increased from 3.52 × 10-3 S/cm and 6.09 × 10-3 S/cm to 4.52 × 10-3 S/cm and 7.87 × 10-3 S/cm, an increase of 28.41% and 29.22%, respectively.

Mitigating grain growth in fully stabilized zirconia via a two-step sintering strategy for esthetic dental restorations.

Overall, 8-mol% yttria-stabilized zirconia (8YSZ), unlike 3YSZ, is optically transparent and stable against low-temperature degradation but has insufficient mechanical properties due to its large grain size. The influence of the grain size of 8YSZ on mechanical properties was investigated to develop an 8YSZ suitable for dental restoration. Modulation of the grain size and relative density was achieved via a two-step sintering (TSS) process, and the corresponding kinetic window was established. The conditions of TSS employed herein yielded a relative density of more than 99% while maintaining a small grain size of 0.75 µm. On the other hand, the highest biaxial strength and the highest total transmittance attained were 833 MPa and 34.6% (1-mm-thick, 39.1% for a 0.5-mm thick sample) in the TSS 8YSZ with a grain size of 1.25 µm. These results suggest that strength has improved only when grain size reduction and increased relative density are achieved at the same time. The results demonstrate that the ceramic processing method has a significant effect on the mechanical and optical properties of 8YSZ needed for dental restoration and provide a new insight that contrasts previous studies focused on the starting material.

Effect of Two-Step Sintering on Properties of Alumina Ceramics Containing Waste Alumina Powder.

This study aims to evaluate the recycling potential of solid waste alumina powder (WAP) by utilization of the two-step sintering (TSS) process. For the study, WAP was collected as an industrial scrap after the machining process for the formation of green alumina compacts. The alumina samples were prepared according to the slip casting method by preparing suspensions containing commercial alumina with 0.8 µm average particle size and by adding up to 20 dwb. % (i.e., expressed on a dry weight basis) of WAP with 3.4 µm average particle size. The samples were sintered at optimized TSS conditions and compared with conventional one-step sintering (OSS) by conducting morphological analyses. The average grain size (AGS) was determined from the obtained field emission scanning electron microscopy (FESEM) images, while the sample porosity was calculated based on apparent densities. The obtained micrographs after TSS implementation revealed a partially textured microstructure. Furthermore, a comparison of the mechanical properties of alumina samples lacking or containing 20 dwb. % of WAP obtained after sintering is presented. The indentation fracture toughness (~3.2 MPa m1/2) and Vickers hardness data (~14.5 GPa) showed a positive effect of adding WAP to alumina samples. The slightly improved mechanical properties of ceramic samples containing waste alumina are a consequence of lower porosity, which is due to the remaining sintering additives in WAP. The collected results demonstrate the possibility of using TSS for sintering ceramic materials that contain WAP.

A Combined Optimization Strategy for Improvement of Comprehensive Energy Storage Performance in Sodium Niobate-Based Antiferroelectric Ceramics.

Sodium niobate (NaNbO3, NN)-based lead-free antiferroelectric (AFE) ceramics are currently the focus of most attention on account of their outstanding energy storage density. Nevertheless, the high loss energy density (Wloss) by unique field-induced AFE-ferroelectric (FE) phase transition in pure NN ceramic and low breakdown electric field (Eb) largely restrict their practical application. Here, a combined optimization strategy was aimed at ameliorating energy storage characteristics of NN-based ceramics. First, the introduction of BiFeO3-SrTiO3 binary solid solution in pure NN ceramics destroys the long-range polar ordering and reduce the tolerance factor (t), thus reducing the polarization hysteresis, stabilizing the AFE phase and enhancing the energy storage efficiency. Then, the two-step sintering method was used to improve the compactness of ceramics and reduce the grain size. Finally, the VPP method was used to reduce the porosity, and thin the ceramic disk to a thickness of ∼100 µm. The high compactness and small thickness could effectively enhance the maximum breakdown electric field of ceramics. Ultimately, the optimum energy storage characteristics were obtained by the improvement of a combined optimization strategy, namely, an exceptional recoverable energy storage density (Wrec = 5.29 J/cm3) and efficiency (η = 82.1%) at a very high breakdown electric field (Eb = 380 kV/cm). This combined optimization strategy establishes a universal approach to ameliorate the energy storage characteristics of NN-based AFE ceramics for energy storage.

Characterization of Titanium Alloy Obtained by Powder Metallurgy.

Ti-based alloys are an important class of materials suitable especially for medical applications, but they are also used in the industrial sector. Due to their low tribological properties it is necessary to find optimal technologies and alloying elements in order to develop new alloys with improved properties. In this paper, a study on the influence of sintering treatments on the final properties of a titanium alloy is presented. The alloy of interest was obtained using the powders in following weight ratio: 80% wt Ti, 8% wt Mn, 3% wt Sn, 6% wt Aluminix123, 2% wt Zr and 1% wt graphite. Two sintering methods were used, namely two-step sintering (TSS) and multiple-step sintering (MSS), as alternatives to conventional sintering which uses a single sintering dwell time. Evolution of sample morphology, composition and crystalline structure with sintering method was evidenced. The lower values for the friction coefficient and for the wear rate was attained in the case of the sample obtained by TSS.

Two-Step Sintering of Partially Stabilized Zirconia for Applications in Ceramic Crowns.

Partially-stabilized zirconia is used in ceramic crowns due to its excellent mechanical properties and bio-inertness but does not match the natural color and translucency of tooth enamel. To reduce scattering of light and improve translucency, the grain size of zirconia ceramics should be less than the wavelength of visible light (0.4-0.7 µm), and porosity should be eliminated. The aim of the present work was to study the effect of two-step sintering of a commercial powder (Zpex Smile, Tosoh Corp., Tokyo, Japan) on the grain size and translucency of zirconia for use in ceramic crowns. Samples were sintered at a first step temperature (T1) of 1300, 1375 and 1400 °C for 5 min, followed by a decrease to the second step temperature (T2) and holding at T2 for 5-20 h. Samples were also conventionally sintered at 1450 °C for 2 h for comparison. Two-step sintered samples with an almost equal density, smaller grain size and narrower grain size distribution compared to conventionally sintered samples could be sintered. However, the translucency of two-step sintered samples had lower values compared to conventionally sintered samples. This is due to the slightly higher porosity in the two-step sintered samples. Density and translucency of both conventionally and two-step sintered samples could be increased further by using a ball milled powder.

Achieving Remarkable Amplification of Energy-Storage Density in Two-Step Sintered NaNbO3-SrTiO3 Antiferroelectric Capacitors through Dual Adjustment of Local Heterogeneity and Grain Scale.

Antiferroelectric (AFE) materials exhibit outstanding advantages against linear or ferroelectric (FE) dielectrics in high-performance energy-storage capacitors. However, their energy-storage performances are usually restricted by both extremely large hysteresis and insufficiently high driving field of the AFE-FE phase transition, which has been a longstanding issue to be overcome in the community. In this work, we report a two-step sintered 0.83NaNbO3-0.17SrTiO3 (NN-ST) lead-free relaxor AFE R-phase ceramic with high relative density of ≥95% and large spans of average grain sizes from 1.2 to 8.2 µm, strikingly achieving a giant amplification of recoverable energy-storage density (Wrec) by 176%. Analyses of permittivity-temperature curves, Raman spectrum and microstructure demonstrate that remarkably enhanced Wrec values should be ascribed to the dual adjustment of local heterogeneity (nanoscale) and grain scale (microscale), resulting in the enhanced threshold field strength for dielectric breakdown and the increased critical electric fields for the AFE-FE phase transition. A high Wrec ≈ 1.60 J/cm3, a fast discharging rate t0.9 ≈ 520 ns, large current density ∼788 A/cm2, and large power density ∼55 MW/cm3 are achieved at room temperature in the NN-ST ceramic sample with an average grain size of ∼1.2 µm. These results suggest that the multiscale structure regulation should be an efficient way for achieving enhanced energy-storage properties in NN-ST relaxor AFE ceramics through a two-step sintering technique.

What We Should Consider for Full Densification when Sintering.

To fully densify a powder compact, we should avoid two things: (i) entrapment of insoluble gases within pores and (ii) entrapment of isolated pores within grains. This paper describes general directions for promoting full densification in view of the above two points. Emphasis is placed on ways to potentially prevent pore entrapment in terms of grain growth control. Currently available techniques that can enhance densification while suppressing grain growth are briefly described, and their major mechanisms are discussed.

Effect of starting powders on the sintering of nanostructured ZrO2 ceramics by colloidal processing.

The effect of starting powders on the sintering of nanostructured tetragonal zirconia was evaluated. Suspensions were prepared with a concentration of 10 vol.% by mixing a bicomponent mixture of commercial powders (97 mol.% monoclinic zirconia with 3 mol.% yttria) and by dispersing commercially available tetragonal zirconia (3YTZ, Tosoh). The preparation of the slurry by bead-milling was optimized. Colloidal processing using 50 µm zirconia beads at 4000 rpm generated a fully deagglomerated suspension leading to the formation of high-density consolidated compacts (62% of the theoretical density (TD) for the bicomponent suspension). Optimum colloidal processing of the bicomponent suspension followed by the sintering of yttria and zirconia allowed us to obtain nanostructured tetragonal zirconia. Three different sintering techniques were investigated: normal sintering, two-step sintering and spark plasma sintering. The inhibition of grain growth in the bicomponent mixed powders in comparison with 3YTZ was demonstrated. The inhibition of the grain growth may have been caused by inter-diffusion of cations during the sintering.

A facile two step heat treatment strategy for development of bioceramic scaffolds for hard tissue engineering applications.

In the present study, a two-step sintering (TSS) method has been used to improve the mechanical properties, biocompatibility, drug release, and osteogenesis abilities of hardystonite (HT) ceramic scaffolds for tissue engineering and drug delivery applications. The average particle size of HT scaffold is kept lower than 80 nm and is reached higher than 130 nm by using two-step and conventional sintering methods, respectively. The compressive strengths of the prepared nanocrystalline HT scaffolds were found to be significantly higher than those of the micro-structure HT and currently available hydroxyapatite scaffolds. A comparative analysis of cell viability and live/dead staining of human mesenchymal stem cells (hMSCs) in nano- and micro-structured HT scaffolds and their drug release potentiation was carried out. The results showed that the nano-structured HT scaffolds have higher cell viability, biocompatibility and longer-term doxorubicin (DOX) release potential than the micro-structured ones. The results of quantitative real-time polymerase chain reaction (qRT-PCR) and immunohistochemistry (IHC) analyses showed that the expression of adhesion and differentiation supporting genes were significantly higher in nano-structured HT scaffolds as compared to the micro-structured ones. The results of qRT-PCR also showed that the mRNA expression level of ERK1/2 and P38 MAPK from hMSCs were significantly higher in nano-structured HT scaffolds than the micro-structured ones. These results potentially open new aspects for using nano-structured scaffolds in bone tissue engineering applications.

Mechanical and biological properties of the micro-/nano-grain functionally graded hydroxyapatite bioceramics for bone tissue engineering.

Functionally graded materials (FGM) open the promising approach for bone tissue repair. In this study, a novel functionally graded hydroxyapatite (HA) bioceramic with micrograin and nanograin structure was fabricated. Its mechanical properties were tailored by composition of micrograin and nanograin. The dynamic mechanical analysis (DMA) indicated that the graded HA ceramics had similar mechanical property compared to natural bones. Their cytocompatibility was evaluated via fluorescent microscopy and MTT colorimetric assay. The viability and proliferation of rabbit bone marrow mesenchymal stem cells (BMSCs) on ceramics indicated that this functionally graded HA ceramic had better cytocompatibility than conventional HA ceramic. This study demonstrated that functionally graded HA ceramics create suitable structures to satisfy both the mechanical and biological requirements of bone tissues.

Effect of alumina contents on phase stability and mechanical properties of magnesium fluorapatite/alumina composites.

The aim of the present work was twofold: to prepare biphasic magnesium fluorapatite (MFA) composites with different amounts of alumina using a two-step sintering process, and to evaluate the effects of various amounts of alumina on the mechanical properties, phase stability, and densification of the composite samples. Initially, MFA powders were prepared with different amounts of alumina by mechanical activation and the MFA composite samples were subsequently prepared using the two-step sintering (TSS) method. In order to determine the appropriate temperature of the first step sintering, conventional sintering of MFA/50% alumina was carried out at temperatures in the range of 1000-1300°C. X-ray diffraction and scanning electron microscopy (SEM) techniques were used to characterize the prepared MFA/alumina composites. The results showed fracture toughness and hardness in the MFA/50% alumina composite samples to increase as a result of alumina addition to their maximum values of 5.82±1.05MPam(1/2) and 22.09±3.5GPa, respectively.