Commenced in January 2007
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Edition: International
Paper Count: 11

Search results for: corundum

11 Oxidation States of Trace Elements in Synthetic Corundum

Authors: Ontima Yamchuti, Waruntorn Kanitpanyacharoen, Chakkaphan Sutthirat, Wantana Klysuban, Penphitcha Amonpattarakit


Natural corundum occurs in various colors due to impurities or trace elements in its structure. Sapphire and ruby are essentially the same mineral, corundum, but valued differently due to their red and blue varieties, respectively. Color is one of the critical factors used to determine the value of natural and synthetic corundum. Despite the abundance of research on impurities in natural corundum, little is known about trace elements in synthetic corundum. This project thus aims to quantify trace elements and identify their oxidation states in synthetic corundum. A total of 15 corundum samples in red, blue, and yellow, synthesized by melt growth process, were first investigated by X-ray diffraction (XRD) analysis to determine the composition. Electron probe micro-analyzer (EPMA) was used to identify the types of trace elements. Results confirm that all synthetic corundums contain crystalline Al₂O₃ and a wide variety type of trace element, particularly Cr, Fe, and Ti. In red, yellow, and blue corundums respectively. To further determine their oxidation states, synchrotron X-ray absorption near edge structure spectrometry (XANES) was used to observe absorbing energy of each element. XANES results show that red synthetic corundum has Cr³⁺ as a major trace element (62%). The pre-edge absorption energy of Cr³⁺ is at 6001 eV. In addition, Fe²⁺ and Fe³⁺ are dominant oxidation states of yellow synthetic corundum while Ti³⁺and Ti⁴⁺ are dominant oxidation states of blue synthetic corundum. the average absorption energy of Fe and Ti is 4980 eV and 7113 eV respectively. The presence of Fe²⁺, Fe³⁺, Cr³⁺, Ti³⁺, and Ti⁴⁺ in synthetic corundums in this study is governed by comparison absorption energy edge with standard transition. The results of oxidation states in this study conform with natural corundum. However yellow synthetic corundums show difference oxidation state of trace element compared with synthetic in electron spin resonance spectrometer method which found that Ni³⁺ is a dominant oxidation state.

Keywords: corundum, trace element, oxidation state, XANES technique

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10 Sintering of Composite Ceramic based on Corundum with Additive in the Al2O3-TiO2-MnO System

Authors: Aung Kyaw Moe, Lukin Evgeny Stepanovich, Popova Nelya Alexandrovna


In this paper, the effect of the additive content in the Al2O3-TiO2-MnO system on the sintering of composite ceramics based on corundum was studied. The samples were pressed by uniaxial semi-dry pressing under 100 MPa and sintered at 1500 °С and 1550 °С. The properties of composite ceramics for porosity and flexural strength were studied. When the amount of additives increases, the properties of composite ceramic samples are better than samples without additives.

Keywords: ceramic, composite material, sintering, corundum

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9 Changes in Serum Neopterin in Workers Exposed to Different Mineral Dust

Authors: Gospodinka Prakova, Pavlina Gidikova, Gergana Sandeva, Kamelia Haracherova, Emil Slavov


Neopterin was demonstrated to be a sensitive marker of cell-mediated immune reactions which plays a key role in the interaction of monocyte / macrophage activation. The purpose of this work was to investigate changes in serum neopterin in workers exposed to different composition of mineral dust. Material and Methods: Serum neopterin was studied in 193 exposed workers, divided into three groups, depending on the mineral dust and content of the quartz in the respirable fraction. The I-st group-coal dust containing less than 2% free crystalline silica (n=44), II-nd group-coal dust containing over 2% free crystalline silica (n=94) and the III-rd group-mixed dust with corundum and carborundum (n=55). The control group was composed of 21 individuals without exposure to dust. Serum neopterin was investigated by Elisa method in ng/ml according to the instructions of the manufacturer. Results and Discussion: It was found significantly higher level of serum neopterin in exposed workers of mineral dust (2,10 ± 0,62 ng / ml), compared with that of the control group (1,10 ± 0,85 ng/ml; p < 0,05). Neopterin levels in workers exposed to coal dust (1,87 ± 0,42 ng / ml-I-st and 3,32 ± 0,77 ng / ml-II-nd group) were significantly higher compared with those exposed to a mixed dust (1,31±0,68 mg / ml-third) and control group (p < 0,05). No significant difference in serum neopterin when exposed to a mixed dust composed of corundum and carborundum (III-rd) and a control group. Conclusion: The results of this study indicate activates a cell-mediated immune response when exposed to a mineral dust. The level of that activation depends mainly on the composition of the dust and is significantly highest in workers exposed to coal dust.

Keywords: mineral dust, neopterin, occupational exposure, respirable crystalline silica

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8 Dry Sliding Wear Behaviour of Ti3SiC2 and the Effect of TiC on Its

Authors: Bendaoudi Seif-Eddine, Bounazef Mokhtar


Wear behaviour of Ti3SiC2 coating in contact sliding under dry condition have been investigated on different pressures (0.1-0.8 MPa) at various speeds from 5 to 60 m/s. The ball-on-disc sliding-wear test was performed in ambient air with a relative humidity of 20%. An equation has been proposed to predict wear rates and describe sliding wear caused by Corundum ball on the studied material. The results show how the wear rate, measured by mass loss, varies in the range of (0.6 – 3.8 x E-6 mm3/Nm) with normal sliding distance under various test conditions; it increases with increasing load and rapidly with speed. The influence of TiC impurities on the wear behaviours was also investigated.

Keywords: ball-on-disc, dry-sliding, Ti3SiC2, wear

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7 Metal Berthelot Tubes with Windows for Observing Cavitation under Static Negative Pressure

Authors: K. Hiro, Y. Imai, T. Sasayama


Cavitation under static negative pressure is not revealed well. The Berthelot method to generate such negative pressure can be a means to study cavitation inception. In this study, metal Berthelot tubes built in observation windows are newly developed and are checked whether high static negative pressure is generated or not. Negative pressure in the tube with a pair of a corundum plate and an aluminum gasket increased with temperature cycles. The trend was similar to that as reported before.

Keywords: Berthelot method, cavitation, negative pressure, observation

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6 Fabrication of Powdery Composites Based Alumina and Its Consolidation by Hot Pressing Method in OXY-GON Furnace

Authors: T. Kuchukhidze, N. Jalagonia, T. Korkia, V. Gabunia, N. Jalabadze, R. Chedia


In this work, obtaining methods of ultrafine alumina powdery composites and high temperature pressing technology of matrix ceramic composites with different compositions have been discussed. Alumina was obtained by solution combustion synthesis and sol-gel methods. Metal carbides containing powdery composites were obtained by homogenization of finishing powders in nanomills, as well as by their single-step high temperature synthesis .Different types of matrix ceramics composites (α-Al2O3-ZrO2-Y2O3, α-Al2O3- Y2O3-MgO, α-Al2O3-SiC-Y2O3, α-Al2O3-WC-Co-Y2O3, α-Al2O3- B4C-Y2O3, α-Al2O3- B4C-TiB2 etc.) were obtained by using OXYGON furnace. Consolidation of powders were carried out at 1550- 1750°C (hold time - 1 h, pressure - 50 MPa). Corundum ceramics samples have been obtained and characterized by high hardness and fracture toughness, absence of open porosity, high corrosion resistance. Their density reaches 99.5-99.6% TD. During the work, the following devices have been used: High temperature vacuum furnace OXY-GON Industries Inc (USA), Electronic Scanning Microscopes Nikon Eclipse LV 150, Optical Microscope NMM- 800TRF, Planetary mill Pulverisette 7 premium line, Shimadzu Dynamic Ultra Micro Hardness Tester DUH-211S, Analysette 12 Dynasizer.

Keywords: α-alumina, consolidation, phase transformation, powdery composites

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5 Preparation Static Dissipative Nanocomposites of Alkaline Earth Metal Doped Aluminium Oxide and Methyl Vinyl Silicone Polymer

Authors: Aparna M. Joshi


Methyl vinyl silicone polymer (VMQ) - alkaline earth metal doped aluminium oxide composites are prepared by conventional two rolls open mill mixing method. Doped aluminium oxides (DAO) using silvery white coloured alkaline earth metals such as Mg and Ca as dopants in the concentration of 0.4 % are synthesized by microwave combustion method and referred as MA ( Mg doped aluminium oxide) and CA ( Ca doped aluminium oxide). The as-synthesized materials are characterized for the electrical resistance, X–ray diffraction, FE-SEM, TEM and FTIR. The electrical resistances of the DAOs are observed to be ~ 8-20 MΩ. This means that the resistance of aluminium oxide (Corundum) α-Al2O3 which is ~ 1010Ω is reduced by the order of ~ 103 to 104 Ω after doping. XRD studies reveal the doping of Mg and Ca in aluminium oxide. The microstructural study using FE-SEM shows the flaky clusterous structures with the thickness of the flakes between 10 and 20 nm. TEM images depict the rod-shaped morphological geometry of the particles with the diameter of ~50-70 nm. The nanocomposites are synthesized by incorporating the DAOs in the concentration of 75 phr (parts per hundred parts of rubber) into VMQ polymer. The electrical resistance of VMQ polymer, which is ~ 1015Ω, drops by the order of 108Ω. There is a retention of the electrical resistance of ~ 30-50 MΩ for the nanocomposites which is a static dissipative range of electricity. In this work white coloured electrically conductive VMQ polymer-DAO nanocomposites (MAVMQ for Mg doping and CAVMQ for Ca doping) have been synthesized. The physical and mechanical properties of the composites such as specific gravity, hardness, tensile strength and rebound resilience are measured. Hardness and tensile strength are found to increase, with the negligible alteration in the other properties.

Keywords: doped aluminium oxide, methyl vinyl silicone polymer, microwave synthesis, static dissipation

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4 Transformation of Aluminum Unstable Oxyhydroxides in Ultrafine α-Al2O3 in Presence of Various Seeds

Authors: T. Kuchukhidze, N. Jalagonia, Z. Phachulia, R. Chedia


Ceramic obtained on the base of aluminum oxide has wide application range, because it has unique properties, for example, wear-resistance, dielectric characteristics, exploitation ability at high temperatures and in corrosive atmosphere. Low temperature synthesis of α-Al2O3 is energo-economical process and it is actual for developing technologies of corundum ceramics fabrication. In the present work possibilities of low temperature transformation of oxyhydroxides in α-Al2O3, during a presence of small amount of rare–earth elements compounds (also Th, Re), have been discussed. Aluminium unstable oxyhydroxides have been obtained by hydrolysis of aluminium isopropoxide, nitrates, sulphate, chloride in alkaline environment at 80-90ºC tempertures. β-Al(OH)3 has been received from aluminium powder by ultrasonic development. Drying of oxyhydroxide sol has been conducted with presence of various types seeds, which amount reaches 0,1-0,2% (mas). Neodymium, holmium, thorium, lanthanum, cerium, gadolinium, disprosium nitrates and rhenium carbonyls have been used as seeds and they have been added to the sol specimens in amount of 0.1-0.2% (mas) calculated on metals. Annealing of obtained gels is carried out at 70 – 1100ºC for 2 hrs. The same specimen transforms in α-Al2O3 at 1100ºC. At this temperature in case of presence of lanthanum and gadolinium transformation takes place by 70-85%. In case of presence of thorium stabilization of γ-and θ-phases takes place. It is established, that thorium causes inhibition of α-phase generation at 1100ºC, at the time in all other doped specimens α-phase is generated at lower temperatures (1000-1050ºC). During the work the following devices have been used: X-ray difractometer DRON-3M (Cu-Kα, Ni filter, 2º/min), High temperature vacuum furnace OXY-GON, electronic scanning microscopes Nikon ECLIPSE LV 150, NMM-800TRF, planetary mill Pulverisette 7 premium line, SHIMADZU Dynamic Ultra Micro Hardness Tester, DUH-211S, Analysette 12 Dyna sizer.

Keywords: α-Alumina, combustion, phase transformation, seeding

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3 Chemical Technology Approach for Obtaining Carbon Structures Containing Reinforced Ceramic Materials Based on Alumina

Authors: T. Kuchukhidze, N. Jalagonia, T. Archuadze, G. Bokuchava


The growing scientific-technological progress in modern civilization causes actuality of producing construction materials which can successfully work in conditions of high temperature, radiation, pressure, speed, and chemically aggressive environment. Such extreme conditions can withstand very few types of materials and among them, ceramic materials are in the first place. Corundum ceramics is the most useful material for creation of constructive nodes and products of various purposes for its low cost, easy accessibility to raw materials and good combination of physical-chemical properties. However, ceramic composite materials have one disadvantage; they are less plastics and have lower toughness. In order to increase the plasticity, the ceramics are reinforced by various dopants, that reduces the growth of the cracks. It is shown, that adding of even small amount of carbon fibers and carbon nanotubes (CNT) as reinforcing material significantly improves mechanical properties of the products, keeping at the same time advantages of alundum ceramics. Graphene in composite material acts in the same way as inorganic dopants (MgO, ZrO2, SiC and others) and performs the role of aluminum oxide inhibitor, as it creates shell, that gives possibility to reduce sintering temperature and at the same time it acts as damper, because scattering of a shock wave takes place on carbon structures. Application of different structural modification of carbon (graphene, nanotube and others) as reinforced material, gives possibility to create multi-purpose highly requested composite materials based on alundum ceramics. In the present work offers simplified technology for obtaining of aluminum oxide ceramics, reinforced with carbon nanostructures, during which chemical modification with doping carbon nanostructures will be implemented in the process of synthesis of final powdery composite – Alumina. In charge doping carbon nanostructures connected to matrix substance with C-O-Al bonds, that provide their homogeneous spatial distribution. In ceramic obtained as a result of consolidation of such powders carbon fragments equally distributed in the entire matrix of aluminum oxide, that cause increase of bending strength and crack-resistance. The proposed way to prepare the charge simplifies the technological process, decreases energy consumption, synthesis duration and therefore requires less financial expenses. In the implementation of this work, modern instrumental methods were used: electronic and optical microscopy, X-ray structural and granulometric analysis, UV, IR, and Raman spectroscopy.

Keywords: ceramic materials, α-Al₂O₃, carbon nanostructures, composites, characterization, hot-pressing

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2 New Findings on the Plasma Electrolytic Oxidation (PEO) of Aluminium

Authors: J. Martin, A. Nominé, T. Czerwiec, G. Henrion, T. Belmonte


The plasma electrolytic oxidation (PEO) is a particular electrochemical process to produce protective oxide ceramic coatings on light-weight metals (Al, Mg, Ti). When applied to aluminum alloys, the resulting PEO coating exhibit improved wear and corrosion resistance because thick, hard, compact and adherent crystalline alumina layers can be achieved. Several investigations have been carried out to improve the efficiency of the PEO process and one particular way consists in tuning the suitable electrical regime. Despite the considerable interest in this process, there is still no clear understanding of the underlying discharge mechanisms that make possible metal oxidation up to hundreds of µm through the ceramic layer. A key parameter that governs the PEO process is the numerous short-lived micro-discharges (micro-plasma in liquid) that occur continuously over the processed surface when the high applied voltage exceeds the critical dielectric breakdown value of the growing ceramic layer. By using a bipolar pulsed current to supply the electrodes, we previously observed that micro-discharges are delayed with respect to the rising edge of the anodic current. Nevertheless, explanation of the origin of such phenomena is still not clear and needs more systematic investigations. The aim of the present communication is to identify the relationship that exists between this delay and the mechanisms responsible of the oxide growth. For this purpose, the delay of micro-discharges ignition is investigated as the function of various electrical parameters such as the current density (J), the current pulse frequency (F) and the anodic to cathodic charge quantity ratio (R = Qp/Qn) delivered to the electrodes. The PEO process was conducted on Al2214 aluminum alloy substrates in a solution containing potassium hydroxide [KOH] and sodium silicate diluted in deionized water. The light emitted from micro-discharges was detected by a photomultiplier and the micro-discharge parameters (number, size, life-time) were measured during the process by means of ultra-fast video imaging (125 kfr./s). SEM observations and roughness measurements were performed to characterize the morphology of the elaborated oxide coatings while XRD was carried out to evaluate the amount of corundum -Al203 phase. Results show that whatever the applied current waveform, the delay of micro-discharge appearance increases as the process goes on. Moreover, the delay is shorter when the current density J (A/dm2), the current pulse frequency F (Hz) and the ratio of charge quantity R are high. It also appears that shorter delays are associated to stronger micro-discharges (localized, long and large micro-discharges) which have a detrimental effect on the elaborated oxide layers (thin and porous). On the basis of the results, a model for the growth of the PEO oxide layers will be presented and discussed. Experimental results support that a mechanism of electrical charge accumulation at the oxide surface / electrolyte interface takes place until the dielectric breakdown occurs and thus until micro-discharges appear.

Keywords: aluminium, micro-discharges, oxidation mechanisms, plasma electrolytic oxidation

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1 Biotite from Contact-Metamorphosed Rocks of the Dizi Series of the Greater Caucasus

Authors: Irakli Javakhishvili, Tamara Tsutsunava, Giorgi Beridze


The Caucasus is a component of the Mediterranean collision belt. The Dizi series is situated within the Greater Caucasian region of the Caucasus and crops out in the core of the Svaneti anticlinorium. The series was formed in the continental slope conditions on the southern passive margin of the small ocean basin. The Dizi series crops out on about 560 square km with the thickness 2000-2200 m. The rocks are faunally dated from the Devonian to the Triassic inclusive. The series is composed of terrigenous phyllitic schists, sandstones, quartzite aleurolites and lenses and interlayers of marbleized limestones. During the early Cimmerian orogeny, they underwent regional metamorphism of chlorite-sericite subfacies of greenschist facies. Typical minerals of metapelites are chlorite, sericite, augite, quartz, and tourmaline, but of basic rocks - actinolite, fibrolite, prehnite, calcite, and chlorite are developed. Into the Dizi series, polyphase intrusions of gabbros, diorites, quartz-diorites, syenite-diorites, syenites, and granitoids are intruded. Their K-Ar age dating (176-165Ma) points out that their formation corresponds to the Bathonian orogeny. The Dizi series is well-studied geologically, but very complicated processes of its regional and contact metamorphisms are insufficiently investigated. The aim of the authors was a detailed study of contact metamorphism processes of the series rocks. Investigations were accomplished applying the following methodologies: finding of key sections, a collection of material, microscopic study of samples, microprobe and structural analysis of minerals and X-ray determination of elements. The Dizi series rocks formed under the influence of the Bathonian magmatites on metapelites and carbonate-enriched rocks. They are represented by quartz, biotite, sericite, graphite, andalusite, muscovite, plagioclase, corundum, cordierite, clinopyroxene, hornblende, cummingtonite, actinolite, and tremolite bearing hornfels, marbles, and skarns. The contact metamorphism aureole reaches 350 meters. Biotite is developed only in contact-metamorphosed rocks and is a rather informative index mineral. In metapelites, biotite is formed as a result of the reaction between phengite, chlorite, and leucoxene, but in basites, it replaces actinolite or actinolite-hornblende. To study the compositional regularities of biotites, they were investigated from both - metapelites and metabasites. In total, biotite from the basites is characterized by an increased of titanium in contrast to biotite from metapelites. Biotites from metapelites are distinguished by an increased amount of aluminum. In biotites an increased amount of titanium and aluminum is observed as they approximate the contact, while their magnesia content decreases. Metapelite biotites are characterized by an increased amount of alumina in aluminum octahedrals, in contrast to biotite of the basites. In biotites of metapelites, the amount of tetrahedric aluminum is 28–34%, octahedral - 15–26%, and in basites tetrahedral aluminum is 28–33%, and octahedral 7–21%. As a result of the study of minerals, including biotite, from the contact-metamorphosed rocks of the Dizi series three exocontact zones with corresponding mineral assemblages were identified. It was established that contact metamorphism in the aureole of the Dizi series intrusions is going on at a significantly higher temperature and lower pressure than the regional metamorphism preceding the contact metamorphism.

Keywords: biotite, contact metamorphism, Dizi series, the Greater Caucasus

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