Search results for: powder x-ray diffraction
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 511

Search results for: powder x-ray diffraction

511 Behavior of Cu-WC-Ti Metal Composite Afterusing Planetary Ball Milling

Authors: A.T.Z. Mahamat, A.M. A Rani, Patthi Husain

Abstract:

Copper based composites reinforced with WC and Ti particles were prepared using planetary ball-mill. The experiment was designed by using Taguchi technique and milling was carried out in an air for several hours. The powder was characterized before and after milling using the SEM, TEM and X-ray for microstructure and for possible new phases. Microstructures show that milled particles size and reduction in particle size depend on many parameters. The distance d between planes of atoms estimated from X-ray powder diffraction data and TEM image. X-ray diffraction patterns of the milled powder did not show clearly any new peak or energy shift, but the TEM images show a significant change in crystalline structure of corporate on titanium in the composites.

Keywords: ball milling, microstructures, titanium, tungstencarbides, X-ray

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510 High-Temperature X-Ray Powder Diffraction of Secondary Gypsum

Authors: D. Gazdič, I. Hájková, M. Fridrichová

Abstract:

This paper involved the performance of a hightemperature X-Ray powder diffraction analysis (XRD) of a sample of chemical gypsum generated in the production of titanium white; this gypsum originates by neutralizing highly acidic water with limestone suspension. Specifically, it was gypsum formed in the first stage of neutralization when the resulting material contains, apart from gypsum, a number of waste products resulting from the decomposition of ilmenite by sulphuric acid. So it can be described as red titanogypsum. By conducting the experiment using XRD apparatus Bruker D8 Advance with a Cu anode (λkα=1.54184 Å) equipped with high-temperature chamber Anton Paar HTK 16, it was possible to identify clearly in the sample each phase transition in the system of CaSO4·xH2O.

Keywords: Anhydrite, Gypsum, Bassanite, Hematite, XRD, Powder, High-Temperature.

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509 Preparation of Vanadium Powder by Hydrogenation and Dehydrogenation

Authors: Weicai Yang, Xianfeng Dong, Dapeng Zeng, Bo Lin, Jun Tang

Abstract:

Low oxygen content vanadium powder was prepared by hydrogenation dehydrogenization (HDH). The effect of purification treatment on hydrogen absorption kinetics of dendritic vanadium was tested, and the effects of milling technique on powder yield and grain size were studied. The crystal phase, oxygen and nitrgen content, and grain size of prepared powder were characterized and analyzed by X-ray diffraction (XRD), oxygen and nitrogen analyzer and grain size analyzer. The results show that the alkaline cleaning can improve the hydrogen absorption of vanadium. The yield of vanadium hydride powder can reach as high as 90% by 4h ball-milling, The resultant product also have an oxygen content less than 600μg/g, and the grain size is smaller than 37μm. Meanwhile, the XRD results show that the phase of hydride vanadium powder is mainly VH0.81. After a hydrogen desorption treatment in vacuum at 700Ôäâ, the phase of the powder converts into V and a little of V2H.

Keywords: V-5Cr-5Ti alloy, HDH, microstructures, mechanical properties.

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508 Magnetic Properties of Sr-Ferrite Nano-Powder Synthesized by Sol-Gel Auto-Combustion Method

Authors: M. Ghobeiti-Hasab, Z. Shariati

Abstract:

In this paper, strontium ferrite (SrO.6Fe2O3) was synthesized by the sol-gel auto-combustion process. The thermal behavior of powder obtained from self-propagating combustion of initial gel was evaluated by simultaneous differential thermal analysis (DTA) and thermo gravimetric (TG), from room temperature to 1200°C. The as-burnt powder was calcined at various temperatures from 700-900°C to achieve the single-phase Sr-ferrite. Phase composition, morphology and magnetic properties were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. Results showed that the single-phase and nano-sized hexagonal strontium ferrite particles were formed at calcination temperature of 800°C with crystallite size of 27 nm and coercivity of 6238 Oe.

Keywords: Hard magnet, Sr-ferrite, Sol-gel auto-combustion, Nano-powder.

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507 Promising Immobilization of Cadmium and Lead inside Ca-rich Glass-ceramics

Authors: A. Karnis, L. Gautron

Abstract:

Considering toxicity of heavy metals and their accumulation in domestic wastes, immobilization of lead and cadmium is envisaged inside glass-ceramics. We particularly focused this work on calcium-rich phases embedded in a glassy matrix. Glass-ceramics were synthesized from glasses doped with 12 wt% and 16 wt% of PbO or CdO. They were observed and analyzed by Electron MicroProbe Analysis (EMPA) and Analytical Scanning Electron Microscopy (ASEM). Structural characterization of the samples was performed by powder XRay Diffraction. Diopside crystals of CaMgSi2O6 composition are shown to incorporate significant amounts of cadmium (up to 9 wt% of CdO). Two new crystalline phases are observed with very high Cd or Pb contents: about 40 wt% CdO for the cadmiumrich phase and near 60 wt% PbO for the lead-rich phase. We present complete chemical and structural characterization of these phases. They represent a promising way for the immobilization of toxic elements like Cd or Pb since glass ceramics are known to propose a “double barrier" protection (metal-rich crystals embedded in a glass matrix) against metal release in the environment.

Keywords: Cadmium, Calcium-rich phases, Diopside, Domesticwastes, Fly ashes, Glass-ceramics, Lead, Municipal Solid WasteIncineration.

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506 Synthesis and Characterization of Gallosilicate Sodalite Containing NO2- Ions

Authors: Ashok V. Borhade, Sanjay G. Wakchaure

Abstract:

Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.

Keywords: Gallosilicate, hydrothermal, nitrite, Reitveldrefinement.

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505 Preparation of Nanocrystalline Mesoporous ThO2 via Surfactant Assisted Sol-gel Procedure

Authors: N. Mohseni, S. Janitabar, S. J. Ahmadi, M. Roshanzamir, M. Thaghizadeh

Abstract:

In this research, thorium dioxide mesoporous nanocrystalline powder was synthesized through the sol-gel method using hydrated thorium nitrate and ammonium hydroxide as starting materials and Triton X100 as surfactant. ThO2 gel was characterized by thermogravimetric (TGA), and prepared ThO2 powder was subjected to scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer-Emett-Teller (BET) analyses studies. Detailed analyses show that prepared powder consisted of phase with the space group Fm3m of thoria and its crystalline size was 12.6 nm. The thoria possesses 16.7 m2/g surface area and the pore volume and size calculated to be 0.0423 cc/g and 1.947 nm, respectively.

Keywords: Thoria, sol-gel, mesoporous, nanocrystalline.

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504 Synthesis of Mg/B Containing Compound in a Modified Microwave Oven

Authors: Gülşah Çelik Gül, Figen Kurtuluş

Abstract:

Magnesium containing boron compounds with hexagonal structure have been drawn much attention due to their superconductive nature. The main target of this work is new modified microwave oven by on our own has an ability about passing through a gas in the oven medium for attainment of oxygen-free compounds such as c-BN.  Mg containing boride was synthesized by modified-microwave method under nitrogen atmosphere using amorphous boron and magnesium source in appropriate molar ratio. Microwave oven with oxygen free environment has been modified to aimed to obtain magnesium boride without oxygen. Characterizations were done by powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Mg containing boride, generally named magnesium boride, with amorphous character without oxygen is obtained via designed microwave oven system.

Keywords: Magnesium containing boron compounds, modified microwave synthesis, powder X-ray diffraction, FTIR.

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503 Effect of Heat Treatment on the Phase Formation of La0.6Sr0.4CoO3-α

Authors: A. A. Samat, N. A. Abdullah, M. A. M. Ishak, N. Osman

Abstract:

Powder of La0.6Sr0.4CoO3-α (LSCO) was synthesized by a combined citrate-EDTA method. The as-synthesized LSCO powder was calcined, respectively at temperatures of 800, 900 and 1000 °C with different heating/cooling rates which are 2, 5, 10 and 15 °C min-1. The effects of heat treatments on the phase formation of perovskite phase of LSCO were investigated by powder X-ray diffraction (XRD). The XRD patterns revealed that the rate of 5 °C min-1 is the optimum heating/cooling rate to obtain a single perovskite phase of LSCO with calcination temperature of 800 °C. This result was confirmed by a thermogravimetric analysis (TGA) as it showed a complete decomposition of intermediate compounds to form oxide material was also observed at 800 °C.

Keywords: La0.6Sr0.4CoO3-α, heat treatment, perovskite-type oxide, XRD.

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502 Growth and Characterization of L-Asparagine (LAS) Crystal Admixture of Paranitrophenol (PNP): A NLO Material

Authors: Grace Sahaya Sheba, P. Omegala Priyakumari, M. Gunasekaran

Abstract:

L-asparagine admixture Paranitrophenol (LAPNP) single crystals were grown successfully by solution method with slow evaporation technique at room temperature. Crystals of size 12mm×5 mm×3mm have been obtained in 15 days. The grown crystals were Brown color and transparent. The solubility of the grown samples has been found out at various temperatures. The lattice parameters of the grown crystals were determined by X-ray diffraction technique. The reflection planes of the sample were confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. Fourier transform infrared (FTIR) studies were used to confirm the presence of various functional groups in the crystals. UV–visible absorption spectrum was recorded to study the optical transparency of grown crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz–Perry powder technique and a study of its second harmonic generation efficiency in comparison with potassium dihydrogen phosphate (KDP) has been made. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to thermo gravimetric and differential thermal analysis (TG/DTA). The dielectric behavior of the sample was also studied

Keywords: Characterization, Microhardnes, Non-linear optical materials, Solution growth, Spectroscopy, XRD.

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501 Numerical Example of Aperiodic Diffraction Grating

Authors: Youssef Khmou, Said Safi, Miloud Frikel

Abstract:

Diffraction grating is periodic module used in many engineering fields, its geometrical conception gives interesting properties of diffraction and interferences, a uniform and periodic diffraction grating consists of a number of identical apertures that are equally spaced, in this case, the amplitude of intensity distribution in the far field region is generally modulated by diffraction pattern of single aperture. In this paper, we study the case of aperiodic diffraction grating with identical rectangular apertures where theirs coordinates are modeled by square root function, we elaborate a computer simulation comparatively to the periodic array with same length and we discuss the numerical results.

Keywords: Diffraction grating, interferences, amplitude modulation, laser.

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500 Thermo-chemical Characteristics of Powder Fabricated by Oxidation of Spent PWR Fuel

Authors: Geun-Il Park, Jae-Won Lee, Dou-Youn Lee, Jung-Won Lee, Kwang-Wook Kim, Kee-Chan Song

Abstract:

Thermochemcial characteristics of powder fabricated using oxidation treatment of spent PWR fuel and SIMFUEL were evaluated for recycling of spent fuel such as DUPIC process. Especially, the influence of spent fuel burn-ups on the powder fabrication characteristics was experimentally evaluated, ranging from 27,300 to 65,000 MWd/tU. Densities of powder manufactured from an oxidation, OREOX and the milling processes at the same process conditions were compared as a function of the fuel burn-ups respectively. Also, based on chemical analysis results, homogeneity of fissile elements in oxidized powder was confirmed.

Keywords: Spent PWR fuel, DUPIC, Oxidation, OREOX, Powder, Chemical analysis

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499 Patterned Growth of ZnO Nanowire Arrays on Zinc Foil by Thermal Oxidation

Authors: Farid Jamali Sheini, Dilip S. Joag, Mahendra A. More

Abstract:

A simple approach is demonstrated for growing large scale, nearly vertically aligned ZnO nanowire arrays by thermal oxidation method. To reveal effect of temperature on growth and physical properties of the ZnO nanowires, gold coated zinc substrates were annealed at 300 °C and 400 °C for 4 hours duration in air. Xray diffraction patterns of annealed samples indicated a set of well defined diffraction peaks, indexed to the wurtzite hexagonal phase of ZnO. The scanning electron microscopy studies show formation of ZnO nanowires having length of several microns and average of diameter less than 500 nm. It is found that the areal density of wires is relatively higher, when the annealing is carried out at higher temperature i.e. at 400°C. From the field emission studies, the values of the turn-on and threshold field, required to draw emission current density of 10 μA/cm2 and 100 μA/cm2 are observed to be 1.2 V/μm and 1.7 V/μm for the samples annealed at 300 °C and 2.9 V/μm and 3.7 V/μm for that annealed at 400 °C, respectively. The field emission current stability, investigated over duration of more than 2 hours at the preset value of 1 μA, is found to be fairly good in both cases. The simplicity of the synthesis route coupled with the promising field emission properties offer unprecedented advantage for the use of ZnO field emitters for high current density applications.

Keywords: ZnO, Nanowires, Thermal oxidation, FieldEmission.

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498 Inventive Synthesis and Characterization of a Cesium Molybdate Compound: CsBi(MoO4)2

Authors: F. Kurtuluş, G. Çelik Gül

Abstract:

Cesium molybdates with general formula CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich polymorphism, and crystallize in a layered structure. These properties cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Keywords: Cesium bismuth dimolybdate, microwave synthesis, powder x-ray diffraction, rare earth dimolybdates.

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497 An Investigation of New Phase Diagram of Ag2SO4 - CaSO4

Authors: Ravi V. Joat, Pravin S. Bodke, Shradha S. Binani, S. S. Wasnik

Abstract:

A phase diagram of the Ag2SO4 - CaSO4 (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag2SO4 + CaSO4) is observed at 10 mole% CaSO4 and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca 2+ in Ag2SO4 is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO4 content. Amongst other binary compositions, the 80AgSO4-20CaSO4 gave improved sinterability/packing density.

Keywords: Ag2SO4-CaSO4 (Silver sulphate–Calcium Sulphate) binaries system, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis).

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496 Structural and Electrochemical Characterization of Columnar-Structured Mn-Doped Bi26Mo10O69-d Electrolytes

Authors: Maria V. Morozova, Zoya A. Mikhaylovskaya, Elena S. Buyanova, Sofia A. Petrova, Ksenia V. Arishina, Robert G. Zaharov

Abstract:

The present work is devoted to the investigation of two series of doped bismuth molybdates: Bi26-2xMn2xMo10O69-d and Bi26Mo10-2yMn2yO69-d. Complex oxides were synthesized by conventional solid state technology and by co-precipitation method. The products were identified by powder diffraction. The powders and ceramic samples were examined by means of densitometry, laser diffraction, and electron microscopic methods. Porosity of the ceramic materials was estimated using the hydrostatic method. The electrical conductivity measurements were carried out using impedance spectroscopy method.

Keywords: Bismuth molybdate, columnar structures, impedance spectroscopy, oxygen ionic conductors.

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495 Waste Lubricating Oil Treatment by Adsorption Process Using Different Adsorbents

Authors: Nabil M. Abdel-Jabbar, Essam A.H. Al Zubaidy, Mehrab Mehrvar

Abstract:

Waste lubricating oil re-refining adsorption process by different adsorbent materials was investigated. Adsorbent materials such as oil adsorbent, egg shale powder, date palm kernel powder, and acid activated date palm kernel powder were used. The adsorption process over fixed amount of adsorbent at ambient conditions was investigated. The adsorption/extraction process was able to deposit the asphaltenic and metallic contaminants from the waste oil to lower values. It was found that the date palm kernel powder with contact time of 4 h was able to give the best conditions for treating the waste oil. The recovered solvent could be also reused. It was also found that the activated bentonite gave the best physical properties followed by the date palm kernel powder.

Keywords: activated bentonite, egg shale powder, datepalm kernel powder, used oil treatment, used oilcharacteristics.

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494 Pioneer Synthesis and Characterization of Boron Containing Hard Materials

Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

The first laboratory synthesis of hard materials such as diamond proceeded to attack of developing materials with high hardness to compete diamond. Boron rich solids are good candidates owing to their short interatomic bond lengths and strong covalent character. Boron containing hard material was synthesized by modifiedmicrowave method under nitrogen atmosphere by using a fuel (glycine or urea), amorphous boron and/or boric acid in appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differential thermal analysis (TG/DTA).

Keywords: Boron containing materials, hard materials, microwave synthesis, powder X-ray diffraction.

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493 Effect of Addition the Dune Sand Powder on Development of Compressive Strength and Hydration of Cement Pastes

Authors: S. Guettala, B. Mezghiche

Abstract:

In this paper, the effect of addition the dune sand powder (DSP) on development of compressive strength and hydration of cement pastes was investigated as a function of water/binder ratio, was varied, on the one hand, the percentage of DSP and on the other, the fineness of DSP. In order to understand better the pozzolanic effect of dune sand powder in cement pastes, we followed the mixtures hydration (50% Pure Lime + 50% DSP) by X-ray diffraction. These mixtures the pastes present a hydraulic setting which is due to the formation of a C-S-H phase (calcium silicate hydrate). The latter is semi-crystallized. This study is a simplified approach to that of the mixtures (80% ordinary Portland cement + 20% DSP), in which the main reaction is the fixing of the lime coming from the cement hydration in the presence of DSP, to form calcium silicate hydrate semi-crystallized of second generation. The results proved that up to (20% DSP) as Portland cement replacement could be used with a fineness of 4000 cm²/g without affecting adversely the compressive strength. After 28 days, the compressive strength at 5, 10 and 15% DSP is superior to Portland cement, with an optimum effect for a percentage of the order of 5% to 10% irrespective of the w/b ratio and fineness of DSP.

Keywords: Ordinary Portland Cement, Pure Lime, Dune Sand Powder, Compressive Strength, Hydration.

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492 Manufacturing Process of S-Glass Fiber Reinforced PEKK Prepregs

Authors: Nassier A. Nassir, Robert Birch, Zhongwei Guan

Abstract:

The aim of this study is to investigate the fundamental science/technology related to novel S-glass fiber reinforced polyether- ketone-ketone (GF/PEKK) composites and to gain insight into bonding strength and failure mechanisms. Different manufacturing techniques to make this high-temperature pre-impregnated composite (prepreg) were conducted i.e. mechanical deposition, electrostatic powder deposition, and dry powder prepregging techniques. Generally, the results of this investigation showed that it was difficult to control the distribution of the resin powder evenly on the both sides of the fibers within a specific percentage. Most successful approach was by using a dry powder prepregging where the fibers were coated evenly with an adhesive that served as a temporary binder to hold the resin powder in place onto the glass fiber fabric.

Keywords: Dry powder technique, PEKK, S-glass, thermoplastic prepreg.

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491 Synthesis of ZnO Nanostructures via Gel-casting Method

Authors: A.A.Rohani, A.Salehi, M.Tabrizi, S. A. Manafi, A. Fardafshari

Abstract:

In this study, ZnO nano rods and ZnO ultrafine particles were synthesized by Gel-casting method. The synthesized ZnO powder has a hexagonal zincite structure. The ZnO aggregates with rod-like morphology are typically 1.4 μm in length and 120 nm in diameter, which consist of many small nanocrystals with diameters of 10 nm. Longer wires connected by many hexahedral ZnO nanocrystals were obtained after calcinations at the temperature over 600° C.The crystalline structures and morphologies of the powder have been characterized by X-ray diffraction(XRD) and Scaning electron microscopy (SEM).The result shows that the different preparation conditions such as concentration H2O, calcinations time and calcinations temperature have a lot of influences upon the properties of nano ZnO powders, an increase in the temperature of the calcinations results in an increase of the grain size and also the increase of the calcinations time in high temperature makes the size of the grains bigger. The existences of extra watter prevent nano grains from improving like rod morphology. We have obtained the smallest grain size of ZnO powder by controlling the process conditions. Finally In a suitable condition, a novel nanostructure, namely bi-rod-like ZnO nano rods was found which is different from known ZnO nanostructures.

Keywords: morphology, nano particles, ZnO, gel-Casting method.

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490 Development of Material Analyzing Software Using X-Ray Diffraction

Authors: Le Chi Cuong

Abstract:

X-ray diffraction is an effective mean for analyzing material properties. This paper developed a new computational software for determining the properties of crystalline materials such as elastic constants, residual stresses, surface hardness, phase components, and etc. The results computed from the X-ray diffraction method were compared to those from the traditional methods and they are in the 95% confidential limits, showing that the newly developed software has high reproducibility, opening a possibility of its commercialization.

Keywords: X-ray diffraction, Nondestructive evaluation, Hardness, Residual stress, Phase determination.

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489 Feasibility of Ground Alkali-Active Sandstone Powder for Use in Concrete as Mineral Admixture

Authors: Xia Chen, Hua-Quan Yang, Shi-Hua Zhou

Abstract:

Alkali-active sandstone aggregate was ground by vertical and ball mill into particles with residue over 45 μm less than 12%, and investigations have been launched on particles distribution and characterization of ground sandstone powder, fluidity, heat of hydration, strength as well as hydration products morphology of pastes with incorporation of ground sandstone powder. Results indicated that ground alkali-active sandstone powder with residue over 45 μm less than 8% was easily obtainable, and specific surface area was more sensitive to characterize its fineness with extension of grinding length. Incorporation of sandstone powder resulted in higher water demand and lower strength, advanced hydration of C3A and C2S within 3days and refined pore structure. Based on its manufacturing, characteristics and influence on properties of pastes, it was concluded that sandstone powder was a good selection for use in concrete as mineral admixture.

Keywords: Concrete, mineral admixture, hydration, structure.

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488 Temperature Effect on the Solid-State Synthesis of Dehydrated Zinc Borates

Authors: N. Tugrul, N. Baran Acarali, A. S. Kipcak, E. Moroydor Derun, S. Piskin

Abstract:

Turkey has 72 % of total world boron reserves on the basis of B2O3.Borates that is a refined form of boron minerals have a wide range of applications. Zinc borates can be used as multifunctional synergistic additives. The most important properties are low solubility in water and high dehydration temperature. Zinc borates dehydrate above 290°C and anhydrous zinc borate has thermal resistance about 400°C. Zinc borates can be synthesized using several methods such as hydrothermal and solid-state processes. In this study, the solid-state method was applied between 500 and 800°C using the starting materials of ZnO and H3BO3 with 1:4 mole ratio. The reaction time was determined as 4 hours after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by XRay Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectrometer. As a result the form of ZnB4O7 was synthesized with the highest crystal score at 800°C.

Keywords: Raman, solid-state method, zinc borate, XRD.

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487 Increased Solubility, Dissolution and Physicochemical Studies of Curcumin- Polyvinylpyrrolidone K-30 Solid Dispersions

Authors: Nattha Kaewnopparat, Sanae Kaewnopparat, Amaravadee Jangwang, Daungkhae Maneenaun, Thitima Chuchome, Pharkphoom Panichayupakaranant

Abstract:

Solid dispersions (SD) of curcuminpolyvinylpyrrolidone in the ratio of 1:2, 1:4, 1:5, 1:6, and 1:8 were prepared in an attempt to increase the solubility and dissolution. Solubility, dissolution, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) of solid dispersions, physical mixtures (PM) and curcumin were evaluated. Both solubility and dissolution of curcumin solid dispersions were significantly greater than those observed for physical mixtures and intact curcumin. The powder X-ray diffractograms indicated that the amorphous curcumin was obtained from all solid dispersions. It was found that the optimum weight ratio for curcumin:PVP K-30 is 1:6. The 1:6 solid dispersion still in the amorphous from after storage at ambient temperature for 2 years and the dissolution profile did not significantly different from freshly prepared.

Keywords: Curcumin, polyvinylpyrrolidone K-30, solid dispersion, dissolution, physicochemical.

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486 Quality Attributes of Various Spray Dried Pulp Powder Prepared from Low Temperature Stored Calcium Salts Pretreated Guava Fruits

Authors: Renu Rahel, A. S. Chauhan, K. Srinivasulu, R. Ravi, V. B. Kudachikar

Abstract:

The effect of calcium salts on the storage stability and on the quality attributes of both fresh and processed product (guava powder) of white flesh guavas (var ‘Allahabad safeda’) was studied. The pulp behavioral studies of fully ripened guava fruits indicated that fruits pretreated with 3% and 4.5% calcium chloride had the least viscosity. The guava pulp powder using spray drying technique was developed and its storage stability and the moisture sorption studies were carried out for product quality evaluation at normal storage condition (27°C; 65%RH). Results revealed that powder obtained from 3% calcium chloride pretreated guavas was found to be at par with the powder obtained from control guavas after 90 days of normal storage. Studies on microbiological quality of guava pulp powder indicated that among the treatments powder obtained from guava fruit pretreated with 3% calcium chloride to be the most effective through restricting microbial counts of total plate count, yeast, mold, Staphylococcus and E. coli below their permissible limit. Moisture sorption studies of guava powder revealed that foil laminate 12μm PET/9 μm foil/38-40 μm is the most suitable packaging material recommended.

Keywords: White flesh guava, calcium salts, spray drying, powder, storage stability.

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485 The Optimization of Copper Sulfate and Tincalconite Molar Ratios on the Hydrothermal Synthesis of Copper Borates

Authors: E. Moroydor Derun, N. Tugrul, F. T. Senberber, A. S. Kipcak, S. Piskin

Abstract:

In this research, copper borates are synthesized by the reaction of copper sulfate pentahydrate (CuSO4.5H2O) and tincalconite (Na2O4B7.10H2O). The experimental parameters are selected as 80oC reaction temperature and 60 of reaction time. The effect of mole ratio of CuSO4.5H2O to Na2O4B7.5H2O is studied. For the identification analyses X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are used. At the end of the experiments, synthesized copper borate is matched with the powder diffraction file of “00-001-0472” [Cu(BO2)2] and characteristic vibrations between B and O atoms are seen. The proper crystals are obtained at the mole ratio of 3:1. This study showed that simplified synthesis process is suitable for the production of copper borate minerals.

Keywords: Hydrothermal synthesis, copper borates, copper sulfate, tincalconite.

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484 Iron Doped Biomaterial Calcium Borate: Synthesis and Characterization

Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA). 

Keywords: Colemanite, conventional synthesis, powder x-ray diffraction, borates.

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483 Production of Composite Materials by Mixing Chromium-Rich Ash and Soda-Lime Glass Powder: Mechanical Properties and Microstructure

Authors: Savvas Varitis, Panagiotis Kavouras, George Vourlias, Eleni Pavlidou, Theodoros Karakostas, Philomela Komninou

Abstract:

A chromium-loaded ash originating from incineration of tannery sludge under anoxic conditions was mixed with low grade soda-lime glass powder coming from commercial glass bottles. The relative weight proportions of ash over glass powder tested were 30/70, 40/60 and 50/50. The solid mixtures, formed in green state compacts, were sintered at the temperature range of 800o C up to 1200o C. The resulting products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDXS) and micro-indentation. The above methods were employed to characterize the various phases, microstructure and hardness of the produced materials. Thermal treatment at 800o C and 1000o C produced opaque ceramic products composed of a variety of chromium-containing and chromium-free crystalline phases. Thermal treatment at 1200o C gave rise to composite products, where only chromium-containing crystalline phases were detected. Hardness results suggest that specific products are serious candidates for structural applications.

Keywords: Chromium-rich tannery residues, glass-ceramic materials, mechanical properties, microstructure

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482 Synthesis and Characterization of Silver/Polylactide Nanocomposites

Authors: Kamyar Shameli, Mansor Bin Ahmad, Wan Md Zin Wan Yunus, Nor Azowa Ibrahim, Maryam Jokar, Majid Darroudi

Abstract:

Silver/polylactide nanocomposites (Ag/PLA-NCs) were synthesized via chemical reduction method in diphase solvent. Silver nitrate and sodium borohydride were used as a silver precursor and reducing agent in the polylactide (PLA). The properties of Ag/PLA-NCs were studied as a function of the weight percentages of silver nanoparticles (8, 16 and 32 wt% of Ag-NPs) relative to the weight of PLA. The Ag/PLA-NCs were characterized by Xray diffraction (XRD), transmission electron microscopy (TEM), electro-optical microscopy (EOM), UV-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FT-IR). XRD patterns confirmed that Ag-NPs crystallographic planes were face centered cubic (fcc) type. TEM images showed that mean diameters of Ag-NPs were 3.30, 3.80 and 4.80 nm. Electro-optical microscopy revealed excellent dispersion and interaction between Ag-NPs and PLA films. The generation of silver nanoparticles was confirmed from the UVvisible spectra. FT-IR spectra showed that there were no significant differences between PLA and Ag/PLA-NCs films. The synthesized Ag/PLA-NCs were stable in organic solution over a long period of time without sign of precipitation.

Keywords: Nanocomposites, Polylactide, Silver Nanoparticles, Sodium Borohydride, Transmission Electron Microscopy.

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