scholarly journals Multiple β Forms of Saturated Monoacid Triacylglycerol Crystals

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5086
Author(s):  
Seiya Takeguchi ◽  
Arisa Sato ◽  
Hironori Hondoh ◽  
Mio Aoki ◽  
Hidetaka Uehara ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Polymorphic Transformation ◽  
Polarized Light ◽  
X Ray Diffraction ◽  
Melting Points ◽  
Scanning Calorimetry ◽  
Additional Heat ◽  
X Ray ◽  
Mouth Feel ◽  
Spherulite Morphology

We have investigated the polymorphism of triacylglycerol (TAG) crystals as they affect the qualities such as shelf life, mouth feel, and texture of chocolate and other products. Saturated monoacid TAGs, like trilaurin, are considered as models for TAG crystallization; however, there is still debate about the number of their polymorphs that exist. In this study, we characterized a set of novel polymorphs, β forms of saturated monoacid TAGs, which were obtained via different pathways depending on the crystallization history, by polarized light microscopy, X-ray diffraction, and differential scanning calorimetry. Saturated monoacid TAGs were crystallized as the unstable polymorphs, the α or β’ forms first, and then they were transformed into β forms by solid–solid transformations. The β form that had transformed from β’ changed its morphology by a polymorphic transformation, while the β form made from the α form kept its spherulite morphology. The β forms obtained showed different melting points. Additional heat treatment promoted further polymorphic transformation. Four novel β forms were found for each of the saturated monoacid TAGs, trilaurin, trimyristin, tripalmitin, and tristearin. They showed similar polymorphism with the same subcell packing.

Study in performance and morphology of polyamide 12 produced by selective laser sintering technology

2018 ◽  
Vol 24 (5) ◽  
pp. 813-820 ◽  
Author(s):  
Junjie Wu ◽  
Xiang Xu ◽  
Zhihao Zhao ◽  
Minjie Wang ◽  
Jie Zhang
Keyword(s):  
Selective Laser Sintering ◽  
Polarized Light ◽  
Chain Scission ◽  
High Energy ◽  
Laser Sintering ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Content Type ◽  
X Ray ◽  
Polyamide 12

Purpose The purpose of this paper is to investigate the effect of selective laser sintering (SLS) method on morphology and performance of polyamide 12. Design/methodology/approach Crystallization behavior is critical to the properties of semi-crystalline polymers. The crystallization condition of SLS process is much different from others. The morphology of polyamide 12 produced by SLS technology was investigated using scanning electron microscopy, polarized light microscopy, differential scanning calorimetry, X-ray diffraction and wide-angle X-ray diffraction. Findings Too low fill laser power brought about bad fusion of powders, while too high energy input resulted in bad performance due to chain scission of macromolecules. There were three types of crystal in the raw powder material, denoted as overgrowth crystal, ring-banded spherulite and normal spherulite. Originality/value In this work, SLS samples with different sintering parameters, as well as compression molding sample for the purpose of comparison, were made to study the morphology and crystal structure of sintered PA12 in detail.

Structure and properties of polypropylene/organic rectorite nanocomposites

Clay Minerals ◽  
2009 ◽  
Vol 44 (1) ◽  
pp. 35-50 ◽  
Author(s):  
Yun Huang ◽  
Xiaoyan Ma ◽  
Guozheng Liang ◽  
Hongxia Yan
Keyword(s):  
Loss Modulus ◽  
Polarized Light ◽  
Clay Content ◽  
Crystal Form ◽  
Ammonium Bromide ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Monoclinic Crystal ◽  
X Ray

AbstractMelt blending using a twin-screw extruder was used to prepare composites of polypropylene (PP)/organic rectorite (PR). The organic rectorite (OREC) was modified with dodecyl benzyl dimethyl ammonium bromide (1227). Wide-angle X-ray diffraction (WAXD) and transmission electron microscopy were used to investigate the dispersion of OREC in the composites. The d spacings of OREC in PR composites was greater than in OREC itself. The dispersion of OREC particles in the PP polymer matrix was fine and uniform when the clay content was small (2 wt.%). The rheology was characterized using a capillary rheometer. The processing behaviour of the PR system improved as the amount of OREC added increased. Non-isothermal crystallization kinetics were analysed using differential scanning calorimetry. It was shown that the addition of OREC had a heterogeneous nucleation effect on PP, and can accelerate the crystallization. However, only when fine dispersion was achieved, and at lower rates of temperature decrease, was the crystallinity greater. Wide-angle X-ray diffraction and polarized light microscopy were used to observe the crystalline form and crystallite size. The PP in the PR composites exhibited an a-monoclinic crystal form, as in pure PP, and in both cases a spherulite structure was observed. However, the smaller spherulite size in the PR systems indicated that addition of OREC can reduce the crystal size significantly, which might improve the ‘toughness’ of the PP. The mechanical properties (tensile and impact strength) improved when the amount of OREC added was appropriate. Dynamic mechanical analysis showed that the storage modulus (E′) and loss modulus (E″) of the nanocomposites were somewhat greater than those of pure PP when an appropriate amount of OREC was added. Finally, thermogravimetric analysis showed that the PR systems exhibited a greater thermal stability than was seen with pure PP.

Thermotropic behavior of sodium cholesteryl carbonate

2009 ◽  
Vol 24 (1) ◽  
pp. 156-163 ◽  
Author(s):  
Rabkwan Chuealee ◽  
Timothy S. Wiedmann ◽  
Teerapol Srichana
Keyword(s):  
Phase Behavior ◽  
Chemical Structure ◽  
Liquid Crystalline ◽  
Polarized Light ◽  
Wave Number ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
X Ray Scattering ◽  
C Nmr

Sodium cholesteryl carbonate ester (SCC) was synthesized, and its phase behavior was studied. The chemical structure was assessed by solid-state infrared spectroscopy based on vibration analysis. The wave number at 1705 and 1276 cm−1 corresponds to a carbonyl carbonate and O–C–O stretching of SCC, respectively. Molecular structure of SCC was further investigated with 1H and 13C NMR spectroscopy. The chemical shift, for the carbonyl carbonate resonance appeared at 155.5 ppm. A molecular mass of SCC was at m/z of 452. Differential scanning calorimetry (DSC), video-enhanced microscopy (VEM) together with polarized light microscopy, and small-angle x-ray scattering (SAXS) were used to characterize the phase behavior as a function of temperature of SCC. Liquid crystalline phase was formed with SCC. Based on the thermal properties and x-ray diffraction, it appears that SCC forms a structure analogous to the type II monolayer structure observed with cholesterol esters.

scholarly journals Stacking Control by Molecular Symmetry of Sterically Protected Phthalocyanines

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5552
Author(s):  
Ryota Kudo ◽  
Masahiro Sonobe ◽  
Yoshiaki Chino ◽  
Yu Kitazawa ◽  
Mutsumi Kimura
Keyword(s):  
Lamellar Structure ◽  
Synthesis And Characterization ◽  
Molecular Symmetry ◽  
X Ray Diffraction ◽  
Melting Points ◽  
Scanning Calorimetry ◽  
Structural Isomers ◽  
X Ray ◽  
Temperature Controlled

The synthesis and characterization of two phthalocyanine (Pc) structural isomers, 1 and 2, in which four 2,6-di(hexyloxy)phenyl units were attached directly to the 1,8,15,22- or 1,4,15,18-positions of the Pc rings, are described. Both Pcs 1 and 2 exhibited low melting points, i.e., 120 and 130 °C respectively, due to the reduction in intermolecular π-π interaction among the Pc rings caused by the steric hindrance of 2,6-dihexyloxybenzene units. The thermal behaviors were investigated with temperature-controlled polarizing optical microscopy, differential scanning calorimetry, powder X-ray diffraction, and absorption spectral analyses. Pc 1, having C4h molecular symmetry, organized into a lamellar structure containing lateral assemblies of Pc rings. In contrast, the other Pc 2 revealed the formation of metastable crystalline phases, including disordered stacks of Pcs due to rapid cooling from a melted liquid.

scholarly journals Microstructure Evolution and Performance Improvement of Hypereutectic Al–Mg2Si Metallic Composite with Ca or Sb

Materials ◽  
2020 ◽  
Vol 13 (12) ◽  
pp. 2714
Author(s):  
Min Zuo ◽  
Boda Ren ◽  
Zihan Xia ◽  
Wenwen Ma ◽  
Yidan Lv ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Nucleation Behavior ◽  
X Ray ◽  
Primary Mg2si ◽  
Before And After ◽  
And Performance ◽  
Hardness Values

In this article, the modification effects on Al–Mg2Si before and after heat treatment were investigated with Ca, Sb, and (Ca + Sb). In comparison with single Ca or Sb, the samples with composition modifiers (Ca + Sb) had the optimal microstructure. The sample with a molar ratio for Ca-to-Sb of 1:1 obtained relatively higher properties, for which the Brinell hardness values before and after heat treatment were remarkably increased by 31.74% and 28.93% in comparison with bare alloy. According to differential scanning calorimetry analysis (DSC), it was found that the nucleation behavior of the primary Mg2Si phase could be significantly improved by using chemical modifiers. Some white particles were found to be embedded in the center of Mg2Si phases, which were deduced to be Ca5Sb3 through X-ray diffraction (XRD) and field-emission scanning electron microscope (FESEM) analyses. Furthermore, Ca5Sb3 articles possess a rather low mismatch degree with Mg2Si particles based on Phase Transformation Crystallography Lab software (PTCLab) calculation, meaning that the efficient nucleation capability of Ca5Sb3 for Mg2Si particles could be estimated.

scholarly journals Influence of Molecular Orientation on the Melting Behavior of Poly(phenylene sulfide) Fibers

2013 ◽  
Vol 8 (3) ◽  
pp. 155892501300800
Author(s):  
Prabhakar Gulgunje ◽  
Gajanan Bhat ◽  
Joseph Spruiell
Keyword(s):  
Differential Scanning Calorimetry ◽  
Molecular Orientation ◽  
Polarized Light ◽  
Melting Behavior ◽  
Probable Mechanism ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Phenylene Sulfide

The influence of molecular orientation on the melting behavior of draw-annealed poly(phenylene sulfide) fibers is investigated in the present paper. Tools used to probe the investigation were differential scanning calorimetry, polarized light optical microscopy, wide angle X-ray diffraction, and small angle X-ray diffraction. It is shown that molecular orientation in the crystalline and amorphous regions play a key role in crystal rearrangement during melting. A probable mechanism by which amorphous orientation influences crystal rearrangement is also discussed.

Investigation on β-Polypropylene/Talc Composites

2012 ◽  
Vol 182-183 ◽  
pp. 259-264
Author(s):  
Jia Wei Duan ◽  
Qiang Dou
Keyword(s):  
Polarized Light ◽  
Nucleating Agent ◽  
Mechanical Tests ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Melt Compounding ◽  
Β Phase ◽  
Α Phase ◽  
Melting And Crystallization

In this study polypropylene (PP) composites containing β-nucleating agent (NT-C) and talc filler were prepared by melt compounding. The melting and crystallization behavior, morphology and mechanical properties of the composites were studied by means of differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), polarized light microscopy (PLM) and mechanical tests. The results indicate that talc suppresses the formation of β phase, but promotes the formation of α phase. The Izod notched impact strength and tensile strength of β-PP/talc composites are superior to those of PP/talc composites, indicating an outstanding balance of stiffness and toughness of β-PP/talc composites.

Crystallization Properties of Nucleated Poly(lactic acid)

2012 ◽  
Vol 549 ◽  
pp. 322-326 ◽  
Author(s):  
Yong Chen ◽  
Qiang Dou
Keyword(s):  
Lactic Acid ◽  
Crystallization Behavior ◽  
Polarized Light ◽  
Nucleating Agent ◽  
Poly Lactic Acid ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Crystallization Properties ◽  
Melting And Crystallization

The effect of a nucleating agent (NT-C) on the crystallization behavior of poly(lactic acid) (PLA) was studied. The melting and crystallization behavior and spherulitic morphology of the nucleated PLA were investigated by means of differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD) and polarized light microscopy (PLM). It is found that the crystallization temperature and crystallinity increase, the spherulitic size decrease for the nucleated PLA. But the crystal structure of the nucleated PLA is not changed.

Preparation of γ–Fe2O3 nanoparticles from a nonaqueous precursor

2001 ◽  
Vol 16 (12) ◽  
pp. 3471-3475 ◽  
Author(s):  
P. Deb ◽  
A. Basumallick
Keyword(s):  
Heat Treatment ◽  
Thermal Characteristics ◽  
Homogeneous Solution ◽  
Nanosized Particles ◽  
Narrow Size Distribution ◽  
Fe2o3 Nanoparticles ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
X Ray Scattering

Nanosized particles of γ–Fe2O3 were prepared by heat treatment of the precipitates, obtained from a homogeneous solution of stearic acid and hydrated iron(III) nitrate. The compositional and thermal characteristics of the precipitates were studied with the aid of infrared spectroscopy and differential scanning calorimetry. The x-ray diffraction and small-angle x-ray scattering investigation shows that γ–Fe2O3 nanoparticles with narrow size distribution can be prepared successfully by this route.

scholarly journals Evaluation of Thermal-Induced Polymorphic Transformation on Desloratadine and Desloratadine-Benzoic Acid Salt

2020 ◽  
Vol 26 (4) ◽  
pp. 399-405
Author(s):  
Ahmad Ainurofiq ◽  
Rachmat Mauludin ◽  
Diky Mudhakir ◽  
Sundani Nurono Soewandhi
Keyword(s):  
Melting Point ◽  
Benzoic Acid ◽  
Polymorphic Transformation ◽  
Heating Process ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Physicochemical Changes ◽  
Transformation Methods

Background: Active pharmaceutical ingredients face a challenge in manufacturing due to adverse physicomechanical properties. Desloratadine (DES) form I exhibits poor mechanical behavior through the formation of capping during the tableting process. Salt formation from DES and benzoic acid (BA) has been observed to resolve poor mechanical properties. However, the ability to withstand heat from the manufacturing process should be implemented in DES and DES-BA salt. The aim of this study was to determine the differences between thermal treatment results on DES and DES-BA salt and whether it causes them to undergo polymorphic transformation. Methods: Salt was crystallized between DES and BA using the solvent evaporation method. DES and DES-BA salt were heated at 110°C, 159°C (melting point of DES), 181°C (melting point of DES-BA), and 190°C. Following this, characterization was performed using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and solubility testing. Results: Polymorphic transformation caused by heat occurred in DES, but not in DES-BA salt. The transformation of DES was induced by the effect of heating, which changed polymorph I to a mixture of polymorph I and III at 110°C, to polymorph II at 159°C, and to a mixture of polymorph I, II, and III at 190°C. Under 190oC, DES-BA is still stable and did not undergo a polymorphic transformation. However, at 190oC, decomposition started to occur, which implied decreased solubility, which did not occur in DES. Conclusion: The heating process did not cause DES-BA salt to undergo a polymorphic transformation. However, it caused decomposition at 190oC. DES underwent a polymorphic transformation when exposed to the same condition without decomposition. This provided information to always pay attention to temperature during manufacturing processes that include DES or DES-BA salt to avoid physicochemical changes.

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