Archaeological ceramic amphorae from underwater marine environments: Influence of firing temperature on salt crystallization decay

Non-desalinated and desalinated fragments of Iberian, Italic and Tarraconensian amphorae sherds, found in different underwater marine environments, were compared to determine the decay caused by salt crystallization. Polarizing light and fluorescence optical microscopy, scanning electron microscopy coupled to energy dispersive X-ray spectroscopy, X-ray diffraction, ion chromatography and mercury intrusion porosimetry tests were conducted on the samples. Non-desalinated samples exhibit a variety of signs of degradation, especially those samples fired at lower temperature. Sherds fired at higher temperatures have a lower surface area and less connected porosity, which entail a lower absorption of soluble salts containing water and eventually less decay than those fired at lower temperatures. The composition and texture reached with the firing temperature is a key factor on salt crystallization decay and hence on the durability of these artefacts. This should be taken into account during desalination procedures that have to be optimized in order to be successful.     

等离子体热解煤制乙炔结焦机理的研究

利用新疆长焰煤为原料在2 MW等离子体热解煤制乙炔中试装置上进行热解实验时反应器壁上有结焦物生成。为了有助于实验中减少乃至避免它们的生成,通过SEM以及XRD方法对这些结焦物进行了研究。结果表明:位于反应器不同部位处的结焦物具有不同的微观形貌。在此基础上推测了结焦物的生成机理,即混合段壁侧结焦物通过铜的催化作用生成,第1以及第2反应段壁侧结焦物由煤粉碎片所组成;相应的气体侧结焦物则分别通过气-固、气-固以及焦油的吸附/去氢反应生成。结焦物的石墨化程度往下游方向逐渐增强,这一现象由结焦物自身石墨化属性所决定。     

Influence of firing temperature on the ceramic properties of clays from Campos dos Goytacazes, Brazil

The characteristics of two clays used for red ceramic production in Campos dos Goytacazes, southeast of Brazil, were investigated. Characterization was performed by X-ray diffraction, chemical analysis, as well as granulometric and plasticity measurements. Technological properties related to water absorption, linear shrinkage and flexural strength were obtained from specific tests. Samples were prepared by pressing clay bodies at 20 MPa, which were then fired at temperatures from 850 to 1200 °C. The results showed that both clays from three deposits are highly plastic due to the elevated percentage of kaolinitic clay minerals. The samples richer in clay minerals present higher linear shrinkage as well as a decrease in water absorption in comparison to the others. The effectiveness of these clays for red ceramic production has been discussed in terms of the Winkler diagram.     

Spectroscopic and porosimetry studies to estimate the firing temperature of some archaeological pottery shreds from India

The present study aims to estimate the firing temperature of archaeological pottery shreds collected from the three archaeological sites namely Maligaimedu, Thiruverkadu and Palur in Tamilnadu state, India. The spectroscopic method Fourier Transform Infrared Spectroscopy (FT-IR) has been employed to find the lower limit of firing temperature of the archaeological pottery shreds by refiring the samples to four different temperatures from 200 °C to 800 °C. From the observation of the hydroxyl band and appearance/disappearance of octahedral sheet structure the firing temperature of the shreds has been estimated. The samples from Maligaimedu site named as MM1, MM3 and MM5, Thiruverkadu and Palur samples were fired to a temperature above 800 °C and the samples of Maligaimedu MM2, MM4 and MM6 were fired below 800 °C. Additionally, porosimetry measurements such as water absorption and mercury intrusion (MIP) were also carried out. The samples MM1, MM3, TK2–TK6, PL3 and PL5 were fired to a temperature less than 900 °C and the other samples to less than 1000 °C.     

The influence of shaping and firing technology on ceramic properties of calcareous and non-calcareous illitic–chloritic clays

Two very different illitic–chloritic clays (calcareous and non-calcareous), both currently used in the Italian brickmaking industry, were used. Technological testing consisted in a simulation of the industrial processing performed at a laboratory scale. The pieces were obtained by three shaping techniques, pressing, extrusion and moulding, and fired at 1000 and 1100 °C, in fast and slow heating cycles. In each case their technological properties were studied. The microstructure and technological parameters of the ceramic pieces vary greatly, depending on the clay composition and the processing techniques. Pressing always produces pieces made from non-calcareous clay with the lowest drying and firing shrinkage, open porosity and water absorption. As it regards the calcareous clay, the lowest values of drying and firing shrinkage and water absorption are obtained by extrusion and moulding, respectively. The mechanical resistance, pore size distribution and critical pore diameter do not reflect clearly the influence of shaping techniques. Independently from the shaping technique adopted, all non-calcareous bodies show higher Maage's indexes than the calcareous ones. In any case, the Maage's durability factor is higher in extruded samples.     

High temperature oxidation of Zr- and Hf-carbides: Influence of matrix and sintering additive

Ultra-high temperature ceramics having melting points above 3500 K and high thermal conductivities are envisaged as future receivers of concentrating solar power plants. The high pressure and solar temperature reactor (Réacteur Hautes Pression et Température Solaire, REHPTS) implemented at the focus of the Odeillo 5 kW solar furnace was used to investigate the oxidation of three refractory carbides containing different sintering additives (HfC/MoSi₂, ZrC/MoSi₂, ZrC/TaSi₂) that could be considered as promising candidates. The concentration of the additive, TaSi₂ or MoSi₂, was 20 vol%. Each kind of sample was oxidized in air for 20 min at 1800, 2000 and 2200 K. Experiments were filmed using a video camera and the gaseous phases were analyzed in situ by mass spectrometry. Various post-test characterizations have shown that the nature of the carbide and additive strongly affects the composition of the oxide layer and therefore the high-temperature behaviour.     

Effect of polymer concentration,needle diameter and annealing temperature on TiO2-PVP composite nanofibers synthesized by electrospinning technique

In this study, TiO₂-PVP nanofibers were successfully synthesized on an aluminium collector by using cost-effective electrospinning technique. The nanofibers were prepared at different polymer concentrations, needle diameters and annealing temperatures and properties were studied by various characterizations. The structural properties were studied by X-ray diffraction (XRD) and Raman spectroscopy techniques. Surface morphology and elemental analysis of the samples were investigated by scanning electron microscopy (SEM) attached with energy dispersive spectroscopy (EDS). The optical properties were carried out by UV–Visible absorption spectroscopy (UV–Vis). By varying the polymer concentration and needle diameter, the effect of viscosity and surface tension on the formation of TiO₂-PVP nanofibers was clearly observed by SEM micro images. EDS spectrum shows effective composition of pure TiO₂ nanofibers. XRD peaks observed at temperatures 500 °C, 700 °C and 900 °C confirmed the anatase, mixed and rutile phases of TiO₂ nanofibers respectively. Raman studies also confirmed these phases of TiO₂ nanofibers. The optical band-gap values calculated using Kubelka-Munk function lies in the range of 3.02–3.22 eV.     

Influence of mineral admixtures on mechanical properties of self‐compacting concrete under elevated temperature

Self‐compacting concrete (SCC) is a form of concrete that is capable of flowing into the congested interior of formwork and consolidating under the action of its own weight without segregation and bleeding. In the present investigation, an attempt has been made to study the effect of elevated temperature on mechanical properties of SCC specimens made with different mineral admixtures that were heated from 27 to 900 °C and cooled by air or water. Silica fume, flyash, metakaolin were used as mineral admixtures. Master Glenium was used as superplasticizer, and Glenium Stream 2 was used as viscosity modifying agent. Mechanical properties of the cooled specimens such as compressive strength, tensile strength, flexural strength, and modulus of elasticity were found. Compressive, tensile, and flexural strengths of specimens were found to decrease by 73.18%, 65.05%, and 63.2%, and 85.2%, 83.52%, and 83.56% for the specimens with metakaolin that were heated and cooled by air and water, respectively. Similar reductions were found for the SCC specimens made with silica fume and flyash. Microstructure investigation has been carried out on SCC samples using scanning electron microscope and X‐ray diffraction analytical techniques to understand the effect of temperature on decrease in strength. Copyright © 2016 John Wiley & Sons, Ltd.     

The effect of SPS parameters on the production of yttria transparent ceramic

In this work, the spark plasma sintering (SPS) of commercial yttria nanopowder is investigated. The SPS parameters such as sintering temperature, applied pressure, and dwell time are varied. Densification without grain growth occurring at occurred up to a sintering temperature of 1400°C and grain growth without further densification taking place at the higher temperature. The optimum sample was obtained at a temperature of 1400°C with a pressure of 70 MPa and dwelling time of 15 minutes. The highest relative density of 99.8% and the average grain size of 1.26 μm were obtained at 1400°C. The yttria ceramic annealed at 1200°C had the in-line transmission of 5%-70% and 70%-82% in the visible and infrared wavelength region, respectively. The measurements of hardness and fracture toughness characteristics of the transparent yttria ceramic showed 9.2 GPa and 2.24 MPa.m^1/2, respectively.     

烧成温度对高铬砖显微结构的影响

利用扫描电子显微镜分析了 170 0℃、174 0℃、1780℃、182 0℃和 186 0℃烧成后高铬砖的显微结构。结果表明 :高铬砖的烧成温度不是越高越好 ,而是有一个合适的烧成温度 174 0℃。在该烧成温度下制得的高铬砖 ,其基质中的Cr2 O3晶粒尺寸适中 ,基质组织结构致密 ,基质和颗粒结合紧密 ,无裂纹 ,并且其力学性能最佳。     

温度对水葫芦热解特性的影响

水葫芦是一种水体污染物,其蕴藏着大量的能量。为了使水葫芦变废为宝,解决环境污染的同时,提供一定的能源补给,在热重分析的基础上,采用固定床,借助GC、GC-MS、XRD和SEM等技术手段,研究不同热解温度段水葫芦热解后的气、液、固三相产物的特性。结果表明,低温热解温度段275～375 ℃生成的生物油不仅产率增加较大,而且生物油酸类较少、酯类较多,热值较高,品质明显优于高温热解温度段450～550 ℃生成的生物油;但高温热解温度段450～550 ℃下,明显有利于气体产物中高热值气体H2和CO的生成,生物质炭的结构孔径较大,晶体相态更加稳固,可见热解温度对三相产物的影响很大。     

The Red Slip Ware from Motya (Sicily,Italy): A multi-analytical approach for determining the production technology and the nature of the raw materials

This study is focused on the Phoenician Red Slip Ware, a cultural and chronological marker, unearthed in the archaeological site of Motya. The vessels are dated back from the 8^th to early 5^th century B.C. The ceramics were investigated using Optical Microscopy (OM), X-ray Powder Diffraction (XRPD), Scanning Electron Microscopy (SEM) and Electron Microprobe Analysis (EMPA). The results on mineralogical assemblage, microstructure and chemical composition of the ceramic body suggest a careful selection of the raw materials (i.e., clay and tempers) and firing temperature in the range > 750 and <850 °C, under oxidizing conditions. The Red Slip decoration consists of clay-rich coating, enriched in Fe. The comparison of the mineralogical and chemical composition of local clay deposits with that of the ceramic production allowed distinguishing local from imported vessels.     

Effects of firing temperature on the microstructures and properties of porous mullite ceramics prepared by foam-gelcasting

Porous mullite ceramics were prepared at 1300–1600°C for 2?h via a foam-gelcasting route using industrial-grade mullite powders as the main raw material, Isobam 104 as the dispersing and gelling agent, triethanolamine lauryl sulphate as the foaming agent and sodium carboxymethyl cellulose as the foam stabilising agent. The effects of firing temperature on the sintering behaviour of green samples as well as microstructures and properties of final porous mullite products were investigated. With increasing the temperature from 1300 to 1600°C, linear shrinkage and bulk density values of fired samples increased, whereas their porosity decreased. Mechanical strength and thermal conductivity values of fired samples decreased with increasing their porosities. Even at a porosity level as high as 79.4%, compressive and flexural strengths of fired samples (with average pore size of 314?μm) remained as high as 9.0 and 3.7?MPa, respectively, and their thermal conductivity (at 200°C) remained as low as 0.21?W?(m^?1?K^?1).     

Effect of dual reinforced ceramic particles on high temperature tribological properties of aluminum composites

The nature and distribution of hard ceramic particles in composite materials influences the properties to greater extent. In the present work, the role of hard ceramic reinforced particles on the tribological behaviour of aluminum metal matrix composites consisting of single (SRP) and dual reinforced particles (DRP) is studied at different temperatures. Zircon sand and silicon carbide particles of size 20–32 μm were used as reinforcement in commercial grade LM13 piston alloy. Composites of dual reinforced particles in aluminum matrix (DRP-AMCs) were developed by mixing 15 wt% reinforced particles by two step stir casting technique. The wear behaviour of DRP-AMCs and SRP-AMCs (single reinforced particles aluminum matrix composite) was investigated using a pin-on-disc method at high temperatures under dry sliding condition. The microstructural examination of developed composites shows globular and finely distributed eutectic silicon in the vicinity of the reinforced particles. Metallographic investigation revealed that the wear zone of the SRP composite consisted of a hardened layer, which is responsible for high wear loss observed in the SRP composite. The results further indicate a transition in the wear mode that occurs after 150 °C for all composites. Study reveals that the dual reinforcement of particles enhances the wear resistance as compared to single reinforced particles if mixed in a definite ratio. A combination of 3% zircon sand and 12% silicon carbide particle reinforced composite exhibits better wear resistance as compared to other combinations at all the temperatures for low and high loads both.     

The effect of self-healing process on the strength increase in clay

In this study, the effect of an additive with nano-montmorillonite brand on the process of self-healing on clay soil was considered. Laboratory tests include Atterberg limits and unpressurized compressive strength on the natural soil and soil samples contain different weight percentages of the additive. The results reveal that the addition of the additive up to 5% of the soil dry weight led to significant changes in the physical and mechanical properties of improved soil such as increasing plasticity index, increasing compressive strength and consequently, increasing the self-healing on clay soil. These changes are functions of the weight percent of the additive and the age of the samples. Moreover, laboratory results were investigated by SEM and FESEM images. Data was collected from uniaxial test and Scanning Electron Microscope images indicate that the maximum amount of self-healing occurred in the samples with 5% nano-clay on the sixtieth day after the initial failure.     

TiO2加入量对高炉渣微晶玻璃析晶的影响

以高炉渣微晶玻璃为研究对象,改变配料中晶核剂TiO2的含量,制得微晶玻璃样品. 以不同的升温速率对样品进行差热分析,根据升温速率和差热分析曲线上的晶化峰温度,采用3种不同的方法计算微晶玻璃样品的析晶活化能. 结果表明,随着TiO2含量的增加,析晶活化能呈现出先减小后增大的趋势,在TiO2的加入量为3.1%时,微晶玻璃的析晶活化能最低,此时拟合出的3种析晶活化能最小值分别为135.7, 143.9, 151.7 kJ/mol. 样品的红外谱图表明,TiO2的含量为3%~4%时析出晶体较多. TiO2含量为3%和4%的样品的X射线衍射图谱表明,样品中析出了以透辉石为主晶相、金红石为次晶相的晶体.     

Effects of sintering temperature on microstructure,properties, and crushing behavior of ceramic proppants

Ceramic proppants with excellent performance were successfully prepared by second grade bauxite. The phase structure and the microstructure were investigated via X-Ray diffraction and scanning electron microscopy. The results suggested that bulk density and apparent density constantly increased, while the breakage ratio gradually decreased with the increasing in sintering temperature. When the sintering temperature reached to 1500°C, the breakage ratio obtained lowest value of 3.6% under 52 MPa closed pressure, which satisfied the requirement of Chinese Petroleum and Gas Industry standard. Furthermore, the mode of fracture for ceramic proppants was transformed from intergranular fracture into transgranular fracture and open pores had larger influence than closed pores for breakage ratio of ceramic proppants.     

The study of the effect of gas-phase fluctuation on slag flow and refractory brick corrosion in the slag tapping hole of an entrained-flow gasifier

The service life of refractory brick in the slag tapping hole of the entrained flow gasifier was significantly lower than that in other locations. It was critically important to study the corrosion mechanism of refractory brick in the slag tapping hole for guiding industrial production. Considering the complex flow field in the slag tapping hole, the influence of gas velocity and temperature fluctuation on the service life of refractory brick was investigated in this study. The results showed th...     

Effects of elevated temperature on pumice based geopolymer composites

Abstract

Aluminosilicate type materials can be activated in alkaline environment and can produce geopolymer cements with low environmental impacts. Geopolymers are believed to provide good fire resistance so the effects of elevated temperatures on mechanical and microstructural properties of pumice based geopolymer were investigated in this study. Pumice based geopolymer was exposed to elevated temperatures of 100, 200, 300, 400, 500, 600, 700 and 800°C for 3?h. The residual strength of these specimens were determined after cooling at room temperature as well as ultrasonic pulse velocity, and the density of pumice based geopolymer pastes before and after exposing to high temperature was determined. Microstructures of these samples were investigated by Fourier transform infrared for all temperatures and SEM analyses for samples that were exposed to 200, 400, 600 and 800°C. Specimens, which were initially grey, turned whitish accompanied by the appearance of cracks as temperatures increased to 600 and 800°C. Consequently, compressive strength losses in geopolymer paste were increased with increasing temperature level. On the other hand, compressive strength of geopolymer paste was less affected by high temperature in comparison with the ordinary Portland cement. As a result of this study, it is concluded that pumice based geopolymer is useful in compressive strength losses exposed to elevated temperatures.     

XRD,SEM, and XPS Analysis of Soybean Protein Powders Obtained Through Extraction Involving Reverse Micelles

Soybean protein powders obtained by aqueous buffer and reverse micelle extractions were examined and characterized using X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction (XRD), and scanning electron microscopy (SEM). These analysis methods provided detailed information about elemental distributions, surface structure, and secondary and microstructures of the protein, respectively. XPS data revealed that the O and N atomic percentages of soybean protein surfaces obtained with bis(2‐ethylhexyl) sodium sulfosuccinate (AOT)/hexane reverse micelles were higher than those obtained with aqueous buffer, whereas the percentage of atomic C was lower. The ratios of nitrogen to carbon (N/C) on the surface of soybean protein obtained through the two extraction methods were similar. The O/C ratio for soybean protein obtained from AOT reverse micelles was large. The obtained results indicated that the reverse micelles could affect the C, O, and N components on the surface of soybean proteins. Moreover, XRD and SEM results also showed the influence of AOT reverse micelles, which lead to more β‐sheet and pore structures.