scholarly journals Effect of the Incorporation of Polycaprolactone (PCL) on the Retrogradation of Binary Blends with Cassava Thermoplastic Starch (TPS)

Polymers ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 38
Author(s):  
José Herminsul Mina Hernandez
Keyword(s):  
Structural Changes ◽  
Thermoplastic Starch ◽  
X Ray Diffraction ◽  
Binary Blend ◽  
Binary Blends ◽  
Immiscible Blends ◽  
Single Screw Extrusion ◽  
Screw Extrusion ◽  
Storage Times ◽  
Short Times

The effects of incorporating polycaprolactone (PCL) in three binary blends with cassava thermoplastic starch (TPS) at TPS/PCL ratios of 60/40, 50/50, and 40/60 were studied. TPS previously obtained by single-screw extrusion was manually mixed with PCL and then transformed by extrusion. The results’ analysis focused mainly on monitoring the retrogradation phenomenon in TPS for different storage times at two relative humidities (29% and 54%) and constant temperature (25 °C). With the plasticization of the starch, a predominantly amorphous mass was generated, as evidenced by the scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) results. The results suggested that two opposite processes coexisted simultaneously: retrogradation, which stiffened the material, and plasticization, which softened it, with the latter mechanism predominating at short times and reversing at longer times. With the incorporation of PCL, immiscible blends were obtained in which TPS was the dispersed phase; the mechanical properties improved with the amount of PCL added. The properties of the binary blends as a function of time showed a trend similar to that observed for TPS alone; this finding indicated that the TPS/PCL interactions were not strong enough to affect the structural changes in the TPS, which continued to occur regardless of the PCL content. Finally, it was found that for the binary blend, the relative humidity during storage was more significant to the retrogradation phenomenon than the amount of PCL.

Influence of Aging Time on the Structural Changes of Cassava Thermoplastic Starch

2012 ◽  
Vol 1372 ◽  
Author(s):  
José H. Mina ◽  
Alex Valadez ◽  
Pedro J. Herrera-Franco ◽  
Tanit Toledano
Keyword(s):  
Yield Stress ◽  
Amorphous Phase ◽  
Structural Changes ◽  
Thermoplastic Starch ◽  
X Ray Diffraction ◽  
X Ray ◽  
Second Stage ◽  
Diffraction Patterns ◽  
Type V ◽  
Stress Drops

ABSTRACTIn this work the change in the structural properties of cassava (manihot sculenta Crantz) thermoplastic starch (TPS) under controlled environment (humidity and temperature) was studied. Fourier Transform Infrared spectroscopy (FTIR) and X-ray diffraction (XRD) results showed an evident increasing in the amorphous phase of the TPS regarding the native starch. There was a relative decrease of the band at 1047 cm-1 associated to crystalline structure of starch compared to the amorphous peak at 1022 cm-1. The X-ray diffraction patterns confirmed the increment of the amorphous phase in the TPS samples. Likewise the X-ray diffraction patterns shows evidence of residual type C crystallinity and the formation of a new crystalline phase type VH due to the orientation induced in plasticization process. In first stage of conditioning the tensile yield stress drops from 7.5 drops to 0.5 MPa and the break strain increases 1000%. At the same time it seems that the crystallinity of the samples increases as was evidenced by the gradually increasing of the FTIR band at 1047 cm-1. In a second stage, the yield stress increases, the break strain drops and the crystallinity continue growing steadily. These findings suggest that coexist two phenomena simultaneously in the samples. A phenomenon of re-crystallization (retrogradation) that tends to make the material more stiff and a process of plasticization that tends to softening it. It seems that the latter mechanism predominates in the first stage, at short times, and the former in the second stage, at older times.

scholarly journals Study of the Effects Induced by Ball Milling Treatment on Different Types of Hydrocolloids in a Corn Starch–Rice Flour System

Foods ◽  
2020 ◽  
Vol 9 (4) ◽  
pp. 517 ◽  
Author(s):  
Luca Nuvoli ◽  
Paola Conte ◽  
Sebastiano Garroni ◽  
Valeria Farina ◽  
Antonio Piga ◽  
...  
Keyword(s):  
Ball Milling ◽  
Structural Changes ◽  
Guar Gum ◽  
Corn Starch ◽  
Rice Flour ◽  
Pasting Properties ◽  
X Ray Diffraction ◽  
Binary Blends ◽  
Starch Gels ◽  
The Individual

The effects of ball milling treatment on both the structure and properties of guar gum (GG), tara gum (TG), and methylcellulose (MC) were analyzed prior to assessing their potential interactions with starch components when they are used alone or in blends in a corn starch–rice flour system. X-ray diffraction profiles showed that the ball milling caused a reduction in the crystallin domain and, in turn, a diminished viscosity of the GG aqueous solutions. Despite an increase in its viscosity properties, effects on TG were minimal, while the milled MC exhibited reduced crystallinity, but similar viscosity. When both milled and un-milled hydrocolloids were individually added to the starch–flour system, the pasting properties of the resulting mixtures seemed to be affected by the type of hydrocolloid added rather than the structural changes induced by the treatment. All hydrocolloids increased the peak viscosity of the binary blends (especially pure GG), but only milled and un-milled MC showed values of setback and final viscosity similar to those of the individual starch. Ball milling seemed to be more effective when two combined hydrocolloids (milled GG and MC) were simultaneously used. No significant differences were observed in the viscoelastic properties of the blends, except for un-milled GG/starch, milled TG/starch, and milled MC/milled TG/starch gels.

scholarly journals Rheological, Thermal, Superficial, and Morphological Properties of Thermoplastic Achira Starch Modified with Lactic Acid and Oleic Acid

Molecules ◽  
2019 ◽  
Vol 24 (24) ◽  
pp. 4433 ◽  
Author(s):  
Carolina Caicedo ◽  
Rocío Yaneli Aguirre Loredo ◽  
Abril Fonseca García ◽  
Omar Hernán Ossa ◽  
Aldo Vázquez Arce ◽  
...  
Keyword(s):  
Lactic Acid ◽  
Oleic Acid ◽  
Complex Viscosity ◽  
Thermoplastic Starch ◽  
Residual Energy ◽  
Morphological Properties ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Rheological Analysis ◽  
Acid Agent

The modification of achira starch a thermoplastic biopolymer is shown. Glycerol and sorbitol, common plasticizers, were used in the molten state with organic acids such as oleic acid and lactic acid obtaining thermodynamically more stable products. The proportion of starch:plasticizer was 70:30, and the acid agent was added in portions from 3%, 6%, and 9% by weight. These mixtures were obtained in a torque rheometer for 10 min at 130 °C. The lactic acid managed to efficiently promote the gelatinization process by increasing the available polar sites towards the surface of the material; as a result, there were lower values in the contact angle, these results were corroborated with the analysis performed by differential scanning calorimetry and X-ray diffraction. The results derived from oscillatory rheological analysis had a viscous behavior in the thermoplastic starch samples and with the presence of acids; this behavior favors the transitions from viscous to elastic. The mixture of sorbitol or glycerol with lactic acid promoted lower values of the loss module, the storage module, and the complex viscosity, which means lower residual energy in the transition of the viscous state to the elastic state; this allows the compounds to be scaled to conventional polymer transformation processes.

Structural changes induced by cation ordering in ferrotapiolite

2006 ◽  
Vol 70 (3) ◽  
pp. 319-328 ◽  
Author(s):  
M. Zema ◽  
S.C. Tarantino ◽  
A. Giorgiani
Keyword(s):  
Structural Changes ◽  
Rapid Determination ◽  
Linear Increase ◽  
X Ray Diffraction ◽  
Ionic Radii ◽  
Structural Modifications ◽  
Lattice Constants ◽  
Structure Factors ◽  
Polyhedral Volumes ◽  
Degree Of Order

AbstractStructural modifications as a function of the degree of order (Q) in FeTa2O6 ferrotapiolite have been characterized by means of single-crystal X-ray diffraction (SC-XRD). A total of 26 datasets covering the range of Q between 0.154 and 1 have been obtained by thermal treatments followed by quenching of natural tapiolite crystals. Ordering of Fe2+ at the A sites and of Ta5+ at the B sites causes a linear increase in the a/c lattice constants ratio, as a consequence of a linear decrease of the c dimension and only slight modifications of the a parameter. Calibration of a/c vs. Q represents a very useful tool for a rapid determination of the degree of order of tapiolite samples. Polyhedral volumes of the two octahedral sites vary linearly with Q as a consequence of the different ionic radii of the two species. Both the sites remain almost regular at all Q values but the B site shows an increasing off-centre displacement of the cation with increasing Q. Observed structure factors of supercell reflections, characterized by l ≠ 3n, increase linearly as a function of Q, thus representing a further tool for a quick evaluation of the degree of order.

scholarly journals High temperature structural study of decagonal Al-Cu-Rh quasicrystal.

2014 ◽  
Vol 70 (a1) ◽  
pp. C94-C94
Author(s):  
Pawel Kuczera ◽  
Walter Steurer
Keyword(s):  
Structural Changes ◽  
Configurational Entropy ◽  
Lattice Vibrations ◽  
X Ray Diffraction ◽  
Stabilization Mechanism ◽  
X Ray ◽  
Comparative Structure ◽  
The Stability

The structure of d(ecagonal)-Al-Cu-Rh has been studied as a function of temperature by in-situ single-crystal X-ray diffraction in order to contribute to the discussion on energy or entropy stabilization of quasicrystals (QC) [1]. The experiments were performed at 293 K, 1223 K, 1153 K, 1083 K, and 1013 K. A common subset of 1460 unique reflections was used for the comparative structure refinements at each temperature. The results obtained for the HT structure refinements of d-Al-Cu-Rh QC seem to contradict a pure phasonic-entropy-based stabilization mechanism [2] for this QC. The trends observed for the ln func(I(T1 )/I(T2 )) vs.|k⊥ |^2 plots indicate that the best on-average quasiperiodic order exists between 1083 K and 1153 K, however, what that actually means is unclear. It could indicate towards a small phasonic contribution to entropy, but such contribution is not seen in the structure refinements. A rough estimation of the hypothetic phason instability temperature shows that it would be kinetically inaccessible and thus the phase transition to a 12 Å low T structure (at ~800 K) is most likely not phason-driven. Except for the obvious increase in the amplitude of the thermal motion, no other significant structural changes, in particular no sources of additional phason-related configurational entropy, were found. All structures are refined to very similar R-values, which proves that the quality of the refinement at each temperature is the same. This suggests, that concerning the stability factors, some QCs could be similar to other HT complex intermetallic phases. The experimental results clearly show that at least the ~4 Å structure of d-Al-Cu-Rh is a HT phase therefore entropy plays an important role in its stabilisation mechanism lowering the free energy. However, the main source of this entropy is probably not related to phason flips, but rather to lattice vibrations, occupational disorder unrelated to phason flips like split positions along the periodic axis.

Investigations of Actinide Metals and Compounds under Pressure Provide Important Insights into Bonding and Chemistry

2003 ◽  
Vol 802 ◽  
Author(s):  
R. G. Haire ◽  
S. Heathman ◽  
T. Le Bihan ◽  
A. Lindbaum ◽  
M. Iridi
Keyword(s):  
Structural Changes ◽  
Chemical Properties ◽  
X Ray Diffraction ◽  
Interatomic Distances ◽  
X Ray ◽  
Effect Of Pressure ◽  
Electronic Configurations ◽  
5F Electrons ◽  
Actinide Series ◽  
Alloys And Compounds

ABSTRACTOne effect of pressure on elements and compounds is to decease their interatomic distances, which can bring about dramatic perturbations in their electronic nature and bonding, which can be reflected in changes in physical and/or chemical properties. One important issue in the actinide series of elements is the effect of pressure on the 5f-electrons. We have probed changes in electronic behavior with pressure by monitoring structure by X-ray diffraction, and have studied several actinide metals and compounds from thorium through einsteinium. These studies have employed angle dispersive diffraction using synchrotron radiation, and energy dispersive techniques via conventional X-ray sources. The 5f-electrons of actinide metals and their alloys are often affected significantly by pressure, while with compounds, the structural changes are often not linked to the involvement of 5 f-electron. We shall present some of our more recent findings from studies of selected actinide metals, alloys and compounds under pressure. A discussion of the results in terms of the changes in electronic configurations and bonding with regard to the element's position in the series is also addressed.

Structural changes in titanium dioxide nanocrystals during plastic deformation

2005 ◽  
Vol 38 (5) ◽  
pp. 749-756 ◽  
Author(s):  
Ulrich Gesenhues
Keyword(s):  
Structural Changes ◽  
Crystal Size ◽  
Lower Layer ◽  
High Energy ◽  
Primary Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Hall Method ◽  
Means Of Transmission

The polygonization of 200 nm rutile crystals during dry ball-milling at 10gwas monitored in detail by means of transmission electron microscopy (TEM) and X-ray diffraction (XRD). The TEM results showed how to modify the Williamson–Hall method for a successful evaluation of crystal size and microstrain from XRD profiles. Macrostrain development was determined from the minute shift of the most intense reflection. In addition, changes in pycnometrical density were monitored. Accordingly, the primary crystal is disintegrated during milling into a mosaic of 12–35 nm pieces where the grain boundaries induce up to 1.2% microstrain in a lower layer of 6 nm thickness. Macrostrain in the interior of the crystals rises to 0.03%. The pycnometrical density, reflecting the packing density of atoms in the grain boundary, decreases steadily by 1.1%. The results bear relevance to our understanding of plastic flow and the mechanism of phase transitions of metal oxides during high-energy milling.

scholarly journals Structural Evolution in Wet Mechanically Alloyed Co-Fe-(Ta,W)-B Alloys

Metals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 800
Author(s):  
Vladimír Girman ◽  
Maksym Lisnichuk ◽  
Daria Yudina ◽  
Miloš Matvija ◽  
Pavol Sovák ◽  
...  
Keyword(s):  
Structural Changes ◽  
Magnetic Measurements ◽  
Structural Evolution ◽  
High Energy ◽  
Control Agent ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
X Ray ◽  
Transmission Electron ◽  
X Ray Absorption

In the present study, the effect of wet mechanical alloying (MA) on the glass-forming ability (GFA) of Co43Fe20X5.5B31.5 (X = Ta, W) alloys was studied. The structural evolution during MA was investigated using high-energy X-ray diffraction, X-ray absorption spectroscopy, high-resolution transmission electron microscopy and magnetic measurements. Pair distribution function and extended X-ray absorption fine structure spectroscopy were used to characterize local atomic structure at various stages of MA. Besides structural changes, the magnetic properties of both compositions were investigated employing a vibrating sample magnetometer and thermomagnetic measurements. It was shown that using hexane as a process control agent during wet MA resulted in the formation of fully amorphous Co-Fe-Ta-B powder material at a shorter milling time (100 h) as compared to dry MA. It has also been shown that substituting Ta with W effectively suppresses GFA. After 100 h of MA of Co-Fe-W-B mixture, a nanocomposite material consisting of amorphous and nanocrystalline bcc-W phase was synthesized.

scholarly journals Investigation and Modeling of the Electrical Conductivity of Graphene Nanoplatelets-Loaded Doped-Polypyrrole

Polymers ◽  
2021 ◽  
Vol 13 (7) ◽  
pp. 1034
Author(s):  
Oladipo Folorunso ◽  
Yskandar Hamam ◽  
Rotimi Sadiku ◽  
Suprakas Sinha Ray ◽  
Neeraj Kumar
Keyword(s):  
Electrical Conductivity ◽  
Structural Changes ◽  
Spherical Shape ◽  
Graphene Nanoplatelets ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermogravimetric Analyzer ◽  
Energy Storage Applications ◽  
Electrical Conductivity Data

In this study, a hybrid of graphene nanoplatelets with a polypyrrole having 20 wt.% loading of carbon-black (HGPPy.CB20%), has been fabricated. The thermal stability, structural changes, morphology, and the electrical conductivity of the hybrids were investigated using thermogravimetric analyzer, differential scanning calorimeter, X-ray diffraction analyzer, scanning electron microscope, and laboratory electrical conductivity device. The morphology of the hybrid shows well dispersion of graphene nanoplatelets on the surface of the PPy.CB20% and the transformation of the gravel-like PPy.CB20% shape to compact spherical shape. Moreover, the hybrid’s electrical conductivity measurements showed percolation threshold at 0.15 wt.% of the graphene nanoplatelets content and the curve is non-linear. The electrical conductivity data were analyzed by comparing different existing models (Weber, Clingerman and Taherian). The results show that Taherian and Clingerman models, which consider the aspect ratio, roundness, wettability, filler electrical conductivity, surface interaction, and volume fractions, closely described the experimental data. From these results, it is evident that Taherian and Clingerman models can be modified for better prediction of the hybrids electrical conductivity measurements. In addition, this study shows that graphene nanoplatelets are essential and have a significant influence on the modification of PPy.CB20% for energy storage applications.

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