Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 11

Crystallinity Related Abstracts

11 Impact of Natural Degradation of Low Density Polyethylene on Its Morphology

Authors: Meryem Imane Babaghayou, Asma Abdelhafidi, Salem Fouad Chabira, Mohammed Sebaa


A challenge of plastics industries is the realization of materials that resist the degradation in its application environment, and that to guarantee a longer life time therefore an optimal time of use. Blown extruded films of low-density polyethylene (LDPE) supplied by SABIC SAUDI ARABIA blown and extruded in SOFIPLAST company in Setif ALGERIA , have been subjected to climatic ageing in a sub-Saharan facility at Laghouat (Algeria) with direct exposure to sun. Samples were characterized by X-ray diffraction (XRD) and differential scanning calorimetry (DSC) techniques after prescribed amounts of time up to 8 months. It has been shown via these two techniques the impact of UV irradiation on the morphological development of a plastic material, especially the crystallinity degree which increases with exposure time. The reason of these morphological changes is related to photooxidative reactions leading to cross linking in the beginning and to chain scissions for an advanced stage of ageing this last ones are the first responsible. The crystallinity degree change is essentially controlled by the secondary crystallization of the amorphous chains whose mobility is enhanced by the chain scission processes. The diffusion of these short segments integrates the surface of the lamellae increasing in this way their thicknesses. The results presented highlight the complexity of the involved phenomena.

Keywords: Ageing, Crystallinity, XRD, DSC, Low Density poly (Ethylene)

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10 Effects of Surface Topography on Roughness of Glazed Ceramic Substrates

Authors: R. Sarjahani, M. Sheikhattar, S. Javadpour, B. Hashemi


Glazes and their surface characterization is an important subject for ceramic industries. Fabrication of a super smooth surface resistant to stains is a big improvement for those industries. In this investigation, surface topography of popular glazes such as Zircon and Titania based opaque glazes, calcium based matte glaze and transparent glaze has been analyzed by Marsurf M300, SEM, EDS and XRD. Results shows that surface roughness of glazes seriously depends on surface crystallinity, crystal size and shapes.

Keywords: Crystallinity, Topography, glaze, surface roughness

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9 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: Crystallinity, XRD, Nanocrystalline cellulose, cotton linter

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8 Production and Characterization of Nanofibrillated Cellulose from Kenaf Core (Hibiscus cannabinus) via Ultrasonic

Authors: R. Rosazley, M. A. Izzati, A. W. Fareezal, M. Z. Shazana, I. Rushdan, M. A. Ainun Zuriyati


This study focuses on production and characterizations of nanofibrillated cellulose (NFC) from kenaf core. NFC was produced by employing ultrasonic treatments in aqueous solution. Field emission scanning electron microscope (FESEM) and scanning transmission electron microscopy (STEM) were used to study the size and morphology structure. The chemical and characteristics of the cellulose and NFC were studied using Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and viscometer. Degrees of polymerization (DP) of cellulose and NFC were obtained via viscosity value. Results showed that 5 to 47 nm diameters of fibrils were measured. Moreover, the thermal stability of the NFC was increased as compared to the cellulose that confirmed by TGA analysis. It was also found that NFC had higher crystallinity and lower viscosity than the cellulose which were measured by XRD and viscometer, respectively. The NFC characteristics have enormous prospect related to bio-nanocomposite.

Keywords: Ultrasonic, Crystallinity, nanofibrillated cellulose, kenaf core

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7 Effect of the Binary and Ternary Exchanges on Crystallinity and Textural Properties of X Zeolites

Authors: H. Hammoudi, S. Bendenia, K. Marouf-Khelifa, R. Marouf, J. Schott, A. Khelifa


The ionic exchange of the NaX zeolite by Cu2+ and/or Zn2+ cations is progressively driven while following the development of some of its characteristic: crystallinity by XR diffraction, profile of isotherms, RI criterion, isosteric adsorption heat and microporous volume using both the Dubinin–Radushkevich (DR) equation and the t-plot through the Lippens–de Boer method which also makes it possible to determine the external surface area. Results show that the cationic exchange process, in the case of Cu2+ introduced at higher degree, is accompanied by crystalline degradation for Cu(x)X, in contrast to Zn2+-exchanged zeolite X. This degradation occurs without significant presence of mesopores, because the RI criterion values were found to be much lower than 2.2. A comparison between the binary and ternary exchanges shows that the curves of CuZn(x)X are clearly below those of Zn(x)X and Cu(x)X, whatever the examined parameter. On the other hand, the curves relating to CuZn(x)X tend towards those of Cu(x)X. This would again confirm the sensitivity of the crystalline structure of CuZn(x)X with respect to the introduction of Cu2+ cations. An original result is the distortion of the zeolitic framework of X zeolites at middle exchange degree, when Cu2+ competes with another divalent cation, such as Zn2+, for the occupancy of sites distributed within zeolitic cavities. In other words, the ternary exchange accentuates the crystalline degradation of X zeolites. An unexpected result also is the no correlation between crystal damage and the external surface area.

Keywords: Adsorption, Zeolite, Crystallinity, ion exchange

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6 Influence of Argon Gas Concentration in N2-Ar Plasma for the Nitridation of Si in Abnormal Glow Discharge

Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq


Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si3N4 confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N2 plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: Crystallinity, Nitriding, sputtering, glow discharge

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5 Effect of Enzymatic Modification on the Crystallinity of Cellulose Pulps

Authors: J. Janicki, M. Rom, C. Slusarczyk, J. Fabia, M. Siika-aho, K. Marjamaa, K. Kruus, K. Langfelder, C. Steel, M. Paloheimo, T. Puranen, S. Mäkinen, D. Wawro


The cellulose is one of the most abundant polymers in the world, however, its application in the high-end value products such as films or fibres, it triggered by the cellulose properties. The noticeable presence of hydrogen bonding reflected with partially crystalline structure makes the cellulose insoluble in common solvents and not meltable. The existing technologies, such as viscose process, suffer from environmental and economical problems, because of the risk of harmful chemicals liberation during the spinning process. The enzymatic modification of cellulose with endoglucanase makes it directly alkali soluble in NaOH solution, giving the opportunities for film and fibers formation. As the effect of enzymatic treatment, there are observed changes in crystalline structure and accompanying changes of the affinity of cellulose to water, demonstrated by water retention value. The objective of the project ELMO - Novel carbohydrate modifying enzymes for fibre modification is is to develop new enzyme products for modification of dissolving grade pulps. The aim is to increase the reactivity of dissolving grade pulps and remove residual hemicellulose. The scientific aim of this paper is to present the effect of enzymatic treatment on the crystallinity and affinity to water of cellulose pulps modified with enzymes.

Keywords: enzyme, Crystallinity, Cellulose, WAXS

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4 Structural and Morphological Characterization of the Biomass of Aquatics Macrophyte (Egeria densa) Submitted to Thermal Pretreatment

Authors: Joyce Cruz Ferraz Dutra, Marcele Fonseca Passos, Rubens Maciel Filho, Douglas Fernandes Barbin, Gustavo Mockaitis


The search for alternatives to control hunger in the world, generated a major environmental problem. Intensive systems of fish production can cause an imbalance in the aquatic environment, triggering the phenomenon of eutrophication. Currently, there are many forms of growth control aquatic plants, such as mechanical withdrawal, however some difficulties arise for their final destination. The Egeria densa is a species of submerged aquatic macrophyte-rich in cellulose and low concentrations of lignin. By applying the concept of second generation energy, which uses lignocellulose for energy production, the reuse of these aquatic macrophytes (Egeria densa) in the biofuels production can turn an interesting alternative. In order to make lignocellulose sugars available for effective fermentation, it is important to use pre-treatments in order to separate the components and modify the structure of the cellulose and thus facilitate the attack of the microorganisms responsible for the fermentation. Therefore, the objective of this research work was to evaluate the structural and morphological transformations occurring in the biomass of aquatic macrophytes (E.densa) submitted to a thermal pretreatment. The samples were collected in an intensive fish growing farm, in the low São Francisco dam, in the northeastern region of Brazil. After collection, the samples were dried in a 65 0C ventilation oven and milled in a 5mm micron knife mill. A duplicate assay was carried, comparing the in natural biomass with the pretreated biomass with heat (MT). The sample (MT) was submitted to an autoclave with a temperature of 1210C and a pressure of 1.1 atm, for 30 minutes. After this procedure, the biomass was characterized in terms of degree of crystallinity and morphology, using X-ray diffraction (XRD) techniques and scanning electron microscopy (SEM), respectively. The results showed that there was a decrease of 11% in the crystallinity index (% CI) of the pretreated biomass, leading to the structural modification in the cellulose and greater presence of amorphous structures. Increases in porosity and surface roughness of the samples were also observed. These results suggest that biomass may become more accessible to the hydrolytic enzymes of fermenting microorganisms. Therefore, the morphological transformations caused by the thermal pretreatment may be favorable for a subsequent fermentation and, consequently, a higher yield of biofuels. Thus, the use of thermally pretreated aquatic macrophytes (E.densa) can be an environmentally, financially and socially sustainable alternative. In addition, it represents a measure of control for the aquatic environment, which can generate income (biogas production) and maintenance of fish farming activities in local communities.

Keywords: biofuels, Morphology, Crystallinity, aquatics macrophyte, pretreatment thermal

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3 Graft Copolymerization of Cellulose Acetate with Nitro-N-Amino Phenyl Maleimides

Authors: Azza. A. Al-Ghamdi, Abir. A. Abdel-Naby


The construction of Nitro -N-amino phenyl maleimide branches onto Cellulose acetate (CA) substrate by free radical graft copolymerization using benzoyl peroxide as initiator led to formation of highly thermal stable copolymers as shown from the results of gravimetric analysis (TGA). CA-g-2,4-dinitro amino phenyl maleimide exhibited higher thermal stability than the CA-g-4-nitro amino phenyl maleimide as shown from the initial decomposition temperature (To). This is due to the ability of nitro group to form hydrogen bonding with hydroxyl group of the glucopyranose ring which increases the crystallinity of polymeric matrix. The crystalline shapes representing the graft part are clearly distinct in the Emission scanning electron microscope (ESEM) morphology of the copolymer. A suggested reaction mechanism for the grafting process was also discussed.

Keywords: Crystallinity, Thermal Properties, cellulose acetate, graft copolymerization

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2 Hot Air Flow Annealing of MAPbI₃ Perovskite: Structural and Optical Properties

Authors: Mouad Ouafi, Lahoucine Atourki, Larbi Laanab, Erika Vega, Miguel Mollar, Bernabe Marib, Boujemaa Jaber


Despite the astonishing emergence of the methylammonium lead triiodide perovskite as a promising light harvester for solar cells, their physical properties in solution-processed MAPbI₃ are still crucial and need to be improved. The objective of this work is to investigate the hot airflow effect during the growth of MAPbI₃ films using the spin-coating process on their structural, optical and morphological proprieties. The experimental results show that many physical proprieties of the perovskite strongly depend on the air flow temperature and the optimization which has a beneficial effect on the perovskite quality. In fact, a clear improvement of the crystallinity and the crystallite size of MAPbI₃ perovskite is demonstrated by the XRD analyses, when the airflow temperature is increased up to 100°C. Alternatively, as far as the surface morphology is concerned, SEM micrographs show that significant homogenous nucleation, uniform surface distribution and pin holes free with highest surface coverture of 98% are achieved when the airflow temperature reaches 100°C. At this temperature, the improvement is also observed when considering the optical properties of the films. By contrast, a remarkable degradation of the MAPbI₃ perovskites associated to the PbI₂ phase formation is noticed, when the hot airflow temperature is higher than 100°C, especially 300°C.

Keywords: Crystallinity, hot air flow, surface coverage, perovskite morphology

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1 Tailoring Piezoelectricity of PVDF Fibers with Voltage Polarity and Humidity in Electrospinning

Authors: Piotr K. Szewczyk, Arkadiusz Gradys, Sungkyun Kim, Luana Persano, Mateusz M. Marzec, Oleksander Kryshtal, Andrzej Bernasik, Sohini Kar-Narayan, Pawel Sajkiewicz, Urszula Stachewicz


Piezoelectric polymers have received great attention in smart textiles, wearables, and flexible electronics. Their potential applications range from devices that could operate without traditional power sources, through self-powering sensors, up to implantable biosensors. Semi-crystalline PVDF is often proposed as the main candidate for industrial-scale applications as it exhibits exceptional energy harvesting efficiency compared to other polymers combined with high mechanical strength and thermal stability. Plenty of approaches have been proposed for obtaining PVDF rich in the desired β-phase with electric polling, thermal annealing, and mechanical stretching being the most prevalent. Electrospinning is a highly tunable technique that provides a one-step process of obtaining highly piezoelectric PVDF fibers without the need for post-treatment. In this study, voltage polarity and relative humidity influence on electrospun PVDF, fibers were investigated with the main focus on piezoelectric β-phase contents and piezoelectric performance. Morphology and internal structure of fibers were investigated using scanning (SEM) and transmission electron microscopy techniques (TEM). Fourier Transform Infrared Spectroscopy (FITR), wide-angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) were used to characterize the phase composition of electrospun PVDF. Additionally, surface chemistry was verified with X-ray photoelectron spectroscopy (XPS). Piezoelectric performance of individual electrospun PVDF fibers was measured using piezoresponse force microscopy (PFM), and the power output from meshes was analyzed via custom-built equipment. To prepare the solution for electrospinning, PVDF pellets were dissolved in dimethylacetamide and acetone solution in a 1:1 ratio to achieve a 24% solution. Fibers were electrospun with a constant voltage of +/-15kV applied to the stainless steel nozzle with the inner diameter of 0.8mm. The flow rate was kept constant at 6mlh⁻¹. The electrospinning of PVDF was performed at T = 25°C and relative humidity of 30 and 60% for PVDF30+/- and PVDF60+/- samples respectively in the environmental chamber. The SEM and TEM analysis of fibers produced at a lower relative humidity of 30% (PVDF30+/-) showed a smooth surface in opposition to fibers obtained at 60% relative humidity (PVDF60+/-), which had wrinkled surface and additionally internal voids. XPS results confirmed lower fluorine content at the surface of PVDF- fibers obtained by electrospinning with negative voltage polarity comparing to the PVDF+ obtained with positive voltage polarity. Changes in surface composition measured with XPS were found to influence the piezoelectric performance of obtained fibers what was further confirmed by PFM as well as by custom-built fiber-based piezoelectric generator. For PVDF60+/- samples humidity led to an increase of β-phase contents in PVDF fibers as confirmed by FTIR, WAXS, and DSC measurements, which showed almost two times higher concentrations of β-phase. A combination of negative voltage polarity with high relative humidity led to fibers with the highest β-phase contents and the best piezoelectric performance of all investigated samples. This study outlines the possibility to produce electrospun PVDF fibers with tunable piezoelectric performance in a one-step electrospinning process by controlling relative humidity and voltage polarity conditions. Acknowledgment: This research was conducted within the funding from m the Sonata Bis 5 project granted by National Science Centre, No 2015/18/E/ST5/00230, and supported by the infrastructure at International Centre of Electron Microscopy for Materials Science (IC-EM) at AGH University of Science and Technology. The PFM measurements were supported by an STSM Grant from COST Action CA17107.

Keywords: Electrospinning, Crystallinity, PVDF, voltage polarity

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