Moderate temperature sintering of BaZr0.8Y0.2O3-δ protonic ceramics by A novel cold sintering pretreatment

The state-of-the-art protonic ceramic conductor BaZr_0.8Y_0.2O_3-δ (BZY20) requires an extremely high sintering temperature (≥1700 °C) to achieve the desired relative density and microstructure necessary to function as a proton conducting electrolyte. In this work, we developed a cold sintering pretreatment assisted moderate-temperature sintering method for the fabrication of high-quality pure BZY20 pellets. BZY20 pellets with high relative density of ~94% were fabricated with a final sintering temperature of 1500 °C (200 °C lower than the traditional sintering temperature). A comparison with BZY20 control samples indicated that the proper amount of BaCO₃ introduced on the BZY20 particle surface and the high green density achieved by cold sintering pretreatment were the main drivers for lowering the sintering temperature. The electrical conductivity measurement by electrochemical impedance spectroscopy showed that the as-prepared BZY20 pellets have a proton conductivity comparable to the state-of-the-art values. The cold sintering pretreatment outlined in this work has the potential to lower the sintering temperatures for similar types of protonic ceramic materials under consideration for a wide range of energy conversion and storage applications.     

Pressure-assisted flash sintering of ZnO ceramics

Implementing pressure-assisted flash sintering of ZnO powder without pretreatment by a new experimental configuration is presented. Rapid and energy-concentrated heating of electrode-sample-electrode area by induction heating allows preheating and flash sintering of loose-pack powder in the die with pressure assistance. Using an insulated die enables the current to flow through the sample during flash sintering. ZnO ceramics with a relative density of 95.1% can be achieved in less than 3 min. The whole process includes 104 s of preheating by a low-power induction heating device and 30 s of flash sintering assisted by a pressure of 26 MPa using the pulsed direct current (DC). The process characteristics of pressure-assisted flash sintering using the pulsed DC are discussed. The effect of pressure on densification and grain size is analyzed in detail, and some potential mechanisms are provided.     

A novel mixing method for powder metallurgy copper-carbon nanotube composites

In this study, copper matrix composite materials with different ratios of carbon nanotubes were produced. The biggest problem faced in the production of carbon nanotube-reinforced composites is that carbon nanotubes do not distribute homogeneously in the matrix. A novel mixing technique was applied to overcome this problem. Hot pressing was used in sample production. A second high-pressure densification process was applied following the hot pressing process for enhancing the properties. The properties of both the hot-pressed specimens and the specimens to which a second high-pressure densification process was applied were characterized with the density measurements, microstructure examinations, and mechanical tests. The microstructure examinations showed that carbon nanotubes could be distributed homogeneously in the copper matrix with the mixing process applied. It was found out that the high-pressure densification process applied following the hot-pressing process increased the relative density and thus, all mechanical properties.     

Effect of the calcium alumino-titanate particle size on the microstructure and properties of bauxite-SiC composite refractories

Alkali resistance and thermo-mechanical properties of the transition zone of cement rotary kilns refractories are the key factors affecting their service life. Calcium alumino-titanate (CAT) containing bauxite-SiC composites were prepared using bauxite, SiC, CAT, Guang Xi white clay, α-alumina, and metallic silicon powder as starting materials and Al(H₂PO₄)₃ as the binder. The effects of the CAT particle size on the phase composition, microstructure, thermo-mechanical properties, and alkali resistance of the CAT-containing bauxite-SiC composites during firing were investigated. The results reveal that the CAT particle size strongly affects the composites’ microstructure and sintering densification. With decreasing particle size, the particle-particle and particle-matrix interfacial bonding deteriorates gradually. When CAT particles are added, the specimens show higher strength, refractoriness under load, and residual rupture strength than the specimens with fine CAT powders. Specimens with fine CAT powders show lower coefficient of thermal expansion compared to the specimens with CAT aggregates. The alkali attack test confirms that the bauxite-SiC composite refractories with CAT aggregates show better alkali resistance than those with CAT fine powder. According to the alkali mechanism, 1) K vapors penetrate the specimen through the open and connected pores and cracks, 2) K vapors react with anorthite and corundum to form kalsilite accompanied by the formation of a liquid phase and new cracks.     

Temperature stability of a pure metakaolin based K-geopolymer: Part 2. Variations in the mesoporous network and its rehydration stability

The thermal behavior of a model MK-based K-geopolymer was investigated between room temperature and 1400°C in order to evaluate its potentiality for high-temperature applications. The purpose of our study was to monitor the behavior of a geopolymer during a temperature rise in order to better understand its variations with respect to temperature. The works from the present paper focus only changes in the porous network; it follows a first part devoted to variations in the mineral matrix. The results obtained here show that the geopolymer material preserves its porous integrity up to 800°C, while maintaining the reversibility of water exchanges corresponding to about 25 weight percent. Together with the results of part 1, the findings of this study allow us to affirm that geopolymer materials are only very little affected by temperatures up to 800°C, or even 900°C (keeping its mesoporous amorphous structure).     

Effect of transition metal doping on the sintering and electrochemical properties of GDC buffer layer in SOFCs

A dense Ce_0.9Gd_0.1O_2−d (GDC) interlayer is an essential component of the SOFCs to inhibit interfacial elemental diffusion between zirconia-based electrolytes (eg YSZ) and cathodes. However, the characteristic high sintering temperature of GDC (>1400°C) makes it challenging to fabricate an effective highly dense interlayer owing to the formation of more resistive (Zr,Ce)O₂ interfacial solid solutions with YSZ at those temperatures. To fabricate a useful GDC interlayer, we studied the influence of transition metal (TM) (Co, Cu, Fe, Mn, & Zn) doping on the sintering and electrochemical properties of GDC. Dilatometry data showed dramatic drops in the necking and final sintering temperatures for the TM-doped GDCs, improving the densification of the GDC in the order of Fe > Co > Mn > Cu > Zn. However, the electrochemical impedance data showed that among various transition metal dopants, Mn doping resulted in the best electrochemical properties. Anode supported SOFCs with Mn-doped, nano, and commercial-micron GDC interlayers were compared with regard to their performance and stability levels. Although all of the SOFCs showed stable performance, the SOFC with the Mn-doped GDC interlayer showed the highest power density of 1.14 W cm⁻² at 750°C. Hence, Mn-doped GDC is suggested for application as an effective diffusion barrier layer in SOFCs.     

Preparation of fully dense and magnetically controllable CaO-Al2O3-SiO2-Na2O-Fe3O4 glass ceramics by hot pressing

Fully dense and magnetically controllable glass ceramics was successfully synthesized by method of hot pressing using CaO-Al₂O₃-SiO₂-Na₂O glass powder and Fe₃O₄ powder as raw materials. The influences of sintering temperature and time, content and particle size of Fe₃O₄, as well as particle size of glass powder on the densification and magnetic properties of samples were investigated. It was found that the saturation magnetization gradually increased with increasing magnetite content. In addition, the samples containing smaller size magnetite particles had a higher coercivity. However, for samples using smaller size glass powder, magnetite particles could partially dissolve into the glass matrix, which led to the decrease of saturation magnetization and the increase of coercivity. It was also concluded that the precipitation of crystalline phase from smaller size glass powder caused the decrease of degree of densification, and after decreasing the sintering temperature, the degree of densification of product was enhanced.     

Hardness and toughness improvement of SiC-based ceramics with the addition of (Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2

The influences of different contents ranging 0–15 wt% of high-entropy boride (HEB) (Hf_0.2Mo_0.2Ta_0.2Nb_0.2Ti_0.2)B₂ on the mechanical properties of SiC-based ceramics using Al₂O₃-Y₂O₃ sintering additives sintered by spark plasma sintering process were investigated in this study. The results showed that the introduction of 5 and 10 wt% (Hf_0.2Mo_0.2Ta_0.2Nb_0.2Ti_0.2)B₂ could facilitate the densification and the grain growth of SiC-based ceramics via the mechanism of liquid phase sintering. However, the grain growth of SiC-based ceramics was inhibited by the grain boundary pinning effect with the addition of 15 wt% (Hf_0.2Mo_0.2Ta_0.2Nb_0.2Ti_0.2)B₂. The SiC-based ceramics with 15 wt% (Hf_0.2Mo_0.2Ta_0.2Nb_0.2Ti_0.2)B₂ showed the enhanced hardness (21.9±0.7 GPa) and high toughness (4.88±0.88 MPa·m^1/2) as compared with high-entropy phase-free SiC-based ceramics, which exhibited a hardness of 16.6 GPa and toughness of 3.10 MPa·m^1/2. The enhancement in mechanical properties was attributed to the addition of higher hardness of HEB phase, crack deflection toughening mechanism, and presence of residual stress due to the mismatch of coefficient of thermal expansion.     

压力和温度对铱铑合金热等静压致密化的影响

纯铱具有较大的致密度,将铑粉与铱粉合金化可以增强铱的高温抗氧化性能。设计了5组热等静压工艺参数制备Ir-20Rh合金。通过观察热等静压后样品的金相显微组织,测量合金的硬度、计算孔隙率以及致密度,研究压力和温度条件对铱铑合金热等静压致密化的影响。结果表明,随着压力和温度的升高,Ir-20Rh合金的致密度都会有所增加,且温度对Ir-20Rh合金致密度的影响幅度大于压力对Ir-20Rh合金致密度的影响。最佳热等静压工艺参数为在1300℃、140 MPa保温2 h。     

ZrB_2-SiC粉末与等离子射流场的相互作用

为了探究等离子喷涂制备ZrB_2-SiC涂层组织结构疏松、致密性差的原因,采用去离子水对经过射流场加热的粉体进行收集,对比前后粉体的组织结构特征以及物相变化。设计单颗粒沉积试验探究粉体的熔化状态以及变形颗粒的形貌特征,并与等离子喷涂制备涂层进行对应分析。结果表明,由于"涡流效应"使得经过等离子射流场的ZrB_2-SiC粉体与卷入的氧气发生反应,粉体出现轻微氧化现象。经过等离子射流场后,ZrB_2-SiC粉体呈现3种形貌特征:表面光滑型、表面多孔型、表面团聚型。其原因与等离子射流温度场非均匀性以及粉体的飞行路径有关。变形颗粒呈现与之相对应的3种形貌特征:熔化充分颗粒、团聚堆积颗粒、以及介于两者间的半熔融半疏松颗粒。共晶组织包裹的ZrB_2颗粒容易在涂层中形成致密区,而团聚堆积的ZrB_2和SiC颗粒是涂层形成疏松区的主要原因。