Influence of powder physicochemical characteristics on microstructural and optical aspects of YAG and Er:YAG ceramics obtained by SPS

The present work aims to establish a correlation between the characteristics of YAG and Er:YAG commercial powders produced by two different synthesis routes and sintered ceramic microstructures and their optical aspect by taking into account the influence of pressure applied during the Spark Plasma Sintering (SPS) process. Physical and chemical characteristics of the powders were compared using various techniques such as SEM, XRD, laser diffraction and chemical analyses. Their behaviours were evaluated through a rheological study, compressibility tests and dilatometry cycles using SPS. This paper pinpoints the most important powder features which influence the optical quality of YAG and Er:YAG ceramics. The optical quality is mainly affected by the porosity, related to powder characteristics that affect particle rearrangement, densification and grain growth. The applied pressure induces microstructural heterogeneities depending on the starting material used and resulting in core-shell aspects of sintered ceramics.     

Reinforcement effect of textured GnPs on advanced ceramics densified by SPS

Graphene nano-platelets (GnPs) are attractive reinforcement fillers for advanced ceramic materials. GnPs present interesting properties like mechanical reinforcement media, additive for improved electrical or thermal properties. The present study reports on the processing and performances of GnPs reinforced alumina based and ZrB₂ based ceramic matrices. In both systems, the effect of the GnPs has been determined for content up to 7.2 vol.%. The influence on the resulting properties due to the preferential orientation of the GnPs has been assessed. The high degree of orientation was tailored by the extrusion method used to pre-form the green compact.The densification was performed by Spark Plasma Sintering (SPS), allowing achievement of near full density compacts.The evolution of mechanical properties as a function of the GnPs content and their dependence on the reinforcing phase orientation is discussed. The evaluation of the electrical conductivity is reported.     

Processing of nano-SiC ceramics: Densification by SPS and mechanical characterization

β-SiC nanopowders with a mean particle size of 16.6 nm were obtained by laser pyrolysis. De-agglomeration of the powder was performed in an aqueous medium under magnetic stirring and ball-milling. Subsequently, green bodies were prepared by slip-casting of slurries. In this context, non-conventional densification routes such as Spark Plasma Sintering (SPS) with an applied pressure of 70 MPa allowed to achieve high final densities (96% TD). Different microstructures were obtained by varying the sintering temperature. Finally, the mechanical properties of the samples (hardness, toughness) were determined and a correlation between the final microstructures and the mechanical behavior was established.     

Tribological behavior of composites fabricated by reactive SPS sintering in Ti-Si-C system

In this study, wear and friction behavior of two based-composites from the Ti-Si-C system, (40 wt% TiC; 28 wt% Ti₅Si₃; 17 wt% Ti₃SiC₂) and (18 wt% TiC; 26 wt% Ti₅Si₃; 41 wt% Ti₃SiC₂) reinforced by 15 wt% of large size SiC (100-150 µm) particles were investigated. The four-phase composites exhibited approximatively the same friction coefficient (µ ~ 0.9) under high loads (10 N and 7 N). The composite with high Ti₃SiC₂ showed higher wear rate values by one order of magnitude. However, under 1 N, the composite with high TiC content showed a higher running-in period and a lower steady state µ value (0.37 after 1000 m sliding distance). Scanning electron microscopy, Energy Dispersive X-Ray and Raman spectroscopy analysis of the worn surfaces of the two composites revealed that oxidation was the dominant wear mechanism. The oxidation process and the removal kinetics of the oxides during sliding controlled the tribological behavior of the composites. The influence of processing variables on microstructures development and wear mechanisms of the composites is discussed.     

Gel-casting of transparent magnesium aluminate spinel ceramics fabricated by spark plasma sintering (SPS)

In this paper, a transparent magnesium aluminate spinel ceramic was fabricated through the newest colloidal gel casting method, using a synthetic powder with the average particle size of 90 nm and Isobutylene-Maleic Anhydride (ISOBAM) additive. ISOBAM served as both a dispersant and a gelation agent to achieve a dense body. Also, the suspension rheological behavior was optimized by the solid loading of 85 wt%, the additive content of 0.7 wt%, and the gelation time of 350 s. This led to a green body with a density equal to 65% of theoretical density and the green strength of 14.48 MPa. The results revealed that the reduction of porosity and the uniform distribution of pores in the green body (smaller than half of the initial powder particle size, 35 nm), as accompanied by spark plasma sintering (SPS), resulted in the final body density of 99.97%, as well as the high in-line transmittance of 86.7% at the wavelength of 1100 nm.     

Densification of monomodal quartz particle beds by tapping

A study has been undertaken to determine how the mean particle size of monomodal quartz particle beds and the bed preparation method affect initial and final bed apparent density and the kinetics of densification by tapping. The study was conducted on eight quartz particle size fractions obtained from a commercial quartz powder by sieving, each having a different mean particle size and a very narrow (monomodal) particle size distribution. The amplitude of the distribution and the particle shape were practically the same for all fractions. Densification experiments were conducted on the beds obtained with each fraction, using an assembly designed for this purpose. A kinetic model representing the densification process of monomodal powder beds by tapping is proposed, in which good relations are obtained between the parameters of the model and the foregoing variables.     

Densification behaviour and three-dimensional printing of Y2O3 ceramic powder by selective laser sintering

The selective laser sintering (SLS) of an yttria (Y₂O₃) ceramic powder was studied to understand both the effects of i) the initial yttria particle characteristics on the powder bed behaviour and ii) the process conditions (laser power, scanning speed, hatching space) on the sintering/melting of three-dimensionally printed objects. The roughness of the powder bed, a sensitive indicator of the layer bed quality, was determined through three-dimensional optical profilometry and the powder bed packing density was modelled using the discrete-element method. Complex shaped objects including spheres and open rings were successfully fabricated by the SLS three-dimensional printing. In addition, SLS cube-shaped samples were characterized by X-ray diffraction and scanning electron microscopy. The open pore volume fraction significantly decreased from 41% without a post-SLS heat treatment to 31% with a post-SLS heat treatment at 1750 °C for 20 h under secondary vacuum. Finally, an anisotropy in elastic properties has been highlighted, Young's modulus reaches 11 GPa in the stiffest direction.     

Rapid fabrication and phase transition of Nd and Ce co-doped Gd2Zr2O7 ceramics by SPS

A series of Nd and Ce co-doped Gd_2-xNd_xZr_2-yCe_yO₇ (0.0 ≤ x, y ≤ 2.0) ceramics were rapidly fabricated through spark plasma sintering (SPS) within 3?min. The effects of Nd and Ce contents on the phase composition, lattice parameter, active modes, microtopography and microstructure have been investigated in detail. XRD studies reveal that the compositions corresponding to 0.0 ≤ y ≤ 1.0 show a single phase and beyond 1.0 exhibit multiphase. The lattice parameters increase with elevated Nd and Ce content. The grains are densely packed on each other with cube-like shape, and the elements are almost homogeneously distributed in the compound. This synthetic method provides a simple pathway for the preparation of highly densified single phase ceramic at 1600–1700 ℃ for 3?min under pressure of 80?MPa.     

Defects and microstructure of highly conducting Al-doped ZnO ceramics obtained via spark plasma sintering

Al-doped ZnO ceramics were sintered by conventional sintering method and spark plasma sintering (SPS) respectively. Electrical properties and microstructure have been investigated by various measurements. The samples sintered via SPS exhibit a huge electrical conductivity, up to 3.0 × 10⁵ S/m at room temperature, which was much higher than that of the sample sintered via the conventional sintering. Structural and morphorlogical characterizations pointed out that the further incorporation of Al ions and the absence of a secondary phase, contribute to the increase of the carrier concentration. Raman spectroscopy revealed the occurrence of structural distortions and a disorder induced by Al doping. Photoluminescence spectra were interpreted by different electronic active defects such as the defect complexes (Al_Zn-Zn_i) which play a key for the high electrical conductivity. Thus, SPS and Al doping modified the microstructure and the concentration of the electronic active defects to ensure high electrical conductivities in doped ZnO-based ceramics.     

Scintillation and dosimeter properties of CaF2 transparent ceramics doped with Nd3+ produced by SPS

We have developed CaF₂:Nd transparent ceramics with varying doping concentrations of Nd by spark plasma sintering (SPS) and evaluated the optical, scintillation and dosimeter properties. The samples showed effective absorption peaks in the visible and near infrared regions due to the 4f-4f transitions of Nd³⁺. In scintillation properties, Nd³⁺ was also active and showed the 4f-4f radiative transitions of Nd³⁺ which appeared at 860 and 1064 nm under X-ray irradiation. In photoluminescence under 160 nm excitation, the samples showed emission peaks in the vacuum ultraviolet region due to the 5d-4f transitions of Nd³⁺. Furthermore, the samples showed thermally stimulated luminescence (TSL) exhibiting glow peaks at 100, 150 and 380 °C. Among the present samples the 5% Nd-doped sample showed the highest sensitivity which allowed to measure radiation dose from 0.1 to 1000 mGy with a good linear response.     

高温热机用陶瓷部件的研究与进展

本文着重讨论当前陶瓷基复合材料的在高温热机上的潜在应用情况，对陶瓷材料的要求及其在发动机上的使用趋势作了探讨，并就其目前最新工艺和制造方法作了探讨，对当前陶瓷发动机存在的问题进行了分析，认为仍需要对复合材料的界面以及高温使用的纤维加强进行研究，并就陶瓷材料部件在将来的发展作了预测。     

CuAlO2 thermoelectric compacts by SPS and thermoelectric performance improvement by orientation control

We fabricated CuO/Al₂O₃ green compacts from plate-like Al₂O₃ and granular CuO powders by multi-press forming and investigated the alumina orientation using Lotgering's method. The results showed that Al₂O₃ particles preferentially aligned perpendicular to the pressure direction and the orientation degree increased as the forming pressure was increased. We proposed a model describing the movement of the alumina particles to explain the pressure effect on their orientation. The orientation calculation was in good agreement with those by Lotgering's method. Furthermore, we prepared the CuAlO₂ compacts by regular or spark plasma sintering (SPS). However, the compacts sintered by SPS exhibited higher orientation degree and density than those produced by regular sintering. The electrical conductivity values of the orientation-controlled compacts sintered by SPS reached 770 S m⁻¹ at 928 K, which was close to that of CuAlO₂ single crystal. The power factor of the CuAlO₂ compacts with highest orientation degree is as high as 5.95 × 10⁻⁵ W m⁻¹ K⁻¹ at 928 K. Therefore, we can conclude that orientation control is an effective method to enhance the thermoelectric performance of compact polycrystalline CuAlO₂ bulks.     

Densification of powder compacts by vibration

Various packing methods such as vibration, shaking, etc., in addition to normal gravitational settling, can be often used to density powder compacts. Many issues relevant to this matter are of great importance in advanced ceramic powder processing. In the present work, the relaxation of structure due to vibration is addressed by using a computer experimental model based on Monte Carlo method. Packing structures, diffraction patterns, radial distribution functions are used for the characterization of structures. Bulk properties such as packing fraction and average height of the deposit are examined. The results agree well with those observed in model experiments, even with more implication.     

Preparation of β"-Al2O3 electrolytes by freeze-drying and SPS

Na-ionic conductivity and mechanical strength are two important parameters for β"-Al₂O₃ ceramics used as electrolyte materials. In this study, the ice-templating and freeze-drying processes were used to prepare uniformly porous Al₂O₃ powder with a certain degree of crystallographic orientation. With the help of spark plasma sintering (SPS) process, solid samples were fabricated from the porous power at a low temperature (1100 °C). Finally, highly conductive and highly strong β"-Al₂O₃ electrolytes were prepared after the solid samples were subject to further treatment at a high temperature (1600 °C). The scanning electron microscopy (SEM) results indicate that integration of the initial SPS process and further high-temperature sintering treatment have turned the freeze-dried Al₂O₃ powder to β"-Al₂O₃ samples whose grain structure is similar to the “brick-bridge-mortar” structure. Regarding such β"-Al₂O₃ samples, the bending strength parallel to the pressure direction is up to 273 MPa; the degree of crystallographic orientation, 0.25, and the ionic conductivity perpendicular to the pressure direction, 0.239 S cm^?1 at 350 °C. Therefore, it can be concluded that the combination of freeze-drying, SPS and an additional high-temperature sintering process has helped generate a structure that improves the ion mobility and bending strength of the β"-Al₂O₃ ceramic, and thereby improving its strength and ionic conductivity.     

Densification of nanocrystalline MgO ceramics by hot-pressing

Densification of pure nanocrystalline MgO powder with 10 nm particle size by hot-pressing was investigated in the temperature range 700–800 °C, applied pressure range 100–200 MPa, and for durations of up to 240 min. It was shown that significant densification under the pressure begins above 440 °C. Densities higher than 99.5% with grain size of 73 nm were achieved at 790 °C and 150 MPa for a 30 min duration. Remarkable densification from 90 to 99.5% was observed by temperature change from 700 to 790 °C, for which the grain size was doubled only. The final grain size decreased with increasing the applied pressure. Higher shrinkage rates and cumulative shrinkages were recorded by the application of pressure at 550 °C rather than from room temperature. The temperature at which the pressure was applied is crucial in determining the maximum shrinkage rate in the nanocrystalline compacts. This effect was related to the morphological changes of the particles caused by plastic deformation at lower temperatures. Analysis of the densification rate and its comparison to the literature data was in agreement with Coble creep, where self-diffusion of Mg²⁺ cations along the grain boundaries acts as a main densification mechanism.     

Densification of SiC by colloidal processing and SPS without sintering additives

Abstract

Silicon carbide is one of the most important ceramics used as structural and functional materials in a wide variety of applications. Many studies have reported the densification of SiC using oxide and nonoxide additives such as the Al₂O₃, B₄C and Al–B–C system. However, it is difficult to densify SiC at temperatures below 2000°C without sintering additives even if spark plasma sintering (SPS) is used. The authors attempted to densify SiC using colloidal processing and SPS without sintering additives. A commercially available SiC powder with the average particle size of 0·55 μm was used as the starting material. The densities of the green body prepared by slip casting and the sintered body by SPS were 65·5 and 98·7% respectively.     

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.     

Synthesis and Densification of Transparent Magnesium Aluminate Spinel by SPS Processing

Mixtures of elementary oxides, MgO–Al₂O₃, were used to fabricate transparent polycrystalline magnesium aluminate spinel specimens by means of the spark plasma sintering technique. A sintering aid, 1 wt% of LiF, was added to the mixed powder. The presence of the additive promotes the synthesis of spinel that starts at 900°C and is completed at 1100°C. The LiF additive wets spinel on its melting and promotes densification, which is completed at 1600°C. LiF vapor plays a cardinal role in eliminating residual carbon contamination and in the fully dense state, allows attaining a 78% level of optical transmittance. The optimal conditions for achieving adequate transparency were determined and the role of the LiF addition in the various stages of the process is discussed.     

利用SPS软件分析输气管道的瞬态工况

准确了解天然气管道的瞬时工况变化情况,对于管道运营管理部门来说,有助于其调度管理和制定管网系统的运行方案,并提前制定相应的应急措施,以此保障天然气管道系统的安全平稳运行。为此,收集了某天然气管道的相关基础资料,利用SPS仿真模拟软件建立某管道的水动力仿真模型,进行相关分析,并得到以下相关结论:当压缩机站内的压缩机组事故停机时,通过该站的瞬时流量变为零,进站压力上升,出站压力下降;天然气管道发生泄漏时,泄漏点处的上游流量瞬间上升,下游流量瞬间下降;天然气管道发生截断阀紧急关断时,通过前后阀门的流量变为零,通过此管段的流量也变为零,同时上游管段流量下降,处于不断储气的状态,压力不断增大。该分析结果对天然气管道的输送安全起到指导作用。     

Immobilization of simulated An3+ into synthetic Gd2Zr2O7 ceramic by SPS without occupation or valence design

To simplify the immobilized process of nuclear waste, synthetic Gd₂Zr₂O₇ ceramic was employed to immobilize simulated An³⁺ (Nd³⁺) by spark plasma sintering (SPS) without any ion occupation or valence design. Sintering and characterization of immobilized simulated An³⁺ with various doping amounts were carried out. The effects of Nd₂O₃ content on the phase composition, active modes, micro-graph and density of the sintered ceramics were investigated. When the Nd₂O₃ doped amount reached up to 50 mol%, the raw peak of Nd₂O₃ existed. The sintered ceramics kept a single fluorite phase when Nd₂O₃ solubility achieved to 40 mol%. The sintered ceramics presented a well crystalline phase and the elements distributed evenly. In addition, as the Nd₂O₃ doped amount increase, the density and Vickers hardness values of Nd₂O₃ doped sample decrease.