Correlation between fracture toughness and microstructure of seeded silicon nitride ceramics

Microstructure development and fracture toughness of Si₃N₄ composites were studied in the presence of seeds and Al₂O₃ + Y₂O₃ as sintering aids. The elongated β-Si₃N₄ seeds were introduced into two different α-Si₃N₄ matrix powders; one was the ultra fine powder matrix and the other was the coarse powder matrix. The amount of seeds varied from 0 to 6 wt%. The grain growth inhibition and the mechanism of toughening were discussed and correlated with microstructure. The maximum fracture toughness of 9.0 MPa m^1/2 was obtained for ultra fine powder with 5 wt% seeds hot pressed at 1,700 °C for 6 h.     

Microstructure and properties of alumina-SiC nanocomposites prepared from ultrafine powders

Alumina-Silicon Carbide nanocomposites were produced and studied under different aspects: characteristics of the starting materials, processing, microstructure and mechanical properties. The raw materials were two kinds of fine SiC powders (30 and 45 nm) and two Al₂O₃ powders (60 and 140 nm). Different compositions (amounts of SiC in the range 0.5–5 vol%) were performed and the characteristics of the resulting materials compared. The oxygen enrichment in SiC nanopowder due to specific powder treatments was controlled, in order to optimize powder processing routes. Densification tests of Al₂O₃-SiC powder mixtures were performed both by pressureless sintering and hot pressing route. The addition of SiC reduced the densification rate and favoured a refinement of the matrix. Improvement of mechanical properties over monolithic alumina was obtained in composites with the 45 nm SiC. The study pointed out that the critical factor for the success of these materials is the choice of the raw SiC powders in terms of grain size and state of agglomeration. The addition of this ultrafine SiC strongly affected the microstructural evolution, even at low volumetric fractions. The results do not substantiate any remarkable effect by dispersoids in the tested nanosize range.     

Mechanical properties of hot isostatically pressed zirconium nitride materials

The influence of powder properties on the sintering behaviour, the microstructural development and the mechanical properties of hot isostatically pressed (HIPed) zirconium nitrides were investigated. The results show that the densification behaviour is dependent on the powder characteristics, more precisely the grain morphology and size, and oxygen, carbon and metallic impurity contents. The mechanical properties are controlled mainly by the amount of porosity and the presence of a complex intergranular phase in direct relation to the purity of the starting powder. The differences in the fracture strength and toughness between the two grades are perceptible. On the other hand, the thermal shock resistance to fracture initiation, as well as the elastic parameters of both dense materials, are similar.     

A study of phase stability and mechanical properties of hydroxylapatite–nanosize α-alumina composites

Hydroxylapatite (HA)–nanosize alumina composites were synthesized to study their phase stability and mechanical properties. To make these composites, nanosize α-Al₂O₃ powder was used because of its better sinterability and densification as compared to nanosize γ-Al₂O₃. The composites were air sintered without pressure and hot pressed in vacuum at 1100 °C and 1200 °C. In the composites, HA decomposed to tri-calcium phosphate faster after the air sintering than hot pressing. Moreover, hexagonal unit cell volume of HA left in the composites showed that there was more decomposition of HA after the air sintering than hot pressing. It also showed that HA in the composites was OH⁻ and Ca²⁺ deficient. As the amount of alumina increased, sinterability considerably decreased. Hot pressing at 1200 °C resulted in better mechanical properties (μ-hardness and fracture toughness) than the hot pressing at 1100 °C.     

The preparation of AI2O3/Ni composites by a powder coating technique

In the present study, nickel particles are coated onto the surface of alumina powder by an impregnation technique. The densification behaviour and the microstructural evolution of the nickel coated alumina powder during sintering are investigated. The strength and the toughness of the resulting Al₂O₃/Ni composites are determined. As the nickel content is less than 13 vol%, fully dense composites can be prepared by pressureless sintering. The matrix grain size decreases as nickel inclusions are added. The strength and the toughness of alumina can be increased by 23 and 42% by adding 5 and 8vol% nickel, respectively. The toughening effect is attributed to plastic deformation of ductile inclusions and crack deflection by the inclusions. The strengthening effect is attributed to microstructural refinement.     

The Effect of Variable Binder Content and Sintering Temperature on the Mechanical Properties of WC–Co–VC/Cr3C2 Nanocomposites

WC powders with an average crystallite size of 10 nm were successfully prepared by ball milling of micron-sized tungsten carbide powders. Grain growth inhibitors (VC and Cr₃C₂) with concentrations of 0.6 wt% each were added to nanocomposites of WC–9Co and WC–12Co, in both as-received and milled WC. Powder mixtures were then consolidated using spark plasma sintering technique at 1200 and 1300 °C for 10 min under high vacuum and pressure of 50 MPa. The influence of WC crystallite size, Co content, and sintering temperature over microstructure and mechanical properties of the resulting composites were studied through XRD and FESEM. Densification and attained grain sizes of the sintered products were measured by Archimedes principle and Scherrer procedure, respectively. Moreover, microhardness (H_v30) and fracture toughness were measured and compared for each composition to comparatively assess the individual effect. It was observed that the addition of VC and Cr₃C₂ resulted in decreased densification of the synthesized composites. These grain growth inhibitors were found to limit grain sizes to 131 nm with an average hardness of 1592 H_v30 and fracture toughness of 9.23 Mpam^1/2.     

Crystallization and microstructural evolution process from the mechanically alloyed amorphous SiBCN powder to the hot-pressed nano SiC/BN(C) ceramic

The mechanically alloyed amorphous SiBCN powders were hot pressed at 1500, 1600, 1700, 1800, and 1900 °C under a pressure of 80 MPa in the nitrogen atmosphere for 30 min. The crystallization, the microstructural evolution, and the properties of the prepared ceramics were carefully studied by XRD, TEM, HRTEM, and property testing. Results show that the crystallization of β-SiC, turbostratic BN(C), and α-SiC in the amorphous matrix starts at about 1500, 1600, and 1700 °C, respectively. When the powder is hot pressed at the temperatures higher than 1700 °C, the prepared ceramics always consist of nano β-SiC, α-SiC, turbostratic BN(C), and amorphous body. With the increase of the sintering temperature, the ceramic crystallinity becomes higher, the grains get larger, and the amorphous content becomes lower. At the temperatures lower than 1800 °C, the bulk density, the relative density, the flexural strength, the Young’s modulus, and the fracture toughness of the prepared ceramics show persistent but insignificant increase. However, when the ceramic is sintered at 1,900 °C, these properties are rapidly improving to 2.6 g/cm³, 91.8 %, 331.0 MPa, 139.4 GPa, and 2.8 MPa m^1/2.     

Synthesis, densification, and mechanical properties of TaB2

Tantalum diboride (TaB₂) was synthesized by reducing Ta₂O₅ using B₄C and graphite at 1600 °C under flowing Ar. The powder had an average particle size of 0.4 μm with both needle-like and rounded particles. The TaB₂ powder was hot pressed to relative densities of 97% at 2000 °C (3.6 μm grain size) and 98% at 2100 °C (5.3 μm grain size). Mechanical properties were measured for TaB₂ hot pressed at 2100 °C and were comparable to those of the commonly studied diborides, ZrB₂ and HfB₂. The Young's modulus was 551 GPa, Vickers' hardness was 25.6 GPa, flexure strength was 555 MPa, and fracture toughness was 4.5 MPa-m^1/2.     

Reaction sintering fabrication of (AlN, TiN)-Al2O3 composite

The (AlN, TiN)-Al₂O₃ composites were fabricated by reaction sintering powder mixtures containing 10-30 wt.% (Al, Ti)-Al₂O₃ at 1420-1520°C in nitrogen. It was found that the densification and mechanical properties of the sintered composites depended strongly on the Al, Ti contents of the starting powder and hot pressing parameters. Reaction sintering 20 wt.% (Al, Ti)-Al₂O₃ powder in nitrogen in 1520°C for 30 min yields (AlN, TiN)-Al₂O₃ composites with the best mechanical properties, with a hardness HRA of 94.1, bending strength of 687 MPa, and fracture toughness of 6.5 MPa m^1/2. Microstructure analysis indicated that TiN is present as well dispersed particulates within a matrix of Al₂O₃. The AlN identified by XRD was not directly observed, but probably resides at the Al₂O₃ grain boundary. The fracture mode of these composites was observed to be transgranular.     

Effect of Ni powder characteristics on the consolidation of ultrafine TiMoCN cermets by means of SPS and HIP technologies

Fully dense titanium carbonitride cermets have been consolidated from Ti(C,N)–Ni–Mo₂C–TiAl₃ powder mixtures either by spark plasma sintering or hot isostatic pressing techniques. Carbonyl Ni powders enhance the densification of the cermets produced by SPS (spark plasma sintering), a phenomenon likely related to a more efficient dissolution of Mo₂C additions and the possible precipitation of α″ phase. Both SPS and HIP (hot isostatic pressing) processes lead to materials with a bimodal Ti(C,N) grain size distribution containing a considerable fraction of nanometric grains. Unlike SPS, HIP induces significant graphite precipitation which could be explained by the destabilization of the carbonitride phase under high isostatic pressures at high temperature. Optimized compositions processed by SPS exhibit a combination of hardness and toughness close to the range covered by ultrafine WC–Co hardmetals of similar binder contents.     

Microstructure and related mechanical properties of hot pressed hydroxyapatite ceramics

Polycrystalline hydroxyapatite (HAP) ceramics were densified by hot pressing. The effects of thermal treatments and of a sintering additive (Na₃PO₄) on the microstructure, flexural strength and fracture toughness were investigated. Hot pressing without additive resulted in dense HAP having a small average grain size (below 0.5 m). Spontaneous microcracking of the material was also noted. This originated from the thermal expansion anisotropy of HAP crystals. The presence of the sintering aid promotes grain growth. Dense materials exhibited mechanical properties depending on the microstructure. The highest values obtained were 137 MPa and 1.2 MPa % MathType!MTEF!2!1!+-% feaafeart1ev1aaatCvAUfeBSjuyZL2yd9gzLbvyNv2CaerbuLwBLn% hiov2DGi1BTfMBaeXatLxBI9gBaerbd9wDYLwzYbItLDharqqtubsr% 4rNCHbGeaGqiVu0Je9sqqrpepC0xbbL8F4rqqrFfpeea0xe9Lq-Jc9% vqaqpepm0xbba9pwe9Q8fs0-yqaqpepae9pg0FirpepeKkFr0xfr-x% fr-xb9adbaqaaeGaciGaaiaabeqaamaabaabaaGcbaWaaOaaaeaaci% GGTbaaleqaaaaa!36FA!\[\sqrt \operatorname{m} \] for the flexural strength and fracture toughness, respectively. A decrease of both strength and toughness was observed with increasing average grain size. This behaviour is attributed to the weakening of the grain boundaries by either the development of initial microcracking or the Na₃PO₄ addition. It is concluded that hot pressing is very useful to elaborate dense HAP having good mechanical characteristics.     

Microstructural development and mechanical properties of pressureless-sintered SiC with plate-like grains using Al2O3-Y2O3 additives

Dense SiC ceramics with plate-like grains were obtained by pressureless sintering using -SiC powder with the addition of 6 wt% Al₂O₃ and 4 wt% Y₂O₃. The relationships between sintering conditions, microstructural development, and mechanical properties for the obtained ceramics were established. During sintering of the -SiC powder compact the equiaxed grain structure gradually changed into the plate-like grain structure that is closely entangled and linked together through the grain growth associated with the phase transformation. With increasing holding time, the fraction of phase transformation, the grain size, and the aspect ratio of grains, increased. Fracture toughness increased from 4.5 MPa m^1/2 to 8.3 MPa m^1/2 with increasing size and aspect ratio of the grains. Crack deflection and crack bridging were considered to be the main operative mechanisms that led to improved fracture toughness.     

The influence of Sr and Mn incorporated ions on the properties of microwave single- and two-step sintered biphasic HAP/TCP bioceramics

The aims of this study were to investigate the effects of Sr- and Mn-doped ions on the sintering behaviors, microstructure and mechanical properties of the bioceramics processed by single- and two-step microwave sintering (MWSSS and MWTSS). Nano-sized calcium hydroxyapatite powders doped with Sr and Mn ions, obtained by modified precipitation synthesis, were isostatically pressed at 400 MPa and processed by MWSSS and MWTSS at different temperatures. In all cases during the sintering, the doped HAP powders turned into biphasic mixtures of HAP and TCP, but the amount of TCP was certainly lower in the case of MWTSS. It was shown that the doped ions significantly affected: density, microstructure, grain size, porosity, hardness, and fracture toughness of the processed bioceramics. Two-step microwave sintering was successfully applied for the processing of HAP/TCP bioceramics doped with strontium and manganese ions. Both two-step microwave sintered doped bioceramics had similar and high hardness values, but the strontium-substituted bioceramic material certainly had higher fracture toughness (1.54 MPam^1/2), with an average grain size of 195 nm. Based on the results presented in this paper, it was concluded that the two-step microwave sintered strontium-doped bioceramics could be suitable materials in the bone regenerative field.     

Microstructural homogeneity improvement in Si3N4 by a powder coating method

The efficiency of a powder coating technique has been quantitatively evaluated through a comparison of the densification behaviour, green compact and dense material microstructural homogeneity in terms of a homogeneity dimension, and mechanical properties, using coated powders and mixed powders in the case of Si₃N₄ powder densified by hot-pressing with the liquid-forming additive system Al₂O₃-TiO₂-SiO₂. For coated powder, a significantly smaller value of the homogeneity dimension was obtained. The oxide phases became re-distributed during densification, with the aluminium-containing phase distributed on a finer scale, and the titanium-containing phase on a coarser scale, compared with the green body. Materials prepared by hot-pressing of coated powders showed a more homogeneous microstructure, higher bend strength and higher Weibull modulus, compared with materials prepared from mixed powders. There were no differences in fracture toughness and hardness between the two types of material.     

Microstructural evolutions of nickel-aluminide nanocomposites during powder synthesis and thermal spray processes

The synthesis and microstructural evolutions of the NiAl-15 wt% (Al₂O₃–13% TiO₂) nanocomposite powders were studied. These nanocomposite powders are used as feedstock materials for thermal spray applications. These powders were prepared using high and low-energy mechanical milling of the Ni, Al powders and Al₂O₃–13% TiO₂ nanoparticle mixtures. High and low-energy ball-milled nanocomposite powders were also sprayed by means of high-velocity oxy fuel (HVOF) and air plasma spraying (APS) techniques respectively. The results showed that the formation of the NiAl intermetallic phase was noticed after 8 h of high-energy ball milling with nanometric grain sizes but in a low-energy ball mill, the powder particles contained only α-Ni solid solution with no trace of the intermetallic phase after 25 h of milling. The crystallite sizes in HVOF coating were in the nanometric range and the coating and feedstock powders showed the same phases. However, under the APS conditions, the coating was composed of the NiAl intermetallic phase in the α-Ni solid solution matrix. In both of the nanocomposite coatings, reinforcing nanoparticles (Al₂O₃–13% TiO₂) were located at the grain boundaries of the coatings and pinned the boundaries, therefore, the grain growth was prohibited during the thermal spraying processes.     

Dense pure binderless WC bulk material prepared by spark plasma sintering

The phases, microstructures and mechanical properties of binderless WC bulk materials prepared by the spark plasma sintering technique were investigated systematically. The addition of carbon was added to eliminate the impurity phase W₂C. The relative density, Vickers hardness and grain size increase obviously with increasing sintering temperature, but increase weakly with increasing pressure or sintering time. The high relative density of 99·1%, HV30 of 27·5 GPa and fracture toughness K_IC of 4·5 MPa m^1/2 of pure binderless WC bulk with a grain size of 400 nm was obtained by sintering the WC powders with a particle size of 200 nm and the addition of 0·63 wt-%C at 1800°C for 6 min under 70 MPa.     

Mechanical and physical properties of sintered YBCO-metal bulk composites with silver powder and fibres

Silver powder and continuous fibres were used in developing sintered YBa₂Cu₃O_7–x (YBCO)-metal composites because applications require further improvement in mechanical and physical properties of the bulk superconducting elements without affecting the critical current capacity. The weight ratios of silver powder to YBCO and silver fibre to YBCO were varied up to 50% and 5%, respectively, in the beam elements. The effect of silver addition on the density of the composite has been quantified. Stress-strain-critical current properties of bulk YBCO-metal composite elements were investigated in bending at 77 K. The addition of silver powder reduced the sintering temperature, increased the dimensional changes after sintering and also improved the strength, toughness and critical current capacity compared to the monolithic. Silver fibres, (aspect ratios varying between 70 and 110), aligned along the length of the element restricted the changes in dimensions of the composite after sintering and also influenced the stress-strain-current capacity relationship, strength and toughness of the composite to varying degrees. The mixture theory was used to predict the composite flexural strength based on the composition of the composite, constituent properties and porosity.     

Densification behaviour of oxide-coated silicon nitride powders

Powder coating has been explored as a method of incorporating sintering additives into a ceramic powder. This procedure has been explored in the case of Si₃N₄ powders coated with thin layers of MgO.The effectiveness of the powder coating technique has been evaluated by comparing the powder properties, densification behaviour, microstructure and mechanical properties of coated Si₃N₄ powders with identical powders in which the additive oxide has been added in particulate form. It is concluded that the powder coating technique is an excellent method of homogeneously incorporating minor amounts of sintering additive into a powder. The coated powder exhibited improved homogeneity, and gave good green compact density, high green strength, and faster densification rate. Moreover, coated powders densified more easily by pressureless sintering and showed a more homogeneous microstructure, higher strength and faster densification rates, compared with materials prepared using mixed oxide powders. Significant improvements in hardness and fracture toughness were observed for the coated powders.     

Synthesis and sintering of Sr- and Ca-doped lanthanum chromite ultrafine powder for SOFC interconnect

In this study, ultrafine powder of mixed Sr- and Ca-doped lanthanum chromite with two different compositions (La_0.7Sr_0.1Ca_0.2CrO₃ and La_0.7Sr_0.2Ca_0.1CrO₃) and average particle size of 150 nm was successfully synthesized by the simple process of glycine nitrate. The samples were characterized by thermal analysis, X-ray diffraction, and nitrogen adsorption–desorption, scanning and transmission electron microscopy. The synthesized ultrafine powders with perovskite type crystal structure and some SrCrO₄ or CaCrO₄ phases were cold isostatically pressed at 200 MPa, and then sintered in air at 1400 °C for several time periods (1–10 h). Relative density measurements were conducted by Archimedes method. The maximum relative density for both samples obtained after sintering in air at 1400 °C for 10 h was 98.2 % of the theoretical density and the average grain size of the sintered pellets was about 2 μm. In addition, the effects of composition on phase transition behavior and electrical properties were studied.     

Densification of ultrafine SiC powders

Recent results on the densification behaviour of ultrafine SiC powders (below 20 nm) are presented and compared with results on the densification of ultrafine silicon-based ceramic powders given in the literature. A study of different powder processing routes and their influence on the pore-size distribution is given. Pressureless sintered green bodies having pore sizes of about 20 nm show extreme coarsening without significant densification. The results indicate a significant influence of green density on shrinkage. Encapsulated hot isostatic pressing (HIPing) led to a reduction of pore size and to considerable density increase at temperatures below 1600 °C. But even then full density without extensive grain growth was difficult to achieve. The applied method to determine grain sizes (X-ray diffraction measurements, XRD, using the Scherrer formula, scanning electron microscopy, SEM, and transmission electron microscopy, TEM) gave similar results for TEM and SEM but lower values for XRD. A possible explanation is presented. Density and grain growth both during pressureless sintering and HIPing showed significant differences between samples with and without sintering additives (B and C). Whether or not the use of sintering agents is favourable in reaching high densities and fine grain sizes, is discussed. HIP densification was modelled assuming diffusion to be the dominant mechanism. Grain growth according to a t ^1/4 dependence and an activation energy of 6.8 eV was introduced into the model. Results on the properties (hardness, also at elevated temperatures, fracture toughness, bending and compression tests, thermal conductivity) of the hot isostatically pressed samples, are presented.