Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 5175

Search results for: crystal size

5175 A Regression Model for Predicting Sugar Crystal Size in a Fed-Batch Vacuum Evaporative Crystallizer

Authors: Sunday B. Alabi, Edikan P. Felix, Aniediong M. Umo


Crystal size distribution is of great importance in the sugar factories. It determines the market value of granulated sugar and also influences the cost of production of sugar crystals. Typically, sugar is produced using fed-batch vacuum evaporative crystallizer. The crystallization quality is examined by crystal size distribution at the end of the process which is quantified by two parameters: the average crystal size of the distribution in the mean aperture (MA) and the width of the distribution of the coefficient of variation (CV). Lack of real-time measurement of the sugar crystal size hinders its feedback control and eventual optimisation of the crystallization process. An attractive alternative is to use a soft sensor (model-based method) for online estimation of the sugar crystal size. Unfortunately, the available models for sugar crystallization process are not suitable as they do not contain variables that can be measured easily online. The main contribution of this paper is the development of a regression model for estimating the sugar crystal size as a function of input variables which are easy to measure online. This has the potential to provide real-time estimates of crystal size for its effective feedback control. Using 7 input variables namely: initial crystal size (Lo), temperature (T), vacuum pressure (P), feed flowrate (Ff), steam flowrate (Fs), initial super-saturation (S0) and crystallization time (t), preliminary studies were carried out using Minitab 14 statistical software. Based on the existing sugar crystallizer models, and the typical ranges of these 7 input variables, 128 datasets were obtained from a 2-level factorial experimental design. These datasets were used to obtain a simple but online-implementable 6-input crystal size model. It seems the initial crystal size (Lₒ) does not play a significant role. The goodness of the resulting regression model was evaluated. The coefficient of determination, R² was obtained as 0.994, and the maximum absolute relative error (MARE) was obtained as 4.6%. The high R² (~1.0) and the reasonably low MARE values are an indication that the model is able to predict sugar crystal size accurately as a function of the 6 easy-to-measure online variables. Thus, the model can be used as a soft sensor to provide real-time estimates of sugar crystal size during sugar crystallization process in a fed-batch vacuum evaporative crystallizer.

Keywords: crystal size, regression model, soft sensor, sugar, vacuum evaporative crystallizer

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5174 The Experimental Study on Reducing and Carbonizing Titanium-Containing Slag by Iron-Containing Coke

Authors: Yadong Liu


The experimental study on reduction carbonization of coke containing iron respectively with the particle size of <0.3mm, 0.3-0.6mm and 0.6-0.9mm and synthetic sea sand ore smelting reduction titanium-bearing slag as material were studied under the conditions of holding 6h at most at 1500℃. The effects of coke containing iron particle size and heat preservation time on the formation of TiC and the size of TiC crystal were studied by XRD, SEM and EDS. The results show that it is not good for the formation, concentration and growth of TiC crystal when the particle size of coke containing iron is too small or too large. The suitable particle size is 0.3~0.6mm. The heat preservation time of 2h basically ensures that all the component TiO2 in the slag are reduced and carbonized and converted to TiC. The size of TiC crystal will increase with the prolongation of heat preservation time. The thickness of the TiC layer can reach 20μm when the heat preservation time is 6h.

Keywords: coke containing iron, formation and concentration and growth of TiC, reduction and carbonization, titanium-bearing slag

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5173 Development of 420 mm Diameter Silicon Crystal Growth Using Continuous Czochralski Process

Authors: Ilsun Pang, Kwanghun Kim, Sungsun Baik


Large diameter Si wafer is used as semiconductor substrate. Large diameter Si crystal ingot should be needed in order to increase wafer size. To make convection of large silicon melt stable, magnetic field is normally applied, but magnetic field is expensive and it is not proper to stabilize the large Si melt. To solve the problem, we propose a continuous Czochralski process which can be applied to small melt without magnetic field. We used granule poly, which has size distribution of 1~3 mm and is easily supplied in double crucible during silicon ingot growth. As the result, we produced 420 mm diameter ingot. In this paper, we describe an experimental study on crystal growth of large diameter silicon by Continuous Czochralski process.

Keywords: Czochralski, ingot, silicon crystal, wafer

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5172 Adjustable Aperture with Liquid Crystal for Real-Time Range Sensor

Authors: Yumee Kim, Seung-Guk Hyeon, Kukjin Chun


An adjustable aperture using a liquid crystal is proposed for real-time range detection and obtaining images simultaneously. The adjustable aperture operates as two types of aperture stops which can create two different Depth of Field images. By analyzing these two images, the distance can be extracted from camera to object. Initially, the aperture stop has large size with zero voltage. When the input voltage is applied, the aperture stop transfer to smaller size by orientational transition of liquid crystal molecules in the device. The diameter of aperture stop is 1.94mm and 1.06mm. The proposed device has low driving voltage of 7.0V and fast response time of 6.22m. Compact size aperture of 6×6×1.1 mm3 is assembled in conventional camera which contain 1/3” HD image sensor and focal length of 3.3mm that can be used in autonomous. The measured range was up to 5m. The adjustable aperture has high stability due to no mechanically moving parts. This range sensor can be applied to the various field of 3D depth map application which is the Advanced Driving Assistance System (ADAS), drones and manufacturing machine.

Keywords: adjustable aperture, dual aperture, liquid crystal, ranging and imaging, ADAS, range sensor

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5171 Effect of Synthesis Parameters on Crystal Size and Perfection of Mordenite and Analcime

Authors: Zehui Du, Chaiwat Prapainainar, Paisan Kongkachuichay, Paweena Prapainainar


The aim of this work was to obtain small crystalline size and high crystallinity of mordenites and analcimes, by modifying the aging time, agitation, water content, crystallization temperature and crystallization time. Two different hydrothermal methods were studied. Both methods used Na2SiO3 as the silica source, NaAlO2 as the aluminum source, and NaOH as the alkali source. The first method used HMI as the template while the second method did not use the template. Mordenite crystals with spherical shape and bimodal in size of about 1 and 5 µm were obtained from the first method using conditions of 24 hr aging time, 170°C and 24 hr crystallization. Modernites with high crystallinity were formed using agitation system in the crystallization process. It was also found that the aging time of 2 hr and 24 hr did not much affect the formation of mordenite crystals. Analcime crystals were formed in spherical shape and facet on surface with the size between 13-15 µm by the second method using the conditions of 30 minutes aging time, 170°C and 24 hr crystallization without calcination. By increasing water content, the crystallization process was slowed down and resulted in smaller analcime crystals. Larger size of analcime crystals were observed when the samples were calcined at 300°C and 580°C. Higher calcination temperature led to higher crystal growth and resulted in larger crystal size. Finally, mordenite and analcime was used as fillers in zeolite/Nafion composite membrane to solve the fuel cross over problem in direct alcohol fuel cell.

Keywords: analcime, hydrothermal synthesis, mordenite, zeolite

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5170 Performances of the Double-Crystal Setup at CERN SPS Accelerator for Physics beyond Colliders Experiments

Authors: Andrii Natochii


We are currently presenting the recent results from the CERN accelerator facilities obtained in the frame of the UA9 Collaboration. The UA9 experiment investigates how a tiny silicon bent crystal (few millimeters long) can be used for various high-energy physics applications. Due to the huge electrostatic field (tens of GV/cm) between crystalline planes, there is a probability for charged particles, impinging the crystal, to be trapped in the channeling regime. It gives a possibility to steer a high intensity and momentum beam by bending the crystal: channeled particles will follow the crystal curvature and deflect on the certain angle (from tens microradians for LHC to few milliradians for SPS energy ranges). The measurements at SPS, performed in 2017 and 2018, confirmed that the protons deflected by the first crystal, inserted in the primary beam halo, can be caught and channeled by the second crystal. In this configuration, we measure the single pass deflection efficiency of the second crystal and prove our opportunity to perform the fixed target experiment at SPS accelerator (LHC in the future).

Keywords: channeling, double-crystal setup, fixed target experiment, Timepix detector

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5169 Carbamazepine Co-crystal Screening with Dicarboxylic Acids Co-Crystal Formers

Authors: S. Abd Rahim, F. A. Rahman, E. M. Nasir, N. A. Ramle


Co-crystal is believed to improve the solubility and dissolution rates and thus, enhanced the bioavailability of poor water soluble drugs particularly during the oral route of administration. With the existing of poorly soluble drugs in pharmaceutical industry, the screening of co-crystal formation using carbamazepine (CBZ) as a model drug compound with dicarboxylic acids co-crystal formers (CCF) namely fumaric (FA) and succinic (SA) acids in ethanol has been studied. The co-crystal formations were studied by varying the mol ratio values of CCF to CBZ to access the effect of CCF concentration on the formation of the co-crystal. Solvent evaporation, slurry, and cooling crystallisations which representing the solution based method co-crystal screening were used. The product crystal from the screening was characterized using X-ray powder diffraction (XRPD). The XRPD pattern profile analysis has shown that the CBZ co-crystals with FA and SA were successfully formed for all ratios studied. The findings revealed that CBZ-FA co-crystal were formed in two different polymorphs. It was found that CBZ-FA form A and form B were formed from evaporation and slurry crystallisation methods respectively. On the other hand, in cooling crystallisation method, CBZ-FA form A was formed at lower mol ratio of CCF to CBZ and vice versa. This study disclosed that different methods and mol ratios during the co-crystal screening can affect the outcome of co-crystal produced such as polymorphic forms of co-crystal and thereof. Thus, it was suggested that careful attentions is needed during the screening since the co-crystal formation is currently one of the promising approach to be considered in research and development for pharmaceutical industry to improve the poorly soluble drugs.

Keywords: co-crystal, dicarboxylic acid, carbamazepine, industry

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5168 Model Predictive Control Using Thermal Inputs for Crystal Growth Dynamics

Authors: Takashi Shimizu, Tomoaki Hashimoto


Recently, crystal growth technologies have made progress by the requirement for the high quality of crystal materials. To control the crystal growth dynamics actively by external forces is useuful for reducing composition non-uniformity. In this study, a control method based on model predictive control using thermal inputs is proposed for crystal growth dynamics of semiconductor materials. The control system of crystal growth dynamics considered here is governed by the continuity, momentum, energy, and mass transport equations. To establish the control method for such thermal fluid systems, we adopt model predictive control known as a kind of optimal feedback control in which the control performance over a finite future is optimized with a performance index that has a moving initial time and terminal time. The objective of this study is to establish a model predictive control method for crystal growth dynamics of semiconductor materials.

Keywords: model predictive control, optimal control, process control, crystal growth

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5167 A Closed-Form Solution and Comparison for a One-Dimensional Orthorhombic Quasicrystal and Crystal Plate

Authors: Arpit Bhardwaj, Koushik Roy


The work includes derivation of the exact-closed form solution for simply supported quasicrystal and crystal plates by using propagator matrix method under surface loading and free vibration. As a numerical example a quasicrystal and a crystal plate are considered, and after investigation, the variation of displacement and stress fields along the thickness of these two plates are presented. Further, it includes analyzing the displacement and stress fields for two plates having two different stacking arrangement, i.e., QuasiCrystal/Crystal/QuasiCrystal and Crystal/QuasiCrystal/Crystal and comparing their results. This will not only tell us the change in the behavior of displacement and stress fields in two different materials but also how these get changed after trying their different combinations. For the free vibration case, Crystal and Quasicrystal plates along with their different stacking arrangements are considered, and displacements are plotted in all directions for different Mode Shapes.

Keywords: free vibration, multilayered plates, surface loading, quasicrystals

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5166 Durability Enhancement of CaSO4 in Repetitive Operation of Chemical Heat Pump

Authors: Y. Shiren, M. Masuzawa, H. Ohkura, T. Yamagata, Y. Aman, N. Kobayashi


An important problem for the CaSO4/CaSO4・1/2H2O Chemical heat pump (CHP) is that the material is deactivated through repetitive reaction between hydration and dehydration in which the crystal phase of the material is transformed from III-CaSO4 to II-CaSO4. We investigated suppression on the phase change by adding a sulfated compound. The most effective material was MgSO4. MgSO4 doping increased the durability of CaSO4 in the actual CHP repetitive cycle of hydration/dehydration to 3.6 times that of undoped CaSO4. The MgSO4-doped CaSO4 showed a higher phase transition temperature and activation energy for crystal transformation from III-CaSO4 to II-CaSO4. MgSO4 doping decreased the crystal lattice size of CaSO4・1/2H2O and II-CaSO4 to smaller than that of undoped CaSO4. Modification of the crystal structure is considered to be related to the durability change in CaSO4 resulting from MgSO4 doping.

Keywords: CaSO4, chemical heat pump, durability of chemical heat storage material, heat storage

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5165 Effect of Si/Al Ratio on SSZ-13 Crystallization and Its Methanol-To-Olefins Catalytic Properties

Authors: Zhiqiang Xu, Hongfang Ma, Haitao Zhang, Weixin Qian, Weiyong Ying


SSZ-13 materials with different Si/Al ratio were prepared by varying the composition of aluminosilicate precursor solutions upon hydrothermal treatment at 150 °C. The Si/Al ratio of the initial system was systematically changed from 12.5 to infinity in order to study the limits of Al composition in precursor solutions for constructing CHA structure. The intermediates and final products were investigated by complementary techniques such as XRD, HRTEM, FESEM, and chemical analysis. NH3-TPD was used to study the Brønsted acidity of SSZ-13 samples with different Si/Al ratios. The effect of the Si/Al ratio on the precursor species, ultimate crystal size, morphology and yield was investigated. The results revealed that Al species determine the nucleation rate and the number of nuclei, which is tied to the morphology and yield of SSZ-13. The size of SSZ-13 increased and the yield decreased as the Si/Al ratio was improved. Varying Si/Al ratio of the initial system is a facile, commercially viable method of tailoring SSZ-13 crystal size and morphology. Furthermore, SSZ-13 materials with different Si/Al ratio were tested as catalysts for the methanol to olefins (MTO) reaction at 350 °C. SSZ-13 with the Si/Al ratio of 35 shows the best MTO catalytic performance.

Keywords: crystallization, MTO, Si/Al ratio, SSZ-13

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5164 Determination of the Structural Parameters of Calcium Phosphate for Biomedical Use

Authors: María Magdalena Méndez-González, Miguel García Rocha, Carlos Manuel Yermo De la Cruz


Calcium phosphate (Ca5(PO4)3(X)) is widely used in orthopedic applications and is widely used as powder and granules. However, their presence in bone is in the form of nanometric needles 60 nm in length with a non-stoichiometric phase of apatite contains CO3-2, Na+, OH-, F-, and other ions in a matrix of collagen fibers. The crystal size, morphology control and interaction with cells are essential for the development of nanotechnology. The structural results of calcium phosphate, synthesized by chemical precipitation with crystal size of 22.85 nm are presented in this paper. The calcium phosphate powders were analyzed by X-ray diffraction, energy dispersive spectroscopy (EDS), infrared spectroscopy and FT-IR transmission electron microscopy. Network parameters, atomic positions, the indexing of the planes and the calculation of FWHM (full width at half maximum) were obtained. The crystal size was also calculated using the Scherer equation d (hkl) = cλ/βcosѲ. Where c is a constant related to the shape of the crystal, the wavelength of the radiation used for a copper anode is 1.54060Å, Ѳ is the Bragg diffraction angle, and β is the width average peak height of greater intensity. Diffraction pattern corresponding to the calcium phosphate called hydroxyapatite phase of a hexagonal crystal system was obtained. It belongs to the space group P63m with lattice parameters a = 9.4394 Å and c = 6.8861 Å. The most intense peak is obtained 2Ѳ = 31.55 (FWHM = 0.4798), with a preferred orientation in 121. The intensity difference between the experimental data and the calculated values is attributable to the temperature at which the sintering was performed. The intensity of the highest peak is at angle 2Ѳ = 32.11. The structure of calcium phosphate obtained was a hexagonal configuration. The intensity changes in the peaks of the diffraction pattern, in the lattice parameters at the corners, indicating the possible presence of a dopant. That each calcium atom is surrounded by a tetrahedron of oxygen and hydrogen was observed by infrared spectra. The unit cell pattern corresponds to hydroxyapatite and transmission electron microscopic crystal morphology corresponding to the hexagonal phase with a preferential growth along the c-plane was obtained.

Keywords: structure, nanoparticles, calcium phosphate, metallurgical and materials engineering

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5163 Texture Observation of Bending by XRD and EBSD Method

Authors: Takashi Sakai, Yuri Shimomura


The crystal orientation is a factor that affects the microscopic material properties. Crystal orientation determines the anisotropy of the polycrystalline material. And it is closely related to the mechanical properties of the material. In this paper, for pure copper polycrystalline material, two different methods; X-Ray Diffraction (XRD) and Electron Backscatter Diffraction (EBSD); and the crystal orientation were analyzed. In the latter method, it is possible that the X-ray beam diameter is thicker as compared to the former, to measure the crystal orientation macroscopically relatively. By measurement of the above, we investigated the change in crystal orientation and internal tissues of pure copper.

Keywords: bending, electron backscatter diffraction, X-ray diffraction, microstructure, IPF map, orientation distribution function

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5162 The Fabrication of Scintillator Column by Hydraulic Pressure Injection Method

Authors: Chien Chon Chen, Chun Mei Chu, Chuan Ju Wang, Chih Yuan Chen, Ker Jer Huang


Cesiumiodide with Na doping (CsI(Na)) solution or melt is easily forming three- dimension dendrites on the free surface. The defects or bobbles form inside the CsI(Na) during the solution or melt solidification. The defects or bobbles can further effect the x-ray path in the CsI(Na) crystal and decrease the scintillation characteristics of CsI(Na). In order to enhance the CsI(Na) scintillated property we made single crystal of CsI(Na) column in the anodic aluminum oxide (AAO) template by hydraulic pressure injection method. It is interesting that when CsI(Na) melt is confined in the small AAO channels, the column grow as stable single column without any dendrites. The high aspect ratio (100~10000) of AAO and nano to sub-micron channel structure which is a suitable template for single of crystal CsI(Na) formation. In this work, a new low-cost approach to fabricate scintillator crystals using anodic aluminum oxide (AAO) rather than Si is reported, which can produce scintillator crystals with a wide range of controllable size to optimize their performance in X-ray detection.

Keywords: cesiumiodide, AAO, scintillator, crystal, X-ray

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5161 Terahertz Glucose Sensors Based on Photonic Crystal Pillar Array

Authors: S. S. Sree Sanker, K. N. Madhusoodanan


Optical biosensors are dominant alternative for traditional analytical methods, because of their small size, simple design and high sensitivity. Photonic sensing method is one of the recent advancing technology for biosensors. It measures the change in refractive index which is induced by the difference in molecular interactions due to the change in concentration of the analyte. Glucose is an aldosic monosaccharide, which is a metabolic source in many of the organisms. The terahertz waves occupies the space between infrared and microwaves in the electromagnetic spectrum. Terahertz waves are expected to be applied to various types of sensors for detecting harmful substances in blood, cancer cells in skin and micro bacteria in vegetables. We have designed glucose sensors using silicon based 1D and 2D photonic crystal pillar arrays in terahertz frequency range. 1D photonic crystal has rectangular pillars with height 100 µm, length 1600 µm and width 50 µm. The array period of the crystal is 500 µm. 2D photonic crystal has 5×5 cylindrical pillar array with an array period of 75 µm. Height and diameter of the pillar array are 160 µm and 100 µm respectively. Two samples considered in the work are blood and glucose solution, which are labelled as sample 1 and sample 2 respectively. The proposed sensor detects the concentration of glucose in the samples from 0 to 100 mg/dL. For this, the crystal was irradiated with 0.3 to 3 THz waves. By analyzing the obtained S parameter, the refractive index of the crystal corresponding to the particular concentration of glucose was measured using the parameter retrieval method. Refractive indices of the two crystals decreased gradually with the increase in concentration of glucose in the sample. For 1D photonic crystals, a gradual decrease in refractive index was observed at 1 THz. 2D photonic crystal showed this behavior at 2 THz. The proposed sensor was simulated using CST Microwave studio. This will enable us to develop a model which can be used to characterize a glucose sensor. The present study is expected to contribute to blood glucose monitoring.

Keywords: CST microwave studio, glucose sensor, photonic crystal, terahertz waves

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5160 Shaped Crystal Growth of Fe-Ga and Fe-Al Alloy Plates by the Micro Pulling down Method

Authors: Kei Kamada, Rikito Murakami, Masahiko Ito, Mototaka Arakawa, Yasuhiro Shoji, Toshiyuki Ueno, Masao Yoshino, Akihiro Yamaji, Shunsuke Kurosawa, Yuui Yokota, Yuji Ohashi, Akira Yoshikawa


Techniques of energy harvesting y have been widely developed in recent years, due to high demand on the power supply for ‘Internet of things’ devices such as wireless sensor nodes. In these applications, conversion technique of mechanical vibration energy into electrical energy using magnetostrictive materials n have been brought to attention. Among the magnetostrictive materials, Fe-Ga and Fe-Al alloys are attractive materials due to the figure of merits such price, mechanical strength, high magnetostrictive constant. Up to now, bulk crystals of these alloys are produced by the Bridgman–Stockbarger method or the Czochralski method. Using these method big bulk crystal up to 2~3 inch diameter can be grown. However, non-uniformity of chemical composition along to the crystal growth direction cannot be avoid, which results in non-uniformity of magnetostriction constant and reduction of the production yield. The micro-pulling down (μ-PD) method has been developed as a shaped crystal growth technique. Our group have reported shaped crystal growth of oxide, fluoride single crystals with different shape such rod, plate tube, thin fiber, etc. Advantages of this method is low segregation due to high growth rate and small diffusion of melt at the solid-liquid interface, and small kerf loss due to near net shape crystal. In this presentation, we report the shaped long plate crystal growth of Fe-Ga and Fe-Al alloys using the μ-PD method. Alloy crystals were grown by the μ-PD method using calcium oxide crucible and induction heating system under the nitrogen atmosphere. The bottom hole of crucibles was 5 x 1mm² size. A <100> oriented iron-based alloy was used as a seed crystal. 5 x 1 x 320 mm³ alloy crystal plates were successfully grown. The results of crystal growth, chemical composition analysis, magnetostrictive properties and a prototype vibration energy harvester are reported. Furthermore, continuous crystal growth using powder supply system will be reported to minimize the chemical composition non-uniformity along the growth direction.

Keywords: crystal growth, micro-pulling-down method, Fe-Ga, Fe-Al

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5159 The Catalytic Activity of CU2O Microparticles

Authors: Kanda Wongwailikhit


Copper (I) oxide microparticles with the morphology of cubic and hollow sphere were synthesized with the assistance of a surfactant as the shape controller. Both particles were then subjected to a study of the catalytic activity and the results of shape effects of catalysts on rate of catalytic reaction was observed. The decolorizing reaction of crystal violet and sodium hydroxide was chosen and the decrease of reactant with respect to time was measured using a spectrophotometer. The result revealed that morphology of the crystal had no effect on the catalytic activity for the crystal violet reaction but contributed to total surface area predominantly.

Keywords: copper (I) oxide, catalytic activity, crystal violet

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5158 Applying the Crystal Model Approach on Light Nuclei for Calculating Radii and Density Distribution

Authors: A. Amar


A new model, namely the crystal model, has been modified to calculate the radius and density distribution of light nuclei up to ⁸Be. The crystal model has been modified according to solid-state physics, which uses the analogy between nucleon distribution and atoms distribution in the crystal. The model has analytical analysis to calculate the radius where the density distribution of light nuclei has obtained from analogy of crystal lattice. The distribution of nucleons over crystal has been discussed in a general form. The equation that has been used to calculate binding energy was taken from the solid-state model of repulsive and attractive force. The numbers of the protons were taken to control repulsive force, where the atomic number was responsible for the attractive force. The parameter has been calculated from the crystal model was found to be proportional to the radius of the nucleus. The density distribution of light nuclei was taken as a summation of two clusters distribution as in ⁶Li=alpha+deuteron configuration. A test has been done on the data obtained for radius and density distribution using double folding for d+⁶,⁷Li with M3Y nucleon-nucleon interaction. Good agreement has been obtained for both the radius and density distribution of light nuclei. The model failed to calculate the radius of ⁹Be, so modifications should be done to overcome discrepancy.

Keywords: nuclear physics, nuclear lattice, study nucleus as crystal, light nuclei till to ⁸Be

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5157 Phase Diagram Including a Negative Pressure Region for a Thermotropic Liquid Crystal in a Metal Berthelot Tube

Authors: K. Hiro, T. Wada


Thermodynamic properties of liquids under negative pressures are interesting and important in fields of scienceand technology. Here, phase transitions of a thermotropic liquid crystal are investigatedin a range from positive to negative pressures with a metal Berthelot tube using a commercial pressure transducer.Two co-existinglines, namely crystal (Kr) – nematic (N), and isotropic liquid (I) - nematic (N) lines, weredrawn in a pressure - temperature plane. The I-N line was drawn to ca. -5 (MPa).

Keywords: Berthelot method, liquid crystal, negative pressure, phase transitions

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5156 Synthesis and Crystal Structure of a Cu(II) Complex of a Pyridine-Naphthoimidazole-Based Ligand

Authors: Shuang Zhao, Shintaro Ito, Yoshihiro Ohba, Hiroshi Katagiri


We present the synthesis and single-crystal X-ray crystallography of a Cu(II) complex(bmn-bpy) of a pyridine-naphthoimidazole-based ligand containing two naphthoimidazoles as the chromophores and a vacant coordination site on Cu(II).

Keywords: synthesis, Cu(II) complex, single-crystal X-ray crystallography

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5155 Development of Materials Based on Phosphates of NaZr2(PO4)3 with Low Thermal Expansion

Authors: V. Yu. Volgutov, A. I. Orlova, S. A. Khainakov


NaZr2(PO4)3 (NZP) and their structural analogues are characterized by a peculiar behaviors on heating – they have different expansion and contraction along different crystallographic directions due to specific arrangements of crystal structure in these compounds. An important feature of such structures is the ability to incorporate into their structural analogues wide variety of metal cations having different size and oxidation states, with different combinations and concentrations. These cations are located in different crystallographic non-equivalent positions of octahedral tetrahedral crystal framework as well as in inter-framework cavities. Through, due to iso- and hetero-valent isomorphism of the cations (and the anions) in NZP, it becomes possible to tuning the compositions and to obtain the compounds with ‘on a plan’ properties. For the design of compounds with low and ultra-low thermal expansion including those with tailored thermal expansion properties, the following crystallochemical principles it seems are promising: 1) Insertion into crystal M1 position the cations having different sizes and, 2) the variation in the composition of compounds, providing different occupation of crystal M1 position. Following these principles we have designed and synthesized the next NZP-type phosphates series: a) where radii of the cations in the M1 crystal position was varied: Zr1/4Zr2(PO4)3 - Th1/4Zr2(PO4)3 (series I); R1/3Zr2(PO4)3 where R= Nd, Eu, Er (series II), b) where the occupation of M1 crystal position was varied: Zr1/4Zr2(PO4)3-Er1/3Zr2(PO4)3 (series III) and Zr1/4Zr2(PO4)3-Sr1/2Zr2(PO4)3 (series IV). The thermal expansion parameters were determined over the range of 25-800ºC. For each series the minimum axial coefficient of thermal expansion αa = αb, αc and their anisotropy Δα = Iαa - αcI, 10-6 K-1 was found as next: -1.51, 1.07, 2.58 for Th1/4Zr2(PO4)3 (series I); -0.72, 0.10, 0.81 for Nd1/3Zr2(PO4)3 (series II); -2.78, 1.35, 4.12 for Er1/6Zr1/8Zr2(PO4)3 (series III); 2.23, 1.32, 0.91 for Sr1/2Zr2(PO4)3 (series IV). The measured tendencies of the thermal expansion of crystals were in good agreement with predicted ones. For one of the members from the studied phosphates namely Th1/16Zr3/16Zr2(PO4)3 structural refinement have been carried out at 25, 200, 600, and 800°C. The dependencies of the structural parameters with the temperature have been determined.

Keywords: high-temperature crystallography, NaZr2(PO4)3, (NZP) analogs, structural-chemical principles, tuning thermal expansion

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5154 Thiourea: Single Crystal with Non Linear Optical Characteristics

Authors: Kishor C. Poria, Deepak Adroja, Arvind Bajaj


During the last few decades, the growth of single crystals has attained enormous importance for both academic research and technology. Single crystals are pillars of modern technology. In recent emerging trends of photonics and optoelectronics technology, there has been increased need for organic and semi organic materials for Non-Linear Optical (NLO) applications. The paper dealt with the initiation of good single crystals of thiourea and metal doped thiourea. The authors have successfully grown thiourea (pure) and metal doped thiourea crystals using relatively simple and inexpensive slow evaporation of aqueous solution technique. Pure thiourea crystals were grown with different light intensities and frequencies as there growth conditions. Metals (Cu, Co, Ni, Fe) doped crystals were grown using a simple evaporation technique. The paper explains growth methods and associated grown parameters in detail. The average size of the crystal is varied in size from 40 mm x 1mm to 1.5 mm x 1.5 mm to 0.5 mm. Crystals obtained are hexagonal, tetragonal, and rectangular in shape with different optical qualities. All grown crystals are characterized using X-Ray Diffraction Analysis (XRD), Ultra Violet Visible analysis, and Fourier Transform Infrared Spectrometry. Their non-linear optical characteristics were determined by Second Harmonic Generation (SHG) and their Laser Dispersive analysis. The grown crystals are characterized using Nd:YAG laser and the highest conversion efficiency of the signal pass light are calculated. It shows 58 % of standard values for KDP crystals. All results are summarized in this work.

Keywords: crystal, metal-doped thiourea, non-linear optical, NLO, thiourea

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5153 The Study on Treatment Technology of Fused Carbonized Blast Furnace Slag

Authors: Jiaxu Huang


The melt carbonized blast furnace slag containing TiC was produced by carbothermal reduction of high titanium blast furnace slag. The treatment technology of melt carbonized blast furnace slag with TiC as raw material was studied, including the influence of different cooling methods, crushing atmosphere and sieving particle size on the target product TiC in the slag. The results show that air-cooling and water-cooling have little effect on TiC content of molten carbide blast furnace slag, and have great effect on crystal structure and grain size. TiC content in slag is different when carbide blast furnace slag is crushed in argon atmosphere and air atmosphere. After screening, the difference of TiC content of carbide blast furnace slag with different particle size distribution is obvious. The average TiC content of 100-400 mesh carbide blast furnace slag is 14%. And the average TiC content of carbide blast furnace slag with particle size less than 400 mesh is 10.5%.

Keywords: crushing atmosphere, cooling methods, sieving particle size, TiC

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5152 Effect of Chemical Additive on Fixed Abrasive Polishing of LBO Crystal with Non-Water Based Slurry

Authors: Jun Li, Wenze Wang, Zhanggui Hu, Yongwei Zhu, Dunwen Zuo


Non-water based fixed abrasive polishing was adopted to manufacture LBO crystal for nano precision surface quality because of its deliquescent. Ethyl alcohol was selected as the non-water based slurry solvent and ethanediamine, lactic acid, hydrogen peroxide were add in the slurry as a chemical additive, respectively. Effect of different additives with non-water based slurry on material removal rate, surface topography, microscopic appearances and surface roughness were investigated in fixed abrasive polishing of LBO crystal. The results show the best surface quality of LBO crystal with surface roughness Sa 8.2 nm and small damages was obtained by non-water based slurry with lactic acid. Non-water based fixed abrasive polishing can achieve nano precision surface quality of LBO crystal with high material removal.

Keywords: non-water based slurry, LBO crystal, fixed abrasive polishing, surface roughness

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5151 Multi-Scale Modeling of Ti-6Al-4V Mechanical Behavior: Size, Dispersion and Crystallographic Texture of Grains Effects

Authors: Fatna Benmessaoud, Mohammed Cheikh, Vencent Velay, Vanessa Vidal, Farhad Rezai-Aria, Christine Boher


Ti-6Al-4V titanium alloy is one of the most widely used materials in aeronautical and aerospace industries. Because of its high specific strength, good fatigue, and corrosion resistance, this alloy is very suitable for moderate temperature applications. At room temperature, Ti-6Al-4V mechanical behavior is generally controlled by the behavior of alpha phase (beta phase percent is less than 8%). The plastic strain of this phase notably based on crystallographic slip can be hindered by various obstacles and mechanisms (crystal lattice friction, sessile dislocations, strengthening by solute atoms and grain boundaries…). The grains aspect of alpha phase (its morphology and texture) and the nature of its crystallographic lattice (which is hexagonal compact) give to plastic strain heterogeneous, discontinuous and anisotropic characteristics at the local scale. The aim of this work is to develop a multi-scale model for Ti-6Al-4V mechanical behavior using crystal plasticity approach; this multi-scale model is used then to investigate grains size, dispersion of grains size, crystallographic texture and slip systems activation effects on Ti-6Al-4V mechanical behavior under monotone quasi-static loading. Nine representative elementary volume (REV) are built for taking into account the physical elements (grains size, dispersion and crystallographic) mentioned above, then boundary conditions of tension test are applied. Finally, simulation of the mechanical behavior of Ti-6Al-4V and study of slip systems activation in alpha phase is reported. The results show that the macroscopic mechanical behavior of Ti-6Al-4V is strongly linked to the active slip systems family (prismatic, basal or pyramidal). The crystallographic texture determines which family of slip systems can be activated; therefore it gives to the plastic strain a heterogeneous character thus an anisotropic macroscopic mechanical behavior of Ti-6Al-4V alloy modeled. The grains size influences also on mechanical proprieties of Ti-6Al-4V, especially on the yield stress; by decreasing of the grain size, the yield strength increases. Finally, the grains' distribution which characterizes the morphology aspect (homogeneous or heterogeneous) gives to the deformation fields distribution enough heterogeneity because the crystallographic slip is easier in large grains compared to small grains, which generates a localization of plastic deformation in certain areas and a concentration of stresses in others.

Keywords: multi-scale modeling, Ti-6Al-4V alloy, crystal plasticity, grains size, crystallographic texture

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5150 Turmeric Mediated Synthesis and Characterization of Cerium Oxide Nanoparticles

Authors: Nithin Krisshna Gunasekaran, Prathima Prabhu Tumkur, Nicole Nazario Bayon, Krishnan Prabhakaran, Joseph C. Hall, Govindarajan T. Ramesh


Cerium oxide and turmeric have antioxidant properties, which have gained interest among researchers to study their applications in the field of biomedicine, such asanti-inflammatory, anticancer, and antimicrobial applications. In this study, the turmeric extract was prepared and mixed with cerium nitrate hexahydrate, stirred continuously to obtain a homogeneous solution and then heated on a hot plate to get the supernatant evaporated, then calcinated at 600°C to obtain the cerium oxide nanoparticles. Characterization of synthesized cerium oxide nanoparticles through Scanning Electron Microscopy determined the particle size to be in the range of 70 nm to 250 nm. Energy Dispersive X-Ray Spectroscopy determined the elemental composition of cerium and oxygen. Individual particles were identified through the characterization of cerium oxide nanoparticles using Field Emission Scanning Electron Microscopy, in which the particles were determined to be spherical and in the size of around 70 nm. The presence of cerium oxide was assured by analyzing the spectrum obtained through the characterization of cerium oxide nanoparticles by Fourier Transform Infrared Spectroscopy. The crystal structure of cerium oxide nanoparticles was determined to be face-centered cubic by analyzing the peaks obtained through theX-Ray Diffraction method. The crystal size of cerium oxide nanoparticles was determined to be around 13 nm by using the Debye Scherer equation. This study confirmed the synthesis of cerium oxide nanoparticles using turmeric extract.

Keywords: antioxidant, characterization, cerium oxide, synthesis, turmeric

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5149 The Effect of the Crystal Field Interaction on the Critical Temperatures and the Sublattice Magnetizations of a Mixedspin-3/2 and Spin-5/2 Ferromagnetic System

Authors: Fathi Abubrig, Mohamed Delfag, Suad Abuzariba


The influence of the crystal field interactions on the mixed spin-3/2 and spin-5/2 ferromagnetic Ising system is considered by using the mean field theory based on Bogoliubov inequality for the Gibbs free energy. The ground-state phase diagram is constructed, the phase diagrams of the second-order critical temperatures are obtained, and the thermal variation of the sublattice magnetizations is investigated in detail. We find some interesting phenomena for the sublattice magnetizations at particular values of the crystal field interactions.

Keywords: crystal field, Ising system, ferromagnetic, magnetization, phase diagrams

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5148 Sorption of Crystal Violet from Aqueous Solution Using Chitosan−Charcoal Composite

Authors: Kingsley Izuagbe Ikeke, Abayomi O. Adetuyi


The study investigated the removal efficiency of crystal violet from aqueous solution using chitosan-charcoal composite as adsorbent. Deproteination was carried out by placing 200g of powdered snail shell in 4% w/v NaOH for 2hours. The sample was then placed in 1% HCl for 24 hours to remove CaCO3. Deacetylation was done by boiling in 50% NaOH for 2hours. 10% Oxalic acid was used to dissolve the chitosan before mixing with charcoal at 55°C to form the composite. The composite was characterized by Fourier Transform Infra-Red and Scanning Electron Microscopy measurements. The efficiency of adsorption was evaluated by varying pH of the solution, contact time, initial concentration and adsorbent dose. Maximum removal of crystal violet by composite and activated charcoal was attained at pH10 while maximum removal of crystal violet by chitosan was achieved at pH 8. The results showed that adsorption of both dyes followed the pseudo-second-order rate equation and fit the Langmuir and Freundlich isotherms. The data showed that composite was best suited for crystal violet removal and also did relatively well in the removal of alizarin red. Thermodynamic parameters such as enthalpy change (ΔHº), free energy change (ΔGº) and entropy change (ΔSº) indicate that adsorption process of Crystal Violet was endothermic, spontaneous and feasible respectively.

Keywords: crystal violet, chitosan−charcoal composite, extraction process, sorption

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5147 Propagation of Cos-Gaussian Beam in Photorefractive Crystal

Authors: A. Keshavarz


A physical model for guiding the wave in photorefractive media is studied. Propagation of cos-Gaussian beam as the special cases of sinusoidal-Gaussian beams in photorefractive crystal is simulated numerically by the Crank-Nicolson method in one dimension. Results show that the beam profile deforms as the energy transfers from the center to the tails under propagation. This simulation approach is of significant interest for application in optical telecommunication. The results are presented graphically and discussed.

Keywords: beam propagation, cos-Gaussian beam, numerical simulation, photorefractive crystal

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5146 Multi-Walled Carbon Nanotubes as Nucleating Agents

Authors: Rabindranath Jana, Plabani Basu, Keka Rana


Nucleating agents are widely used to modify the properties of various polymers. The rate of crystallization and the size of the crystals have a strong impact on mechanical and optical properties of a polymer. The addition of nucleating agents to the semi-crystalline polymers provides a surface on which the crystal growth can start easily. As a consequence, fast crystal formation will result in many small crystal domains so that the cycle times for injection molding may be reduced. Moreover, the mechanical properties e.g., modulus, tensile strength, heat distortion temperature and hardness may increase. In the present work, multi-walled carbon nanotubes (MWNTs) as nucleating agents for the crystallization of poly (e-caprolactone)diol (PCL). Thus nanocomposites of PCL filled with MWNTs were prepared by solution blending. Differential scanning calorimetry (DSC) tests were carried out to study the effect of CNTs on on-isothermal crystallization of PCL. The polarizing optical microscopy (POM), and wide-angle X-ray diffraction (WAXD) were used to study the morphology and crystal structure of PCL and its nanocomposites. It is found that MWNTs act as effective nucleating agents that significantly shorten the induction period of crystallization and however, decrease the crystallization rate of PCL, exhibiting a remarkable decrease in the Avrami exponent n, surface folding energy σe and crystallization activation energy ΔE. The carbon-based fillers act as templates for hard block chains of PCL to form an ordered structure on the surface of nanoparticles during the induction period, bringing about some increase in equilibrium temperature. The melting process of PCL and its nanocomposites are also studied; the nanocomposites exhibit two melting peaks at higher crystallization temperature which mainly refer to the melting of the crystals with different crystal sizes however, PCL shows only one melting temperature.

Keywords: poly(e-caprolactone)diol, multiwalled carbon nanotubes, composite materials, nonisothermal crystallization, crystal structure, nucleation

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