Densification and properties of zirconia prepared by three different sintering techniques

Densification of nanocrystalline yttria stabilized zirconia (YSZ) powder with 8 mol% Y₂O₃, prepared by a glycine/nitrate smoldering combustion method, was investigated by spark plasma sintering, hot pressing and conventional sintering. The spark plasma sintering technique was shown to be superior to the other methods giving dense materials (≥96%) with uniform morphology at lower temperatures and shorter sintering time. The grain size of the materials was 0.21, 0.37 and 12 μm after spark plasma sintering, hot pressing and conventional sintering, respectively. Total electrical conductivity of the materials showed no clear correlation with the grain size, but the activation energy for spark plasma sintered materials was slightly higher than for materials prepared by the two other densification methods. The hardness, measured by the Vickers indentation method, was found to be independent on grain size while fracture toughness, derived by the indentation method, was slightly decreasing with increasing grain size.     

Effect of sintering temperature on the structural and magnetic properties of MgFe2O4 ceramics prepared by spark plasma sintering

Spark plasma sintering (SPS) is a powerful technique to produce fine grain dense ferrite at low temperature. This work was undertaken to study the effect of sintering temperature on the densification, microstructures and magnetic properties of magnesium ferrite (MgFe₂O₄). MgFe₂O₄ nanoparticles were synthesized via sol–gel self-combustion method. The powders were pressed into pellets which were sintered by spark plasma sintering at 700–900 °C for 5 min under 40 MPa. A densification of 95% of the theoretical density of Mg ferrite was achieved in the spark plasma sintered (SPSed) ceramics. The density, grain size and saturation magnetization of SPSed ceramics were found to increase with an increase in sintering temperature. Infrared (IR) spectra exhibit two important vibration bands of tetrahedral and octahedral metal-oxygen sites. The investigations of microstructures and magnetic properties reveal that the unique sintering mechanism in the SPS process is responsible for the enhancement of magnetic properties of SPSed compacts.     

Densification and Grain Growth of Porous Alumina Compacts

Densification and grain growth of porous alumina compacts during various high-temperature processes were investigated. Experimental data were obtained for densification and grain growth of alumina powder during hot pressing. A set of constitutive equations was proposed based on the constitutive equations by Helle et al. ¹ for hydrostatic response and by Rahaman et al. ² for deviatoric response. Theoretical results from the proposed constitutive equations were compared with various experimental data for alumina powder compacts in the literature, including pressureless sintering, sinter forging, and hot pressing. The proposed model well predicts the densification and grain growth of alumina compacts.     

Laser shock wave consolidation of micropowder compacts of fully stabilised zirconia with addition of nanoparticles

Abstract

Abstract

Laser shock waves were utilised to sinter green micropowder compacts (average particle size?=?16?μm) of cubic crystalline form of ZrO₂/8?mol.‐%Y₂O₃ (yttria stabilised zirconia) with and without the addition of nanoparticles (average particle size?=?45?nm) of identical composition for 0, 25 and 50% molar concentrations. Results indicated that yttria stabilised zirconia micropowder compacts with 0% nanoparticles excessively cracked and chipped, while those containing 25 and 50% nanoparticles underwent smooth sintering without any crack formation. Hardness increase of up to 64% was found in the laser shock compacted samples; however, the per cent increase in hardness was lower for the compacts with higher concentration of nanoparticles. Thermal conductivity measurements indicated that the addition of nanoparticles dramatically reduced the conductivity by nearly 50%. Laser shock waves have thus potential to make novel advances in the state‐of‐the‐art densification of ceramics.     

Hot‐Pressing Kinetics and Densification Mechanisms of Boron Carbide

The hot‐pressing kinetics of boron carbide at different stages in the hot‐pressing process was investigated. Based general densification equation and pore‐dragged creep model, the densification and grain growth kinetics were analyzed as a function of various parameters such as sintering temperature, sintering pressure and dwell time. Stress exponent of n ≈ 3 at the initial dwell stage suggests the plastic deformation may dominates the densification. The further TEM observations and the calculation based on effective stress and plastic yield stress also indicate that plastic deformation may occur and account for the large increase in density at the initial stage of sintering. Calculated grain size exponent of m ≈ 3 suggests that the grain‐boundary diffusion dominates the densification at the final stage. During the final stage of sintering, grain growth may be determined by evaporation/condensation and grain‐boundary migration.     

Densification of alumina by SPS and HP: A comparative study

In this study, the densification of alumina by spark plasma sintering (SPS) was investigated and compared to conventional hot pressing. It was shown that SPS is very effective in the sintering of alumina leading to higher densities and allows to work at lower temperatures and with shorter sintering cycles. The effect of the heating rate is dependent on the heating mode (SPS or HP). The identification of active sintering mechanisms was attempted by an isothermal and an anisothermal methods, showing that other mechanisms probably related to electrical effects enhance the densification. We suggest the higher contribution of surface diffusion mainly during the initial stage of sintering and an influence of the presence of impurities segregated at the grain boundaries. They could create conductive layers and also introduce ions with a lower valence than Al³⁺; defects are created in the surface layers and the diffusion of the species is increased.     

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.     

High field ZnO varistors prepared by spark plasma sintering

Abstract

ZnO varistors with submicrometre and nanoscaled microstructures and enhanced electrical properties were prepared by spark plasma sintering (SPS). The densification, grain size and switch field of the varistors were compared with those of hot pressed material. The switching field increased with decreasing grain size, and very rapidly below 500 nm. Switching fields up to 180 kV cm^?1 were obtained for ceramics with submicrometre grain sizes (380 nm). This is nearly two orders of magnitude higher than those currently reported for commercial ZnO varistors. A nano powder, prepared by high energy milling, was sintered to a high density at much lower temperatures compared with the submicron powders and had a nanoscale grain size (45 nm). The nanoceramic broke down dielectrically under very high fields (>260 kV cm^?1) before a varistive response was apparent.     

Sintering and densification mechanisms of tantalum carbide ceramics

Dense tantalum carbide (TaC) ceramics were prepared using TaC nanopowder via spark plasma sintering (SPS). The effects of the sintering temperature and applied pressure on the densification and grain growth behaviour of TaC ceramics were investigated. The results showed that high temperature and pressure promoted sintering densification, while their increase caused an increase in the grain size of TaC ceramics. A highly dense TaC ceramic (∼97.19%) with a fine grain size of 2.67 μm was obtained by sintering at 1800 °C for 10 min under 80 MPa. The Vickers hardness, Young's modulus and fracture toughness were 15.60 GPa, 512.66 GPa and 3.59 MPa·m^1/2, respectively. The densification kinetics were investigated using a creep deformation model. Diffusion and grain boundary sliding were proven to be the dominant densification mechanisms based on the stress and grain size exponents combined with the microstructural characteristics. The apparent activation energy of the mechanism controlling densification was 252.94 kJ/mol.     

Spark plasma sintering and hot pressing of ZTA-NbC materials – A comparison of mechanical and electrical properties

Zirconia toughened alumina can be made electrically conductive and thus electric discharge machinable by addition of a percolating dispersion of niobium carbide. In order to boost the productivity of the sintering process spark plasma sintering was tested at identical temperature and pressure but shorter dwell than in hot pressing. SPS sintering parameters for ZTA-NbC are developed and spark plasma sintered ceramics are compared to the hot pressed benchmark.During SPS a percolating NbC backbone of niobium carbide grains is formed which enhances electrical conductivity but impedes densification. Identical strength at however higher sintering temperature is achieved by SPS but the fracture resistance and hardness were always superior in hot pressed samples. The monoclinic content of zirconia grains in as fired SPS samples is higher despite smaller average grain size and the transformation toughening effect is less pronounced. SPS promises economic benefits due to shorter dwell and cooling cycles.     

固相烧结——Ⅲ 实验：超细氧化锆素坯烧结过程中的 晶粒与气孔生长及致密化行为

研究了超细Y-TZP和YSZ粉料成型体在烧结中期的晶粒生长、气孔生长和致密化行为.根据作者前文     

Compaction and Pressureless Sintering of Zirconia Nanoparticles

Four nanometer-sized zirconia powders stabilized by 3 mol% Y₂O₃ were used for the preparation of dense bulk ceramics. Ceramic green bodies were prepared by cold isostatic pressing at pressures of 300–1000 MPa. The size of the pores in ceramic green bodies and their evolution during sintering were correlated with the characteristics of individual nanopowders and with the sintering behavior of powder compacts. Only homogeneous green bodies with pores of <10 nm could be sintered into dense bodies (>99% t.d.) at a sufficiently low temperature to keep the grain sizes in the range <100 nm. Powders with uniform particles 10 nm in size yielded green bodies of required microstructure. These nanoparticle compacts were sintered without pressure to give bodies (diameter 20 mm, thickness 4 mm) with a relative density higher than 99% and a grain size of about 85 nm (as determined by the linear intercept method).     

Is spark plasma sintering suitable for the densification of continuous carbon fibre - UHTCMCs?

For the first time we show that spark plasma sintering can efficiently replace hot pressing for the densification of UHTCMCs, in the present case ZrB₂/SiC composites reinforced with continuous carbon fibres. To this purpose, the same materials were first produced by hot pressing as baseline samples and then by spark plasma sintering (SPS) to compare microstructure and basic mechanical properties. A special emphasis was given to the study of interfaces, in case of both coated and uncoated carbon fibres.SPS allowed for faster sintering but required an adjustment of the temperature to avoid fibre degradation compared to hot pressing. With similar porosity levels, we observed a slight decrease of flexural strength (300 vs 470 MPa), and an improvement of fracture toughness (15 vs 10 MPa√m) for SPSed samples. SPS was proved to be an effective method for the consolidation of continuous fibre reinforced UHTC composites.     

Construction and validation of master sintering curve for TiO2 for pressureless sintering

Abstract

One of the ultimate objectives for sintering research is to predict densification results under different thermal profiles for a given processing method. This paper studies the construction and validation of the master sintering curve (MSC) for rutile TiO₂ for pressureless sintering. The MSC was constructed using dilatometry data at two heating rates and was then validated using isothermal holds at three different temperatures. The scanning electron microscopy (SEM) observation shows that the partially sintered samples have the same density under different heating procedures, which demonstrates that the assumptions of the model are reliable. The concept of the MSC could be used to predict the sintering shrinkage and final density and calculate the activation energy. A value of 105 kJ mol^-1 for TiO₂ was obtained. The MSC could be applied to predict the sintering profile to prepare ceramics with required density and a minimum of grain growth.     

Hot pressing of nanocrystalline zinc oxide compacts: Densification and grain growth during sintering

Sintering behavior of nanocrystalline zinc oxide (ZnO) powder compacts using hot pressing method was investigated. The sintering conditions (temperature and total time) and results (density and grain size) of two-step sintering (TSS), conventional sintering (CS) and hot pressing (HP) methods were compared. The HP technique versus CS was shown to be a superior method to obtain higher final density (99%), lower sintering temperature, shorter total sintering time and rather fine grain size. The maximum density achieved via HP, TSS and CS methods were 99%, 98.3% and 97%, respectively. The final grain size of samples obtained by HP was greater than that of TSS method. However, the ultra-prolonged sintering total time and the lower final density (88 ks and 98.3%) are the drawbacks of TSS in comparison with the faster HP (17 ks and 99%) method.     

Spark plasma sintering of lead phosphovanadate Pb3(VO4)1.6(PO4)0.4

Lead phosphovanadates can be used as reactants for the synthesis of iodoapatite. Because of its high chemical durability, iodoapatite has considerable potential interest for immobilizing radioactive iodine. Iodine-bearing compounds must be synthesized and consolidated at low temperatures to avoid iodine volatilization. Spark plasma sintering (SPS) thus appears to be a suitable sintering process because of its short processing time. This paper deals with spark plasma sintering of lead phosphovanadate powder prepared mechanically by attrition and planetary ball milling. The influence of sintering parameters such as the heating rate, temperature, and holding time on the degree of densification and the microstructure of bulk materials is discussed. The bulk characteristics were directly correlated with the shrinkage curves. The powder characteristics were determined (grain size and size distribution, specific area, crystallite size, etc.) to explain the singular sintering behavior of the attrited powder; we also investigated whether the latter exhibited the same singular behavior during conventional sintering and hot pressing.     

Microstructure andphase stability of Y–PSZ codoped with MgO or CaO prepared via polymeric route

Abstract

Fully dense nanostructured Y-PSZ ceramics with microstructural uniformity and stable high temperature zirconia phases were prepared by hot pressing at 1400°C. The addition of 1 mol-% MgO or CaO as codopant has a significant influence on grain growth characteristics. Addition of MgO tends to promote densification during sintering and assists in the preparation of nanosized material (<200 nm grain size) with uniform microstructure. X-ray diffraction investigations of samples hot pressed at 35 MPa and 1400°C for 20 min and thermally etched at 1350°C for 3 h showed the presence of three zirconia phases, cubic, tetragonal, and monoclinic. The existence of the cubic phase with the two other phases is associated with a fine crystallite structure. T his desirable microstructure, combined with good stabilisation of the high temperature phases, was recorded in nanostructured samples codoped with 1 mol-% of either MgO or CaO.     

Nanostructure and bimodal structure of Si3N4 ceramics developed by spark plasma sintering method

Abstract

The densification of high energy ball milled Si₃N₄ nanopowders through spark plasma sintering was investigated. Nanoceramics of Si₃N₄, with fine microstructure, comprising of grains with a diameter of ～70 nm, were produced after sintering at 1600°C for 5 min in N₂ atmosphere with a fast heating rate of 300 K min^?1. The size and the aspect ratio of Si₃N₄ grains increased with decreasing heating rate and increasing holding time and temperature. Post-annealing of sintered ceramics at 1850°C for 3 h favoured development of a self-reinforced bimodal microstructure containing large elongated grains.     

Consolidation of ceramic nanopowders

Abstract

This review is dedicated to the problems of nanostructured ceramics consolidation.

Laboratory practice in recent years has displayed several potentially important technologies for consolidation of ceramic nanopowders, such as spark plasma sintering, high pressure sintering and rate controlled sintering. The grain growth factor in these processes was found to be less than 10. These advanced technologies have to be adapted to consolidation of nanopowders and require nanopowders specifically designed for consolidation purposes. When adapted to nanopowders, these techniques must be accomplished in rapid rate mode to eliminate residual porosity and retain nanosize grains. Practical verification, however, has exposed problems such as large residual porosity, stable pores in triple junctions, defective grain boundaries and intensive grain growth. All these problems can be avoided when the temperature–pressure–time schedule of sintering is optimised with respect to minimal grain growth.     

Densification mechanisms of UO2 consolidated by spark plasma sintering

Despite the growing interest in the spark plasma sintering (SPS) of uranium dioxide, its sintering mechanisms have yet to be studied in great detail. Herein we propose a direct method to calculate the apparent activation energy for densification, Q_act, and the stress exponent, n, for SPS of nearly stoichiometric UO₂. A set of experiments performed at different heating rates (CHR) and different pressures levels allowed us to calculate Q_act and n, respectively, though we were limited to a theoretical density between 50% to 75 %. The master sintering curve was employed as a complementary method to compare Q_act. The average values were Q_act =96 kJ/mol (CHR), Q_act = 100 kJ/mol (MSC) and n = 1.4. We have therefore proposed grain boundary diffusion coupled with grain boundary sliding as the densification mechanism. The activation energy in SPS tends to be lower compared with that in other processes like conventional sintering (250?450 kJ/mol), creep (350?550 kJ/mol) and hot pressing (222 kJ/mol and 480 kJ/mol).This decrease could be due to the effect of the electric field combined with the higher heating rates, typical of SPS.