Structural and mechanical characterization of polyurethane-CaCO3 composites synthesized at high calcium carbonate loading: An experimental and theoretical study

2021 ◽  
pp. 002199832199641
Author(s):  
Ana P de Moura ◽  
Enio HP da Silva ◽  
Vanessa S dos Santos ◽  
Miguel F Galera ◽  
Flaminio CP Sales ◽  
...  

Due to its exceptional biocompatibility, Polyurethane (PU) reinforced with calcium carbonate (CaCO3) is a composite material with significant biomedical applications. However, much of the currently known mechanical and chemical information regarding composites has been obtained at low and moderate CaCO3 content levels. This study employs experimental and theoretical tools to evaluate the structural, morphological, and mechanical properties of pristine polyurethane, and when doped with CaCO3 at 25 and 50 wt.%. In the experiments the samples are characterized using X-ray diffraction (XRD), infrared spectrophotometry (FT-IR), scanning electron microscopy (SEM), and tensile and flexural mechanical tests, while theoretical calculations are performed to evaluate the carbonate-polymer interaction. The XRD and FT-IR results indicate that CaCO3 is at the calcite phase and that PU-CaCO3 materials exhibit a broadening of bands related to the NH2 group. This result is explained using theoretical calculations that demonstrate a weak interaction between those molecules with the CaCO3 surface, where the molecule-calcite interaction occurs primarily through the NH2 molecular link. With respect to mechanical behaviour, the results show less fracture resistance and greater stiffness for the materials containing CaCO3, compared to those containing only PU. These results are explained in terms of the stress concentration due to CaCO3 within the polymer. Finally, the results detailed in this paper show that a high calcium carbonate loading is suitable for increasing the rigidity and decreasing the fracture toughness of the biomaterial, in association with a reduction of the plastic region.

2016 ◽  
Vol 675-676 ◽  
pp. 209-212 ◽  
Author(s):  
Wichian Siriprom ◽  
Nirun Witit-Anun ◽  
Auttapol Choeysuppaket ◽  
T. Ratana

In this study were to explore the properties of interaction between cellulose and calcium carbonate particle (CaCO3) which derive from Papia Undulates Shell in procedure of biocomposite synthesis. The structural properties of cellulose powder Papia Undulates Shell and cellulose-calcium carbonate composite film were investigated by using X-ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) and the compositions of cellulose/CaCO3 biocomposite film were studied by Energy Dispersive X-ray Fluorescence (EDXRF). The experimental results demonstrated the morphology of Papia Undulates Shell were crystalline aragonite phase and the cellulose have structural as amorphous-crystalline but after film forming the composite film between cellulose and Papia Undulates Shell also have amorphous structural. The result of FTIR used to confirmed the formation of bonding between molecular, it indicated that the cellulose/CacO3 biocomposite film had good biocompatibility due to the biocomposite film have both characteristic feature of CO3-2 group (~874 cm-1 and ~713 cm-1) and the glucose of cellulose at ~1635, ~1064 and ~946 cm-1. Another that, the result from EDXRF shown the chemical composition of organic compound of cellulose/CaCO3 biocomposite film was highest with 99.437 while the Papia Undulates Shell have 0.341 Wt% with corresponding with the ratio of filler material which mixture as 1%. So that, the cellulose/calcium carbonate bicomposite film could be candidate for biocomposite film application.


2010 ◽  
Vol 658 ◽  
pp. 49-52 ◽  
Author(s):  
Wen Kun Zhu ◽  
Xue Gang Luo ◽  
An Kai Luo ◽  
Xuan Liang

Calcium carbonate with various structures and morphologies were prepared under double injection of the CaCl2 and Na2CO3 solutions with molar ratio of 1:1 at 30 °C, taking lignin as the induction agents. They were characterized by scanning electron microscopy, infrared spectroscopy thermal analysis and X-ray diffraction. The synthesis mechanism was also discussed. The results showed that calcium carbonate of different shape were obtained with the concentration of lignin at 10g/L, 20g/L and 30g/L, respectively, under 30°C while CaCl2 and Na2CO3 were kept at the same concentration of 0.5mol/L. The size of the particles was in a range between 3 and 5μm and the particles were calcites. Compared with the normal calcium carbonate, the compound has advanced thermal decomposition behavior. Fourier transform infrared spectroscopy (FT-IR) analysis revealed the presence of lignin and calcite. The electrostatic interaction of Ca2+ with lignin and the complementary of stereo-structure play important roles in the formation of Dumbbell Shaped Calcium Carbonate.


Molbank ◽  
10.3390/m1179 ◽  
2021 ◽  
Vol 2021 (1) ◽  
pp. M1179
Author(s):  
Eleftherios Halevas ◽  
Antonios Hatzidimitriou ◽  
Barbara Mavroidi ◽  
Marina Sagnou ◽  
Maria Pelecanou ◽  
...  

A novel Cu(II) complex based on the Schiff base obtained by the condensation of ortho-vanillin with gamma-aminobutyric acid was synthesized. The compounds are physico-chemically characterized by elemental analysis, HR-ESI-MS, FT-IR, and UV-Vis. The complex and the Schiff base ligand are further structurally identified by single crystal X-ray diffraction and 1H and 13C-NMR, respectively. The results suggest that the Schiff base are synthesized in excellent yield under mild reaction conditions in the presence of glacial acetic acid and the crystal structure of its Cu(II) complex reflects an one-dimensional polymeric compound. The molecular structure of the complex consists of a Cu(II) ion bound to two singly deprotonated Schiff base bridging ligands that form a CuN2O4 chelation environment, and a coordination sphere with a disordered octahedral geometry.


2018 ◽  
Vol 91 (3) ◽  
pp. 389-396 ◽  
Author(s):  
Yanshan Yin ◽  
Jie Yin ◽  
Wei Zhang ◽  
Hong Tian ◽  
Zhangmao Hu ◽  
...  

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.


1996 ◽  
Vol 459 ◽  
Author(s):  
E. Ching-Prado ◽  
W. Pérez ◽  
A. Reynés-Figueroa ◽  
R. S. Katiyar ◽  
D. Ravichandran ◽  
...  

ABSTRACTThin films of SrBi2Nb2O9 (SBN) with thicknesses of 0.1, 0.2, and 0.4 μ were grown by Sol-gel technique on silicon, and annealed at 650°C. The SBN films were investigated by Raman scatering for the first time. Raman spectra in some of the samples present bands around 60, 167, 196, 222, 302, 451, 560, 771, 837, and 863 cm−1, which correspond to the SBN formation. The study indicates that the films are inhomogeneous, and only in samples with thicknesses 0.4 μ the SBN material was found in some places. The prominent Raman band around 870 cm−1, which is the A1g mode of the orthorhombic symmetry, is assigned to the symmetric stretching of the NbO6 octahedrals. The frequency of this band is found to shift in different places in the same sample, as well as from sample to sample. The frequency shifts and the width of the Raman bands are discussed in term of ions in non-equilibrium positions. FT-IR spectra reveal a sharp peak at 1260 cm−1, and two broad bands around 995 and 772 cm−1. The bandwidths of the latter two bands are believed to be associated with the presence of a high degree of defects in the films. The experimental results of the SBN films are compared with those obtained in SBT (T=Ta) films. X-ray diffraction and SEM techniques are also used for the structural characterization.


Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 774
Author(s):  
Eleonora Sočo ◽  
Dorota Papciak ◽  
Magdalena M. Michel ◽  
Dariusz Pająk ◽  
Andżelika Domoń ◽  
...  

(1) Hydroxyapatite (Hap), which can be obtained by several methods, is known to be a good adsorbent. Coal fly ash (CFA) is a commonly reused byproduct also used in environmental applications as an adsorbent. We sought to answer the following question: Can CFA be included in the method of Hap wet synthesis to produce a composite capable of adsorbing both heavy metals and dyes? (2) High calcium lignite CFA from the thermal power plant in Bełchatów (Poland) was used as the base to prepare CFA–Hap composites. Four types designated CFA–Hap1–4 were synthesized via the wet method of in situ precipitation. The synthesis conditions differed in terms of the calcium reactants used, pH, and temperature. We also investigated the equilibrium adsorption of Cu(II) and rhodamine B (RB) on CFA–Hap1–4. The data were fitted using the Langmuir, Freundlich, and Redlich–Peterson models and validated using R2 and χ2/DoF. Surface changes in CFA–Hap2 following Cu(II) and RB adsorption were assessed using SEM, SE, and FT-IR analysis. (3) The obtained composites contained hydroxyapatite (Ca/P 1.67) and aluminosilicates. The mode of Cu(II) and RB adsorption could be explained by the Redlich–Peterson model. The CFA–Hap2 obtained using CFA, Ca(NO3)2, and (NH4)2HPO4 at RT and pH 11 exhibited the highest maximal adsorption capacity: 73.6 mg Cu/g and 87.0 mg RB/g. (4) The clear advantage of chemisorption over physisorption was indicated by the Cu(II)–CFA–Hap system. The RB molecules present in the form of uncharged lactone were favorably adsorbed even on strongly deprotonated CFA–Hap surfaces.


2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.


2012 ◽  
Vol 560-561 ◽  
pp. 434-437 ◽  
Author(s):  
Lan Wang ◽  
Wen Ji Guo ◽  
Yan Zhao Zhao

The objective of this paper was to prepare the composite of crefradine/montmorillionite in the method of solution intercalation. The drug load and intercalation rate varied with the drug concentration. X-ray diffraction (XRD), Fourier transformed infrared (FT-IR) Spectroscopy, and thermal analysis (TG-DSC) were applied to characterize composite mentioned above. Together with drug release tests, results indicate cefradine intercalated into montmorillionite.The release profiles of cefradine/MMT in simulated gastric fluid (pH 1.2) and simulated intestinal fluid (pH 7.4) at 37°Cduring 10h are shown in Fig. 4. The amount of cefradine in the beginning 2h came up to 35% and 50%, and in the following time, cefradine released slowly. The release behaviors met the requirements of sustained release.


2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Michael B. Toffolo ◽  
Giulia Ricci ◽  
Luisa Caneve ◽  
Ifat Kaplan-Ashiri

Abstract In nature, calcium carbonate (CaCO3) in the form of calcite and aragonite nucleates through different pathways including geogenic and biogenic processes. It may also occur as pyrogenic lime plaster and laboratory-precipitated crystals. All of these formation processes are conducive to different degrees of local structural order in CaCO3 crystals, with the pyrogenic and precipitated forms being the least ordered. These variations affect the manner in which crystals interact with electromagnetic radiation, and thus formation processes may be tracked using methods such as X-ray diffraction and infrared spectroscopy. Here we show that defects in the crystal structure of CaCO3 may be detected by looking at the luminescence of crystals. Using cathodoluminescence by scanning electron microscopy (SEM-CL) and laser-induced fluorescence (LIF), it is possible to discern different polymorphs and their mechanism of formation. We were thus able to determine that pyrogenic calcite and aragonite exhibit blue luminescence due to the incorporation of distortions in the crystal lattice caused by heat and rapid precipitation, in agreement with infrared spectroscopy assessments of local structural order. These results provide the first detailed reference database of SEM-CL and LIF spectra of CaCO3 standards, and find application in the characterization of optical, archaeological and construction materials.


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