Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 77

Search results for: nanocrystalline

77 Microstructure Study of NanoCrystalline Cellulose Obtained from Cotton Linter

Authors: Farid Amidi-Fazli


Problems and disadvantages of using conventional plastics are more apparent in recent years and have attracted researchers' attention. Polymers from natural resources or bio polymers represent a suitable replacement to overcome to the disadvantages of plastics. But due to the some flaws of bio polymers, using suitable filler almost seems necessary. Nanocrystalline cellulose with low cost and availability can be applied as appropriate filler. In this study nanocrystalline cellulose was produced from cotton Linter and was characterized. The cotton Linter was hydrolyzed in sulfuric acid then neutralized by the two different concentrations of NaOH. The resulted suspension was treated by ultrasound waves. Process efficiency was determined as 90%. The final product was studied using scanning electron microscopy and x-ray diffraction technique. The obtained diagram of XRD experiment confirmed that the produced material was nanocrystalline cellulose. Also percentage of crystallinity was calculated as 84% in the obtained material as well as the size of crystals. It can be said that the applied method is a rapid and easy method for the production of nanocrystalline cellulose.

Keywords: nanocrystalline cellulose, crystallinity, XRD, cotton linter

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76 Obtaining of Nanocrystalline Ferrites and Other Complex Oxides by Sol-Gel Method with Participation of Auto-Combustion

Authors: V. S. Bushkova


It is well known that in recent years magnetic materials have received increased attention due to their properties. For this reason a significant number of patents that were published during the last decade are oriented towards synthesis and study of such materials. The aim of this work is to create and study ferrite nanocrystalline materials with spinel structure, using sol-gel technology with participation of auto-combustion. This method is perspective in that it is a cheap and low-temperature technique that allows for the fine control on the product’s chemical composition.

Keywords: magnetic materials, ferrites, sol-gel technology, nanocrystalline powders

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75 Fabrication and Characterization of Cu50 (Zr50-xNix) 50 Nanocrystalline Coating by Cold Spray Technique for Potential Antibiofilm Application

Authors: Ahmad Alazemi, M. Sherif El-Eskandrany, Mohamad Kishk, Thanyan AlOnaizi, Ahmad Alduweesh, Shorouq Abdullaleel


Arc melting technique followed by top-down approach, using a high-energy ball milling technique were employed to synthesize nanocrystalline of Cu50(Zr50-xNix)50 (x = 0, 10, 20 and 30 at.%) powder particles. The end-products of the alloy powders obtained after 50 h of the ball milling time were uniform in composition and had spherical-like morphology with an average particle size of 0.75 µm in diameter. The powders, which consisted of nanocrystalline grains with an average grain size of 10 nm in diameter, were used as feedstock materials for double face coating of stainless (SUS304) sheets, using cold spraying process. The coating materials enjoyed nanocrystalline structure and uniform composition. Biofilms were grown on 20-mm2 SUS304 sheets coated coupons inoculated with 1.5 × 108 CFU ml−1 E. coli. Significant biofilm inhibition was recorded in the nanoparticles coated coupons in comparison to non-coated SUS304 coupon. In conclusion, this study demonstrates that formation of biofilms can be significantly inhibited by Cu-based alloys especially in case of high (Ni) content. The inhibition of biofilm formation by nanocrystalline powders of Cu-based provides a practical approach to achieve the inhibition of biofilms formed by an emerging pathogen.

Keywords: biofilm, Cu, E.coli, FE-HRTEM/EDS, nanomaterials, nanocrystalline

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74 Preparation of Nanocrystalline Mesoporous ThO2 Via Surfactant Assisted Sol-gel Procedure

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


There has been proposed a technique for getting thorium dioxide mesoporous nanocrystalline. In this paper thorium dioxide 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 (TG), 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 27 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: mesoporous, nanocrystalline, sol-gel, thoria

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73 Development of Nanocomposite from Poly (Lactic Acid) Plasticised Epoxidised Jatropha Oil and Nanocrystalline Cellulose

Authors: Siti Hasnah Kamarudin, Luqman Chuah Abdullah, Min Min Aung, Chantara Thevy Ratnam


The primary objective of this work was to develop fully nanocomposite material based on poly(lactic acid), epoxidized jatropha oil (EJO) and nanocrystalline cellulose. EJO was investigated as a sustainable alternative to petrochemical-based plasticizers to reinforce the ductility and toughness of plastics, in this case, nanocellulose/poly(lactic acid) (PLA). The EJO was melt blended into nanocellulose/PLA at concentrations from 1 wt% to 5 wt%. The blends were then hot-pressed into sheets to characterize their mechanical and physical properties. Microcrystalline cellulose had been converted to nanocrystalline cellulose by acid mercerisation technique and the effects thereof on the composites’ tensile, flexural, and impact properties, as well as their water absorption and density, were studied. The impact strengths of the nanocomposites were improved with the addition of NCC up to 0.5 wt%, with a maximum over 10 times that of the neat PLA. The flexural strength and modulus increased 4% and 50%, respectively, for NCC/PLA plasticized with EJO. This increase demonstrated the nanocrystalline cellulose addition gave notable improvements to the composites’ properties. Furthermore, analysis by scanning electron microscopy (SEM) of the nanocomposites’ tensile fracture surfaces indicated better interaction adhesion of the NCC/PLA plasticized with EJO compared with the PLA/EJO composites.

Keywords: nanocrystalline cellulose, nanocomposite, poly (lactic acid), epoxidised jatropha oil

Procedia PDF Downloads 53
72 Effect of Precursor’s Grain Size on the Conversion of Microcrystalline Gallium Antimonide GaSb to Nanocrystalline Gallium Nitride GaN

Authors: Jerzy F. Janik, Mariusz Drygas, Miroslaw M. Bucko


A simple precursor system has been recently developed in our laboratory for the conversion of affordable microcrystalline gallium antimonide GaSb to a range of nanocrystalline powders of gallium nitride GaN – a wide bandgap semiconductor indispensable in modern optoelectronics. The process relies on high temperature nitridation reactions of GaSb with ammonia. Topochemical relationships set up by the cubic lattice of GaSb result in some metastable cubic GaN formed in addition to the stable hexagonal GaN. A prior application of high energy ball milling to the initially microcrystalline GaSb precursor is shown to alter the nitridation output.

Keywords: nanocrystalline, gallium nitride, GaN, gallium antimonide, GaSb, nitridation, ball milling

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71 Wet Chemical Synthesis for Fe-Ni Alloy Nanocrystalline Powder

Authors: Neera Singh, Devendra Kumar, Om Parkash


We have synthesized nanocrystalline Fe-Ni alloy powders where Ni varies as 10, 30 and 50 mole% by a wet chemical route (sol-gel auto-combustion) followed by reduction in hydrogen atmosphere. The ratio of citrate to nitrate was maintained at 0.3 where citric acid has worked as a fuel during combustion. The reduction of combusted powders was done at 700°C/1h in hydrogen atmosphere using an atmosphere controlled quartz tube furnace. Phase and microstructure analysis has shown the formation of α-(Fe,Ni) and γ-(Fe,Ni) phases after reduction. An increase in Ni concentration resulted in more γ-(Fe,Ni) formation where complete γ-(Fe,Ni) formation was achieved at 50 mole% Ni concentration. Formation of particles below 50 nm size range was confirmed using Scherrer’s formula and Transmission Electron Microscope. The work is aimed at the effect of Ni concentration on phase, microstructure and magnetic properties of synthesized alloy powders.

Keywords: combustion, microstructure, nanocrystalline, reduction

Procedia PDF Downloads 69
70 Nanocrystalline Cellulose from Oil Palm Fiber

Authors: Ridzuan Ramli, Zianor Azrina Zianon Abdin, Mohammad Dalour Beg, Rosli M. Yunus


Nanocrystalline cellulose (NCC) were produced by using the ultrasound assisted acid hydrolysis from oil palm empty fruit bunch (EFB) pulp with different hydrolysis time then were analyzed by using FESEM and TGA as in comparison with EFB fiber and EFB pulp. Based on the FESEM analysis, it was found that NCC has a rod like shaped under the acid hydrolysis with an assistant of ultrasound. According to thermal stability, the NCC obtained show remarkable sign of high thermal stability compared to EFB fiber and EFB pulp. However, as the hydrolysis time increase, the thermal stability of NCC was deceased. As in conclusion, the NCC can be prepared by using ultrasound assisted acid hydrolysis. The NCC obtained have good thermal stability and have a great potential as the reinforcement in composite materials.

Keywords: Nanocrystalline cellulose, ultrasound assisted acid hydrolysis, thermal stability, morphology, empty fruit bunch (EFB)

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69 Spark Plasma Sintering of Aluminum-Based Composites Reinforced by Nanocrystalline Carbon-Coated Intermetallic Particles

Authors: B. Z. Manuel, H. D. Esmeralda, H. S. Felipe, D. R. Héctor, D. de la Torre Sebastián, R. L. Diego


Aluminum Matrix Composites reinforced with nanocrystalline Ni3Al carbon-coated intermetallic particles, were synthesized by powder metallurgy. Powder mixture of aluminum with 0.5-volume fraction of reinforcement particles was compacted by spark plasma sintering (SPS) technique and the compared with conventional sintering process. The better results for SPS technique were obtained in 520ºC-5kN-3min.The hardness (70.5±8 HV) and the elastic modulus (95 GPa) were evaluated in function of sintering conditions for SPS technique; it was found that the incorporation of these kind of reinforcement particles in aluminum matrix improve its mechanical properties. The densities were about 94% and 97% of the theoretical density. The carbon coating avoided the interfacial reaction between matrix-particle at high temperature (520°C) without show composition change either intermetallic dissolution.

Keywords: aluminum matrix composites, intermetallics, spark plasma sintering, nanocrystalline

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68 Preparation and Characterization of Nanocrystalline Cellulose from Acacia mangium

Authors: Samira Gharehkhani, Seyed Farid Seyed Shirazi, Abdolreza Gharehkhani, Hooman Yarmand, Ahmad Badarudin, Rushdan Ibrahim, Salim Newaz Kazi


Nanocrystalline cellulose (NCC) were prepared by acid hydrolysis and ultrasound treatment of bleached Acacia mangium fibers. The obtained rod-shaped nanocrystals showed a uniform size. The results showed that NCC with high crystallinity can be obtained using 64 wt% sulfuric acid. The effect of synthesis condition was investigated. Different reaction times were examined to produce the NCC and the results revealed that an optimum reaction time has to be used for preparing the NCC. Morphological investigation was performed using the transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA) were performed. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments. The NCC suspension was homogeneous and stable and no sedimentation was observed for a long time.

Keywords: acid hydrolysis, nanocrystalline cellulose, nano material, reaction time

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67 Nanocellulose Incorporated Polyvinyl Alcohol Hydrogel

Authors: Rosli Mohd Yunus, Zianor Azrina Zianon Abdin, Mohammad Dalour Hossen Beg, Ridzuan Ramli


Recently, nanocrystalline cellulose (NCC) has gained considerable interest as a promising biomaterial due to their outstanding properties such as high surface area, high mechanical properties, hydrophilicity, biocompatibility and biodegradability. The NCC also has good stability in water which is compatible for mixing of water based polymer solution or emulsions with NCC. Oil palm empty fruit bunch (EFB) contained different amount of lignocellulosic materials such as lignin, hemicellulose and cellulose. Cellulose is the most significant materials that can be extracted from EFB as nanocrystalline cellulose (NCC). In this work the nanocrystalline cellulose were produced through acid hydrolysis together with ultrasound technique. The morphology of NCC was characterized by TEM, thermal behavior has been studied with DSC, TGA analysis. Structural properties were illustrated X-Ray diffraction as well as FTIR. The hydrogel was produced using polyvinyl alcohol (PVA) with different concentration of NCC. The hydrogel composite was characterized by swelling ratio, crosslinking density, mechanical properties and morphology.

Keywords: nanocellulose, oil palm, hydrogel, water treatment

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66 Surface Nanocrystalline and Hardening Effects of Ti–Al–V Alloy by Electropulsing Ultrasonic Shock

Authors: Xiaoxin Ye, Guoyi Tang


The effect of electropulsing ultrasonic shock (EUS) on the surface hardening and microstructure of Ti6Al4V alloy was studied. It was found that electropulsing improved the microhardness dramatically both in the influential depth and maximum value, compared with the only ultrasonic-shocked sample. It’s indicated that refined surface layer with nanocrystalline and improved microhardness were obtained on account of surface severe plastic deformation, dynamic recrystallization (DRX) and phase change, which was implemented at relative low temperature and high strain rate/capacity due to the coupling of the thermal and athermal effects of EUS. It’s different from conventional experiments and theory. It’s discussed that the positive contributions of EPT in the thermodynamics and kinetics of microstructure and properties change were attributed to the reduction of nucleation energy barrier and acceleration of atomic diffusion. Therefore, it’s supposed that EUS is an energy-saving and high-efficiency method of surface treatment technique with the help of high-energy electropulses, which is promising in cost reduction of the surface engineering and energy management.

Keywords: titanium alloys, electropulsing, ultrasonic shock, microhardness, nanocrystalline

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65 Effects of Al on Microstructure and Magnetic Properties of (Nd,Pr)-(Fe,Co)-B Alloys Prepared by Mechanical Alloying

Authors: Rahim Sabbaghizadeh, Mansor Hashim, Nooshin Shourcheh


Nanocrystalline Nd8Pr2Fe79-xCo5B6Alx (x=0, 1, 2, 3) magnets were prepared by mechanical alloying and respective heat treatment, and the effects of the addition of Al on the microstructure and magnetic properties of Nd-Fe-Co-B alloy were studied. The changes in the nanostructure and magnetic properties were examined by X-Ray diffraction, combined with Field Emission Scanning electron microscopy (FeSEM) and vibrating sample magnetometer (VSM). Addition of Al was found to be effective for improving the coercivity and the hysteresis squareness in Nd–Fe–Co–B magnets without decreasing much the remanent magnetization.

Keywords: mechanical alloying, nanocrystalline, Nd-Fe-B, vibrating sample magnetomete

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64 Microstructural Study of Mechanically Alloyed Powders and the Thin Films of Cufe Alloys

Authors: Mechri hanane, Azzaz Mohammed


Polycrystalline CuFe thin film was prepared by thermal evaporation process (Physical vapor deposition), using the nanocrystalline CuFe powder obtained by mechanical alloying After 24 h of milling elemental powders. The microscopic study of nanocrystalline powder and the thin film of Cu70Fe30 binary alloy were examined using transmission electron microscopy (TEM) and scanning electron microscope (SEM). The cross-sectional TEM images showed that the obtained CuFe layer was polycrystalline film of about 20 nm thick and composed of grains of different size ranging from 4 nm to 18 nm.

Keywords: nanomaterials, thin films, TEM, SEM

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63 Thermally Stable Nanocrystalline Aluminum Alloys Processed by Mechanical Alloying and High Frequency Induction Heat Sintering

Authors: Hany R. Ammar, Khalil A. Khalil, El-Sayed M. Sherif


The as-received metal powders were used to synthesis bulk nanocrystalline Al; Al-10%Cu; and Al-10%Cu-5%Ti alloys using mechanical alloying and high frequency induction heat sintering (HFIHS). The current study investigated the influence of milling time and ball-to-powder (BPR) weight ratio on the microstructural constituents and mechanical properties of the processed materials. Powder consolidation was carried out using a high frequency induction heat sintering where the processed metal powders were sintered into a dense and strong bulk material. The sintering conditions applied in this process were as follow: heating rate of 350°C/min; sintering time of 4 minutes; sintering temperature of 400°C; applied pressure of 750 Kgf/cm2 (100 MPa); cooling rate of 400°C/min and the process was carried out under vacuum of 10-3 Torr. The powders and the bulk samples were characterized using XRD and FEGSEM techniques. The mechanical properties were evaluated at various temperatures of 25°C, 100°C, 200°C, 300°C and 400°C to study the thermal stability of the processed alloys. The bulk nanocrystalline Al; Al-10%Cu; and Al-10%Cu-5%Ti alloys displayed extremely high hardness values even at elevated temperatures. The Al-10%Cu-5%Ti alloy displayed the highest hardness values at room and elevated temperatures which are related to the presence of Ti-containing phases such as Al3Ti and AlCu2Ti, these phases are thermally stable and retain the high hardness values at elevated temperatures up to 400ºC.

Keywords: nanocrystalline aluminum alloys, mechanical alloying, hardness, elevated temperatures

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62 Production of Nanocrystalline Cellulose (NCC) from Rice Husk Biomass by Chemical Extraction Process

Authors: Md. Sakinul Islam, Nhol Kao, Sati Bhattacharya, Rahul Gupta


The objective of the study is to produce naocrystalline cellulose (NCC) from rice husk by chemical extraction process. The chemical extraction processes of this production are delignification, bleaching and hydrolysis. In order to produce NCC, raw rice husk (RRH) was grinded and converted to powder form. Powder rice husk was obtained by sieving and the particles in the 75-710 μm size range was used for experimental work. The production of NCC was conducted into the jacketed glass reactor at 80 ˚C temperature under predetermined experimental conditions. In this work NaOH (4M) solution was used for delignification process. After certain experimental time delignified powder RH was collected from the reactor then washed, bleached and finally hydrolyzed in order to degrade cellulose to nanocrystalline cellulose (NCC). For bleaching and hydrolysis processes NaOCl (20%) and H2SO4 (4M) solutions were used, respectively. The resultant products from hydrolysis was neutralized by buffer solution and analyzed by FTIR, XRD, SEM, AFM and TEM. From the analysis, NCC has been identified successfully and the particle dimension has been confirmed to be in the range of 20-50 nm. From XRD results, the crystallinity of NCC was found to be approximately 45%.

Keywords: nanocrystalline cellulose, NCC, rice husk, biomass, chemical extraction

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61 Optical Properties of Nanocrystalline Europium-Yttrium Titanate EuYTi2O7

Authors: J. Mrazek, R. Skala, S. Bysakh, Ivan Kasik


Lanthanide-doped yttrium titanium oxides, which crystallize in a pyrochlore structure with general formula (RExY1-x)2Ti2O7 (RE=rare earth element), have been extensively investigated in recent years for their interesting physical and chemical properties. Despite that the pure pyrochlore structure does not present luminescence ability, the presence of yttrium ions in the pyrochlore structure significantly improves the luminescence properties of the RE. Moreover, the luminescence properties of pyrochlores strongly depend on the size of formed nanocrystals. In this contribution, we present a versatile sol-gel synthesis of nanocrystalline EuYTi2O7pyrochlore. The nanocrystalline powders and thin films were prepared by the condensation of titanium(IV)butoxide with europium(III) chloride followed by the calcination. The introduced method leads to the formation of the highly-homogenous nanocrystalline EuYTi2O7 with tailored grain size ranging from 20 nm to 200 nm. The morphology and the structure of the formed nanocrystals are linked to the luminescence properties of Eu3+ ions incorporated into the pyrochlore lattice. The results of XRD and HRTEM analysis show that the Eu3+ and Y3+ ions are regularly distributed inside the lattice. The lifetime of Eu3+ ions in calcinated powders is regularly decreasing from 140 us to 68 us and the refractive index of prepared thin films regularly increases from 2.0 to 2.45 according to the calcination temperature. The shape of the luminescence spectra and the decrease of the lifetime correspond with the crystallinity of prepared powders. The results present fundamental information about the effect of the size of the nanocrystals to their luminescence properties. The promising application of prepared nanocrystals in the field of lasers and planar optical amplifiers is widely discussed in the contribution.

Keywords: europium, luminescence, nanocrystals, sol-gel

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60 Synthesis and Thermoluminescence Study of Nanocrystalline Radiation Dosimeter CaSO₄:Ce/Sm/Dy

Authors: Anant Pandey, Kanika Sharma, Vibha Chopra, Shaila Bahl, Pratik Kumar, S. P. Lochab, Birendra Singh


This paper reports the thermoluminescence (TL) properties of nanocrystalline CaSO₄ activated by Ce, Sm, and Dy. TL properties are investigated by chiefly changing the dopant element and also by varying the concentration of the dopant elements (from 0.05 mol % to 0.5 mol %) so as to establish the optimized dopant concentration for each of the activators. The method of salt preparation used is the typical chemical co-precipitation method and the technique used for characterization of the prepared samples is the X-Ray Diffraction (XRD) technique. Further, the phosphors are irradiated with gamma radiation from Co-60 (1.25 MeV) source (dose range- 30 Gy to 500 Gy). The optimized concentration (vis-a-vis TL peak intensity) of activator for CaSO₄:Ce is found to be 0.2 mol %, for CaSO₄:Sm it is 0.1 mol % and for CaSO₄:Dy it is 0.2 mol %. Further, the primary study of the TL response curves for all the three phosphors confirms linearity in the studied dose range (i.e., 30 Gy to 500 Gy). Finally, CaSO₄:Dy was also studied for its energy dependence property which plays an important role in defining the utility of a phosphor for dosimetric applications. The range of doses used for the energy dependence study was from 30 Gy to 500 Gy from Cs-137 (0.662 MeV). The nano-phosphors showed potential to be used as radiation dosimeter in the studied range of gamma radiation and thus must be studied for a wider range of doses.

Keywords: gamma radiation, nanocrystalline, radiation dosimetry, thermoluminescence

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59 Effect of the Deposition Time of Hydrogenated Nanocrystalline Si Grown on Porous Alumina Film on Glass Substrate by Plasma Processing Chemical Vapor Deposition

Authors: F. Laatar, S. Ktifa, H. Ezzaouia


Plasma Enhanced Chemical Vapor Deposition (PECVD) method is used to deposit hydrogenated nanocrystalline silicon films (nc-Si: H) on Porous Anodic Alumina Films (PAF) on glass substrate at different deposition duration. Influence of the deposition time on the physical properties of nc-Si: H grown on PAF was investigated through an extensive correlation between micro-structural and optical properties of these films. In this paper, we present an extensive study of the morphological, structural and optical properties of these films by Atomic Force Microscopy (AFM), X-Ray Diffraction (XRD) techniques and a UV-Vis-NIR spectrometer. It was found that the changes in DT can modify the films thickness, the surface roughness and eventually improve the optical properties of the composite. Optical properties (optical thicknesses, refractive indexes (n), absorption coefficients (α), extinction coefficients (k), and the values of the optical transitions EG) of this kind of samples were obtained using the data of the transmittance T and reflectance R spectra’s recorded by the UV–Vis–NIR spectrometer. We used Cauchy and Wemple–DiDomenico models for the analysis of the dispersion of the refractive index and the determination of the optical properties of these films.

Keywords: hydragenated nanocrystalline silicon, plasma processing chemical vapor deposition, X-ray diffraction, optical properties

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58 Spark Plasma Sintering/Synthesis of Alumina-Graphene Composites

Authors: Nikoloz Jalabadze, Roin Chedia, Lili Nadaraia, Levan Khundadze


Nanocrystalline materials in powder condition can be manufactured by a number of different methods, however manufacture of composite materials product in the same nanocrystalline state is still a problem because the processes of compaction and synthesis of nanocrystalline powders go with intensive growth of particles – the process which promotes formation of pieces in an ordinary crystalline state instead of being crystallized in the desirable nanocrystalline state. To date spark plasma sintering (SPS) has been considered as the most promising and energy efficient method for producing dense bodies of composite materials. An advantage of the SPS method in comparison with other methods is mainly low temperature and short time of the sintering procedure. That finally gives an opportunity to obtain dense material with nanocrystalline structure. Graphene has recently garnered significant interest as a reinforcing phase in composite materials because of its excellent electrical, thermal and mechanical properties. Graphene nanoplatelets (GNPs) in particular have attracted much interest as reinforcements for ceramic matrix composites (mostly in Al2O3, Si3N4, TiO2, ZrB2 a. c.). SPS has been shown to fully densify a variety of ceramic systems effectively including Al2O3 and often with improvements in mechanical and functional behavior. Alumina consolidated by SPS has been shown to have superior hardness, fracture toughness, plasticity and optical translucency compared to conventionally processed alumina. Knowledge of how GNPs influence sintering behavior is important to effectively process and manufacture process. In this study, the effects of GNPs on the SPS processing of Al2O3 are investigated by systematically varying sintering temperature, holding time and pressure. Our experiments showed that SPS process is also appropriate for the synthesis of nanocrystalline powders of alumina-graphene composites. Depending on the size of the molds, it is possible to obtain different amount of nanopowders. Investigation of the structure, physical-chemical, mechanical and performance properties of the elaborated composite materials was performed. The results of this study provide a fundamental understanding of the effects of GNP on sintering behavior, thereby providing a foundation for future optimization of the processing of these promising nanocomposite systems.

Keywords: alumina oxide, ceramic matrix composites, graphene nanoplatelets, spark-plasma sintering

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57 Synthesis and Thermoluminescence Investigations of Doped LiF Nanophosphor

Authors: Pooja Seth, Shruti Aggarwal


Thermoluminescence dosimetry (TLD) is one of the most effective methods for the assessment of dose during diagnostic radiology and radiotherapy applications. In these applications monitoring of absorbed dose is essential to prevent patient from undue exposure and to evaluate the risks that may arise due to exposure. LiF based thermoluminescence (TL) dosimeters are promising materials for the estimation, calibration and monitoring of dose due to their favourable dosimetric characteristics like tissue-equivalence, high sensitivity, energy independence and dose linearity. As the TL efficiency of a phosphor strongly depends on the preparation route, it is interesting to investigate the TL properties of LiF based phosphor in nanocrystalline form. LiF doped with magnesium (Mg), copper (Cu), sodium (Na) and silicon (Si) in nanocrystalline form has been prepared using chemical co-precipitation method. Cubical shape LiF nanostructures are formed. TL dosimetry properties have been investigated by exposing it to gamma rays. TL glow curve structure of nanocrystalline form consists of a single peak at 419 K as compared to the multiple peaks observed in microcrystalline form. A consistent glow curve structure with maximum TL intensity at annealing temperature of 573 K and linear dose response from 0.1 to 1000 Gy is observed which is advantageous for radiotherapy application. Good reusability, low fading (5 % over a month) and negligible residual signal (0.0019%) are observed. As per photoluminescence measurements, wide emission band at 360 nm - 550 nm is observed in an undoped LiF. However, an intense peak at 488 nm is observed in doped LiF nanophosphor. The phosphor also exhibits the intense optically stimulated luminescence. Nanocrystalline LiF: Mg, Cu, Na, Si phosphor prepared by co-precipitation method showed simple glow curve structure, linear dose response, reproducibility, negligible residual signal, good thermal stability and low fading. The LiF: Mg, Cu, Na, Si phosphor in nanocrystalline form has tremendous potential in diagnostic radiology, radiotherapy and high energy radiation application.

Keywords: thermoluminescence, nanophosphor, optically stimulated luminescence, co-precipitation method

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56 Photoluminescence Spectroscopy to Probe Mixed Valence State in Eu-Doped Nanocrystalline Glass-Ceramics

Authors: Ruchika Bagga, Mauro Falconieri, Venu Gopal Achanta, José M. F. Ferreira, Ashutosh Goel, Gopi Sharma


Mixed valence Eu-doped nanocrystalline NaAlSiO4/NaY9Si6O26 glass-ceramics have been prepared by controlled crystallization of melt quenched bulk glasses. XRD and SEM techniques were employed to characterize the crystallization process of the precursor glass and their resultant glass-ceramics. Photoluminescence spectroscopy was used to analyze the formation of divalent europium (Eu2+) from Eu3+ ions during high temperature synthesis under ambient atmosphere and is explained on the basis of optical basicity model. The observed luminescence properties of Eu: NaY9Si6O26 are compared with that of well explored Eu: β-PbF2 nanocrystals and their marked differences are discussed.

Keywords: rare earth, oxyfluoride glasses, nano-crystalline glass-ceramics, photoluminescence spectroscopy

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55 Nanocrystalline Na0.1V2O5.nH2Oxerogel Thin Film for Gas Sensing

Authors: M. S. Al-Assiri, M. M. El-Desoky, A. A. Bahgat


Nanocrystalline thin film of Na0.1V2O5.nH2O xerogel obtained by sol-gel synthesis was used as a gas sensor. Gas sensing properties of different gases such as hydrogen, petroleum and humidity were investigated. Applying XRD and TEM the size of the nanocrystals is found to be 7.5 nm. SEM shows a highly porous structure with submicron meter-sized voids present throughout the sample. FTIR measurement shows different chemical groups identifying the obtained series of gels. The sample was n-type semiconductor according to the thermoelectric power and electrical conductivity. It can be seen that the sensor response curves from 130°C to 150°C show a rapid increase in sensitivity for all types of gas injection, low response values for heating period and the rapid high response values for cooling period. This result may suggest that this material is able to act as gas sensor during the heating and cooling process.

Keywords: sol-gel, thermoelectric power, XRD, TEM, gas sensing

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54 High Pressure Delignification Process for Nanocrystalline Cellulose Production from Agro-Waste Biomass

Authors: Sakinul Islam, Nhol Kao, Sati Bhattacharya, Rahul Gupta


Nanocrystalline cellulose (NCC) has been widely used for miscellaneous applications due to its superior properties over other nanomaterials. However, the major problems associated with the production of NCC are long reaction time, low production rate and inefficient process. The mass production of NCC within a short period of time is still a great challenge. The main objective of this study is to produce NCC from rice husk agro waste biomass from a high pressure delignification process (HPDP), followed by bleaching and hydrolysis processes. The HPDP has not been explored for NCC production from rice husk biomass (RHB) until now. In order to produce NCC, powder rice husk (PRH) was placed into a stainless steel reactor at 80 ˚C under 5 bars. Aqueous solution of NaOH (4M) was used for the dissolution of lignin and other amorphous impurities from PRH. After certain experimental times (1h, 3.5h and 6h), bleaching and hydrolysis were carried out on delignified samples. NaOCl (20%) and H2SO4 (4M) solutions were used for bleaching and hydrolysis processes, respectively. The NCC suspension from hydrolysis was sonicated and neutralized by buffer solution for various characterisations. Finally NCC suspension was dried and analyzed by FTIR, XRD, SEM, AFM and TEM. The chemical composition of NCC and PRH was estimated by TAPPI (Technical Association of Pulp and Paper Industry) standard methods to observe the product purity. It was found that, the 6h of the HPDP was more efficient to produce good quality NCC than that at 1h and 3.5h due to low separation of non-cellulosic components from RHB. The analyses indicated the crystallinity of NCC to be 71 %, particle size of 20-50 nm (diameter) and 100-200 nm in length.

Keywords: nanocrystalline cellulose, NCC, high pressure delignification, bleaching, hydrolysis, agro-waste biomass

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53 Thermoluminescent Response of Nanocrystalline BaSO4:Eu to 85 MeV Carbon Beams

Authors: Shaila Bahl, S. P. Lochab, Pratik Kumar


Nanotechnology and nanomaterials have attracted researchers from different fields, especially from the field of luminescence. Recent studies on various luminescent nanomaterials have shown their relevance in dosimetry of ionizing radiations for the measurements of high doses using the Thermoluminescence (TL) technique, where the conventional microcrystalline phosphors saturate. Ion beams have been used for diagnostic and therapeutic purposes due to their favorable profile of dose deposition at the end of the range known as the Bragg peak. While dealing with human beings, doses from these beams need to be measured with great precision and accuracy. Henceforth detailed investigations of suitable thermoluminescent dosimeters (TLD) for dose verification in ion beam irradiation are required. This paper investigates the TL response of nanocrystalline BaSO4 doped with Eu to 85 MeV carbon beam. The synthesis was done using Co-precipitation technique by mixing Barium chloride and ammonium sulphate solutions. To investigate the crystallinity and particle size, analytical techniques such as X-ray diffraction (XRD) and Transmission electron microscopy (TEM) were used which revealed the average particle sizes to 45 nm with orthorhombic structure. Samples in pellet form were irradiated by 85 MeV carbon beam in the fluence range of 1X1010-5X1013. TL glow curves of the irradiated samples show two prominent glow peaks at around 460 K and 495 K. The TL response is linear up to 1X1013 fluence after which saturation was observed. The wider linear TL response of nanocrystalline BaSO4: Eu and low fading make it a superior candidate as a dosimeter to be used for detecting the doses of carbon beam.

Keywords: radiation, dosimetry, carbon ions, thermoluminescence

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52 Nitrogen-Doped Ultrananocrystalline Diamond/Hydrogenated Amorphous Carbon Composite Films Prepared by Coaxial Arc Plasma Deposition

Authors: Abdelrahman Zkria, Tsuyoshi Yoshitake


Diamond is one of the most interesting semiconducting carbon materials owing to its unique physical and chemical properties, yet its application in electronic devices is limited due to the difficulty of realizing n-type conduction by nitrogen doping. In contrast Ultrananocrystalline diamond with diamond grains of about 3–5 nm in diameter have attracted much attention for device-oriented applications because they may enable the realization of n-type doping with nitrogen. In this study, nitrogen-doped Ultra-Nanocrystalline diamond films were prepared by coaxial arc plasma deposition (CAPD) method, the nitrogen content was estimated by X-ray photoemission spectroscopy (XPS). The electrical conductivity increased with increasing nitrogen contents. Heterojunction diodes with p-type Si were fabricated and evaluated based on current–voltage (I–V) and capacitance–voltage (C–V) characteristics measured in dark at room temperature.

Keywords: heterojunction diodes, hopping conduction mechanism, nitrogen-doping, ultra-nanocrystalline diamond

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51 A Fast Chemiresistive H₂ Gas Sensor Based on Sputter Grown Nanocrystalline P-TiO₂ Thin Film Decorated with Catalytic Pd-Pt Layer on P-Si Substrate

Authors: Jyoti Jaiswal, Satyendra Mourya, Gaurav Malik, Ramesh Chandra


In the present work, we have fabricated and studied a resistive H₂ gas sensor based on Pd-Pt decorated room temperature sputter grown nanocrystalline porous titanium dioxide (p-TiO₂) thin film on porous silicon (p-Si) substrate for fast H₂ detection. The gas sensing performance of Pd-Pt/p-TiO₂/p-Si sensing electrode towards H₂ gas under low (10-500 ppm) detection limit and operating temperature regime (25-200 °C) was discussed. The sensor is highly sensitive even at room temperature, with response (Ra/Rg) reaching ~102 for 500 ppm H₂ in dry air and its capability of sensing H₂ concentrations as low as ~10 ppm was demonstrated. At elevated temperature of 200 ℃, the response reached more than ~103 for 500 ppm H₂. Overall the fabricated resistive gas sensor exhibited high selectivity, good sensing response, and fast response/recovery time with good stability towards H₂.

Keywords: sputtering, porous silicon (p-Si), TiO₂ thin film, hydrogen gas sensor

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50 Synthesis and Characterization of CaZrTi2O7 from Tartrate Precursor Employing Microwave Heating Technique

Authors: B. M. Patil, S. R. Dharwadkar


Zirconolite (CaZrTi2O7) is one of the three major phases in the synthetic ceramic 'SYNROC' which is used for immobilization of high-level nuclear waste and also acts as photocatalytic and photophysical properties. In the present work the nanocrystalline CaZrTi2O7 was synthesized from Calcium Zirconyl Titanate tartrate precursor (CZTT) employing two different heating techniques such as Conventional heating (Muffle furnace) and Microwave heating (Microwave Oven). Thermal decomposition of the CZTT precursors in air yielded nanocrystalline CaZrTi2O7 powder as the end product. The products obtained by annealing the CZTT precursor using both heating method were characterized using simultaneous TG-DTA, FTIR, XRD, SEM, TEM, NTA and thermodilatometric study. The physical characteristics such as crystallinity, morphology and particle size of the product obtained by heating the CZTT precursor at the different temperatures in a Muffle furnace and Microwave oven were found to be significantly different. The microwave heating technique considerably lowered the synthesis temperature of CaZrTi2O7. The influence of microwave heating was more pronounced as compared to Muffle furnace heating. The details of the synthesis of CaZrTi2O7 from CZTT precursor are discussed.

Keywords: CZTT, CaZrTi2O7, microwave, SYNROC, zirconolite

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49 Barrier Properties of Starch-Ethylene Vinyl Alcohol Nanocomposites

Authors: Farid Amidi Fazli


Replacement of plastics used in the food industry seems to be a serious issue to overcome mainly the environmental problems in recent years. This study investigates the hydrophilicity and permeability properties of starch biopolymer which ethylene vinyl alcohol (EVOH) (0-10%) and nanocrystalline cellulose (NCC) (1 -15%) were used to enhance its properties. Starch -EVOH nanocomposites were prepared by casting method in different formulations. NCC production by acid hydrolysis was confirmed by scanning electron microscopy. Solubility, water vapor permeability, water vapor transmission rate and moisture absorbance were measured on each of the nanocomposites. The results were analyzed by SAS software. The lowest moisture absorbance was measured in pure starch nanocomposite containing 8% NCC. The lowest permeability to water vapor belongs to starch nanocomposite containing 8% NCC and the sample containing 7.8% EVOH and 13% NCC. Also, the lowest solubility was observed in the composite contains the highest amount of EVOH. Applied Process resulted in production of bio films which have good resistance to water vapor permeability and solubility in water. The use of NCC and EVOH leads to reduced moisture absorbance property of the biofilms.

Keywords: starch, EVOH, nanocrystalline cellulose, hydrophilicity

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48 Effect of Milling Parameters on the Characteristics of Nanocrystalline TiAl Alloys Synthesized by Mechanical Alloying

Authors: Jinan B. Al-Dabbagh, Rozman Mohd Tahar, Mahadzir Ishak


TiAl alloy nano-powder was successfully produced by a mechanical alloying (MA) technique in a planetary ball mill. The influence of milling parameters, such as the milling duration, rotation speed, and balls-to-powder mass ratio, on the characteristics of the Ti50%Al powder, including the microstructure, crystallite size refinement, and phase formation, were investigated. It was found that MA of elemental Ti and Al powders promotes the formation of TiAl alloys, as Ti (Al) solid solution was formed after 5h of milling. Milling without the addition of process control agents led to a dramatic decrease in the crystallite size to 17.8 nm after 2h of milling. Higher rotation energy and a higher ball-to-powder weight ratio also accelerated the reduction in crystallite size. Subsequent heating up to 850°C resulted in the formation of a new intermetallic phase with a dominant TiAl3 phase plus minor γ-TiAl or α2-Ti3Al phase or both. A longer milling duration also exhibited a better effect on the micro-hardness of Ti50%Al powders.

Keywords: TiAl alloys, nanocrystalline materials, mechanical alloying, materials science

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