Hydroxyapatite/bioactive glass functionally graded materials (FGM) for bone tissue engineering

In this work, HA/bioactive glass Functionally Graded Materials (FGMs) are obtained for the first time by means of Spark Plasma Sintering (SPS). Two series of highly dense 5 layered products, namely FGMS1 and FGMS2, are prepared under optimized SPS conditions, i.e. 1000 °C/2 min/16 MPa and 800 °C/2 min/50 MPa, respectively, using a die with varying cross section.Results arising from XRD, SEM, mechanical and biological characterization in SBF, evidence that lower temperature and higher-pressure levels used for FGMS2 samples provide better materials in terms of microstructure, compactness, hardness, elastic modulus and in vitro bioactivity. Indeed, a fully sintered and crack-free microstructure with no crystallisation at the top layer (100% bioactive glass) is correspondingly produced.The obtainment of such FGMs is quite promising, since it permits to vary the relative volume fractions of the two constituents and, consequently, tailor the biological response for specific clinical applications.     

Effect of carbon nanoparticle reinforcement on mechanical and thermal properties of silicon carbide ceramics

This research presents an analysis of the influence of graphene reinforcement on the thermal and mechanical properties of silicon carbide ceramics, at 2.5% (wt%) graphene content. The SiC composites, containing various carbon nanofillers (graphene oxide and graphene nanoparticles), were sintered by the classical two stage spark plasma sintering method. Two current modes were used, the continuous mode and the pulsed current mode. The results from photothermal radiometry and investigations of the mechanical properties showed that graphene additives significantly improve the thermal properties and toughness of material, sintered from a SiC powder. An 45% growth in the toughness was observed, which increased from 1.21 to 1.75?MPa/m^1/2. The thermal diffusivity value also increased from 0.60 to 0.71?cm²/s and giving an improvement in thermal properties of 18%. The friction coefficient reached 7% giving an increase in value from 0.62 to 0.66. Microscopic investigations supported the photothermal radiometry (PTR) results. Whilst, thermal imaging revealed homogeneity of the local thermal properties of the products fabricated from the starting SiC powder.     

Densification improvement of spark plasma sintered TiB2-based composites with micron-, submicron- and nano-sized SiC particulates

Taguchi design of experiments methodology was used to determine the most influential spark plasma sintering (SPS) parameters on densification of TiB₂–SiC ceramic composites. In this case, four processing factors (SPS temperature, soaking time, applied external pressure and SiC particle size) at three levels were examined in order to acquire the optimum conditions. The statistical analysis identified the sintering temperature as the most effective factor influencing the relative density of TiB₂–SiC ceramics. A relative density of 99.5% was achieved at the optimal SPS conditions; i.e. temperature of 1800?°C, soaking time of 15?min and pressure of 30?MPa by adding 200-nm SiC particulates to the TiB₂ matrix. The experimental measurements and predicted values for the relative density of composite fabricated at the optimum SPS conditions and reinforced with the proper SiC particle size were almost similar. The mechanisms of sintering and densification of spark plasma sintered TiB₂–SiC composites were discussed in details.     

Densification mechanisms and microstructural evolution during spark plasma sintering of boron carbide powders

Micron-sized boron carbide (B₄C) powders were subjected to spark plasma sintering (SPS) under temperature ranging from 1700 °C to 2100 °C for a soaking time of 5, 10 and 20 min and their densification kinetics was determined using a creep deformation model. The densification mechanism was interpreted on the basis of the stress exponent n and the apparent activation energy Q_d from Harrenius plots. Results showed that within the temperature range 1700–2000 °C, creep deformation which was controlled by grain-boundary sliding or by interface reaction contributed to the densification mechanism at low effective stress regime (n = 2,Q_d = 459.36 kJ/mol). While at temperature higher than 2000 °C or at high stress regime, the dominant mechanism appears to be the dislocation climb (n = 6.11).     

Effects of spark plasma sintering on ferroelectricity of 0.8Bi3.15Nd0.85Ti3O12-0.2CoFe2O4 composite ceramic

The 0.8Bi_3.15Nd_0.85Ti₃O₁₂ (BNdT)-0.2CoFe₂O₄ (CFO) composite multiferroic ceramics have been fabricated by spark plasma sintering (SPS) at 850?°C. The relative density of as-sintered SPS ceramic reaches 97.4 (±0.3)%. The composites are composed of pure BNdT and CFO phases without any preferred c-orientation. The a-orientation preference is more obvious perpendicular to the pressure direction. The average grain-sizes of BNdT and CFO are 163 and 146?nm, respectively. The BNdT phase has more grains below 100?nm (～20%). The super energy-dispersive X-ray analyses suggest no serious reaction between BNdT and CFO. The Raman spectrum verifies the nano-structure of the SPS ceramic via the broadening bands and peak shifts. The Curie temperature of the SPS ceramic declines to 560?°C with stabilized dielectric loss. The grain boundary resistance plays a dominant role on impedance above 700?°C. The remanent polarization approaches to 15.2?μC/cm² (300?kV/cm) with lower coercive fields (?89/+95?kV/cm).     

放电等离子技术连接铬酸镧陶瓷

铬酸镧陶瓷脆性高、难以变形,使其在加工上存在难度。利用陶瓷连接技术可以将小部件连接为大部件,实现低成本制造形状复杂的大型陶瓷构件。以铬酸镧的前驱体料浆作为中间层材料,利用放电等离子技术进行了铬酸镧陶瓷的连接,测定了连接件的连接强度,并借助SEM、EDS等手段分析了连接温度及保温时间对连接件强度的影响。结果表明,连接温度为1400℃时,连接件可以获得最高的连接强度,连接过程中母材中出现第二相Cr4O5。     

Synthesis and sintering at low temperature of a new nanostructured beta-Eucryptite dense compact by spark plasma sintering

The solid state reaction between kaolin and Li₂CO₃ with a 1:1 M composition has been studied in the temperature range 380°C-550 °C. The role played by Li₂CO₃ (basic medium) in the thermal transformation of the kaolin has been investigated by X-Ray diffraction, FESEM, TEM, MAS-NMR and XPS techniques. For the first time, a nanostructured high density β- Eucryptite (<10 nm) has been obtained by Spark Plasma Sintering (SPS) at 550 °C in high vacuum. The atmosphere used in sintering treatments has a determinant role in lithium migration and crystallization of β- Eucryptite. In the case of low vacuum treatments, an amorphous LiAlSiO₄ geopolymer type material was obtained. Due to exclusive properties and performances of β- Eucryptite based materials, the results reported in the present investigation open new perspectives for new nanostructured and amorphous functional materials with null thermal expansion, ionic conduction and remarkable mechanical properties.     

SPS反应烧结HfB2复合材料的制备和性能

针对HfB2陶瓷材料难烧结和韧性差等问题,选择ZrC粉、Si粉和C粉为烧结助剂,借助ZrC-Si-C间的原位反应生成ZrSi2和SiC,促进HfB2陶瓷的烧结,并提高HfB2陶瓷的综合力学性能。结果表明,HfB2与烧结助剂的混合粉体经放电等离子烧结(SPS)在1600℃保温10 min和40 MPa的压力条件下制备出相对密度为96.6 1%的HfB2-ZrSi2-SiC复合材料,所制样品的硬度、抗弯强度和断裂韧性均随着烧结助剂ZrC-Si-C含量的增加呈现先上升后降低的趋势。当ZrC-Si-C添加量为10%时所制备样品的综合力学性能最好,其硬度值为26.80±1.2 GPa、抗弯强度为504±40 MPa、断裂韧性值为4.66±0.21 MPa·m1/2。     

Synthesis of BaCe0.9-xZrxY0.1O3-δ nanopowders and the study of proton conductors fabricated on their basis by low-temperature spark plasma sintering

Using a citrate-nitrate process, BaCe_0.9-xZr_xY_0.1O_3-δ (x = 0, 0.5, 0.6, 0.7 and 0.8) nanopowders were synthesized, on the basis of which proton-conducting solid electrolytes (average size of coherent scattering region (CSR) - 15–53 nm) were obtained by spark plasma sintering (SPS) at a low temperature (900°С). The dependence of phase composition, microstructure and electrophysical properties of the obtained samples on ZrO₂ content and consolidation conditions was established. It was found that the BaCe_0.4Zr_0,5Y_0.1O_3-δ solid solution had the highest electrical conductivity among zirconium-containing ceramic materials in the studied concentration range. It was shown that SPS is a promising method for obtaining solid electrolytes for proton-conducting solid oxide fuel cells (PCFC) at lower temperatures (by 400–500°С), compared to traditionally-used temperature conditions (1400–1800 °C).     

Microstructure and mechanical properties of a copper–stainless-steel dual-phase system prepared by spark plasma sintering

Spark plasma sintering (SPS) has been used to synthesise samples of a model dual-phase (DP) system, consisting of copper and AISI420 martensitic steel. Mixed powders were sintered at different temperatures in the range from 850°C to 1000°C using a loading pressure of 60?MPa. Tensile testing revealed dimpled fracture surfaces in samples sintered at higher temperatures, indicating ductile failure and good interfacial bonding between the phases, with the best results overall obtained for samples sintered from wet-mixed powders. The results show that by control of the mixing, sintering and post-sintering heat treatment conditions, the fabrication of dense samples covering a range of DP microstructures is possible using SPS, with independent control of the microstructure and properties of the two phases.