Characterization of Polystyrene (PS)/Organomodified Layered Double Hydroxide (OLDH) Nanocomposites Prepared by In Situ Polymerization

2011 ◽  
Vol 410 ◽  
pp. 164-167 ◽  
Author(s):  
Balakrushna Sahu ◽  
G. Pugazhenthi

PS/LDH nanocomposites were synthesized via in-situ polymerization technique using styrene monomer with toluene as a solvent. A series of LDHs (Mg-Al, Co-Al, Ni-Al, Cu-Al, Cu-Fe and Cu-Cr LDHs) was first prepared from their nitrate salts by co-precipitation method. The above prepared, pristine LDHs were organically modified using sodium dodecyl sulfate (SDS) to obtain organomodified LDHs (OLDH). Then, PS nanocomposites containing 5 wt.% OLDHs were prepared by in-situ polymerization method. The structural and thermal properties of LDHs and corresponding nanocomposites were characterized by X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA). The absence of OLDH peak (003) in the XRD patterns of PS/OLDH nanocomposite confirms the formation of exfoliated nanocomposites. The presence of sulfate groups in the modified LDHs is confirmed by FTIR analysis. The appearance of new peaks in the FTIR spectra in the region of 3400-3500 cm-1, 1670-1680 cm-1and 1200-1260 cm-1for O-H stretching, H-O-H vibration and stretching vibration of sulfate, respectively indicate the existence of LDHs in the PS/OLDH nanocomposites. The entire exfoliated PS/OLDH nanocomposites exhibit enhanced thermal stability relative to the pure PS. When 50% weight loss is selected as point of comparison, the decomposition temperature of nanocomposites is about 3-5oC higher than that of pure PS.

MRS Advances ◽  
2017 ◽  
Vol 2 (64) ◽  
pp. 4025-4030 ◽  
Author(s):  
T. Kryshtab ◽  
H. A. Calderon ◽  
A. Kryvko

ABSTRACTThe microstructure of Ni-Mg-Al mixed oxides obtained by thermal decomposition of hydrotalcite-like compounds synthesized by a co-precipitation method has been studied by using X-ray diffraction (XRD) and atomic resolution transmission electron microscopy (TEM). XRD patterns revealed the formation of NixMg1-xO (x=0÷1), α-Al2O3 and traces of MgAl2O4 and NiAl2O4 phases. The peaks profile analysis indicated a small grain size, microdeformations and partial overlapping of peaks due to phases with different, but similar interplanar spacings. The microdeformations point out the presence of dislocations and the peaks shift associated with the presence of excess vacancies. The use of atomic resolution TEM made it possible to identify the phases, directly observe dislocations and demonstrate the vacancies excess. Atomic resolution TEM is achieved by applying an Exit Wave Reconstruction procedure with 40 low dose images taken at different defocus. The current results suggest that vacancies of metals are predominant in MgO (NiO) crystals and that vacancies of Oxygen are predominant in Al2O3 crystals.


2012 ◽  
Vol 557-559 ◽  
pp. 371-374
Author(s):  
Lian Liu ◽  
Teng Yu ◽  
Pei Wang ◽  
Guang Shuo Wang

Nanocomposites of poly(ε-caprolactone) (PCL) and layered double hydroxide (LDH) were prepared by in situ polymerization at low LDHs loadings in this work. The resultants were characterized by FTIR spectroscopy, X-ray diffraction (XRD), differential scanning calorimeter (DSC) and UV-visible spectroscopy (UV-vis). FTIR showed that the PCL/LDHs nanocomposites were prepared successfully by in situ polymerization and XRD spectra showed that the crystal structure did not change greatly in the presence of LDHS. DSC results confirmed that LDHs could act as nucleating agents. UV-vis spectra showed that LDHs had stronger absorbance peak than LDH. Moreover, the PCL/LDHs nanocomposites had strong anti-ultraviolet effect by introduction of LDHs into polymer matrix.


2005 ◽  
Vol 284-286 ◽  
pp. 701-704 ◽  
Author(s):  
S.A. Costa ◽  
J. Miguel Oliveira ◽  
Isabel B. Leonor ◽  
Rui L. Reis

In this study, it is shown that it is possible to prepare carboxymethyl-chitosan/Ca-P hybrids using an innovative “auto-catalytic” co-precipitation method, namely by using an acid and an oxidant bath. The X-ray diffraction (XRD) patterns evidenced the formation of crystalline calcium-phosphate precipitates when using an acid bath, while amorphous ones were obtained for those produced in the oxidant bath. The Fourier Transform Infrared spectroscopy (FTIR) and Scanning Electron Microscopy (SEM/EDS) studies revealed that the extent of the polymer precipitation and formation of calcium-phosphates is directly dependent on the pH and composition of the baths. Furthermore, by conducting bioactivity tests in a simulated body fluid (SBF) followed by the SEM/EDS analysis it was possible to detect the formation of an apatite layer with a cauliflower-like morphology on the surface of hybrids prepared by the acid bath, after 7 days of immersion. These results are quite promising because they can allow for the production of bioactive and biodegradable 3D porous scaffolds to be used in bone tissue engineering applications.


2019 ◽  
Vol 32 (1) ◽  
pp. 49-52
Author(s):  
M. Jaganadha Rao ◽  
K.S.R. Murthy ◽  
Ch. Ravi Shankar Kumar ◽  
Anjali Jha ◽  
G.S.V.R.K. Choudary ◽  
...  

Present day technology requires synthesis of materials with low energy consumption, free mercury pollution and its reliability. A novel material with control of crystallite size, composition and simple for white light relies in synthesis of materials. The present focus of article attributes series of manganese doped Ca1-xMnxWO4 luminescent materials with co-precipitation method. Reported studies attempts with change in structure of calcium tungstate (CaWO4) are observed with dopants like Eu3+, Eu2+, Tb3+, etc. However the effect of Mn2+ on structural properties of CaWO4 are quite interesting. The synthesized samples were characterized with X-ray diffraction for lattice parameters, crystallite size and FTIR studies for bonding mechanism of O-W-O stretching and W-O-W bridge bond. Rietveld profile refinement of XRD patterns using MAUD program Ca1-xMnxWO4 revealed the Scheelite type structure with C4h point group and I41/a space group. Characterization studies reveal that doping of Mn2+ doping upto 0.1 in place of Ca2+ will not change the phase of Scheelite structure.


Catalysts ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 70 ◽  
Author(s):  
Eliana Nope ◽  
Ángel G. Sathicq ◽  
José J. Martínez ◽  
Hugo A. Rojas ◽  
Rafael Luque ◽  
...  

Lamellar double hydroxides (LDH) with double divalent cations were synthesized by the co-precipitation method and studied in the multicomponent synthesis of 4H-pyrans. The solids obtained were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR), N2 adsorption isotherms, and thermogravimetric analysis (TGA). The XRD patterns confirmed the formation of LDHs in which the incorporation of Ni2+ or Co2+ improves their crystalline and textural properties. The results of catalytic activity showed that the synthesis of 4H-pyrans is favored in solvent-free conditions with the LDH–Ni catalyst, avoiding calcination processes. In addition, it was found that hydrotalcite with double divalent cations can conduct this reaction through multicomponent synthesis or by the Michael addition reaction, which can be performed by different types of basicity that depend on the composition of another divalent cation in the brucite layer or a calcination process.


2018 ◽  
Vol 27 (6) ◽  
pp. 1655-1660 ◽  
Author(s):  
Na Zhang ◽  
Xiaoyu Zhang ◽  
Erbo Shi ◽  
Shiyong Zhao ◽  
Kezhu Jiang ◽  
...  

2020 ◽  
Vol 829 ◽  
pp. 154536 ◽  
Author(s):  
Chengxiang Huang ◽  
Chenghao Ni ◽  
Lingze Yang ◽  
Tiantian Zhou ◽  
Chen Hao ◽  
...  

Author(s):  
Chinh

CuxMg1.xFe2O4 nanoparticles were successfully synthesized by co-precipitation. The samples were calcined at 900 oC for 3 h and X-ray diffraction analysis showed that Cu0.5Mg0.5Fe2O4 had a single phase cubic spinel structure, while formation of secondary phase of Fe2O3 was observed in XRD patterns of CuFe2O4, MgFe2O4. The saturation magnetization (Ms) of Cu0.5Mg0.5Fe2O4 is in between the saturation magnetization values of CuFe2O4 and MgFe2O4 nanoparticles, CuFe2O4 is a ferromagnetic material, while MgFe2O4 and Cu0.5Mg0.5Fe2O4 show superparamagnetic behavior. The synthesized spinel ferrites were fully characterized using scanning electron microscopy (SEM), FTIR spectroscopy, energy dispersive spectroscopy (EDS) and UV-vis spectrophotometry.


Author(s):  
Ali A. Ati ◽  
Zulkafli Othaman ◽  
Shadab Dabagh ◽  
R. M. Rosnan ◽  
Samad Zare

Nano crystalline powders of Co-Ni ferrite compounds having the chemical formula Co(x)Ni(1-x) Fe2O4( x = 0.0, 0.2 and 1.0) have been successfully synthesized by co-precipitation technique. These synthesized compounds are characterized by X-ray diffraction (XRD), field emission scan electron microscopy (FESEM), fourier transformed infrared (FTIR) spectrum, energy dispersive X-ray diffraction (EDX) and TGA-DTA. The XRD analyses of the samples sintered at 600 °C clearly show the formation of single cubic spinel structure. XRD patterns are further analyzed to calculate the lattice constant and jump length of charge carriers. Average crystalline sizes for ferrite powders are determined from XRD line using Debye-Scherrer's formula is found to be in the range of 16 to 19 nm with narrow size distribution. The Fourier transformed infrared (FTIR) spectrum characterization of the  spinel ferrite structure sintered at 600 °C shows two fundamental strong band in the range 385-600 cm-1, which is attributed to different main metal-oxygen bands.


Author(s):  
B. Suryanarayana ◽  
V. Raghavendra ◽  
K. Chandra Mouli

Nickel zinc nanoparticles NixZn1-xFe2O4 (where x= 0.2, 0.4, 0.5, 0.6 and 0.8) by Chemical Co-Precipitation method. The samples were characterised by X-ray diffraction (XRD), TEM, VSM .The powders of XRD patterns confirm a single spinel crystalline phase with cubic structure formation with no indication of any other secondary or unidentified phase. The lattice parameter changed from 8.336 Å to 8.382 Å. The average particle size ranged 20 to 80 nm was observed by TEM.


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