Preparation and characterization of poly(2-hydroxyethyl methacrylate)/ Na-montmorillonite intercalated nanocomposites

2013 ◽  
Vol 33 (1) ◽  
pp. 27-32 ◽  
Author(s):  
Zafer Koç ◽  
Meltem Çelik ◽  
Müşerref Önal ◽  
Yüksel Sarıkaya ◽  
Yesim Mogulkoc

Abstract A series of intercalated nanocomposites were prepared via in situ polymerization of 2-hydroxyethyl methacrylate (HEMA) between the interlayer spacing of hydrous Na-montmorillonite (Na-MMT) using benzoyl peroxide (Bz2O2) as a radical initiator. X-ray diffraction patterns showed the absence of any intercalation up to 61.7 mass% of HEMA, but anhydrous Na-MMT formed by the hydrophilic effect of HEMA. The interlayer spacing (d001) values of hydrous and anhydrous Na-MMT were calculated as 1.19 and 1.03 nm, respectively. At higher monomer contents, the increase in the value of d001 from 1.19 to 2.01 nm indicated intercalation of polymer in the interlayer spacing of Na-MMT. Besides, transmission electron microscopy results supported the formation of the intercalated nanocomposites. Thermogravimetric analysis showed that the thermal stability of the nanocomposites increased considerably by intercalation of pure poly-HEMA. Specific surface area and specific nanopore volume of the nanocomposites decreased with the increasing of the monomer content taken by the preparations. The decrease is due to the nonporous nature of the polymer matrix.

Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


2000 ◽  
Vol 15 (7) ◽  
pp. 1617-1621 ◽  
Author(s):  
Jan Schroers ◽  
Konrad Samwer ◽  
Frigyes Szuecs ◽  
William L. Johnson

The reaction of the bulk glass forming alloy Zr41Ti14Cu12Ni10Be23 (Vit 1) with W, Ta, Mo, AlN, Al2O3, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structure and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials.


2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.


e-Polymers ◽  
2013 ◽  
Vol 13 (1) ◽  
Author(s):  
Mohammad Galehassadi ◽  
Fatemeh Hosseinzadeh ◽  
Mehrdad Mahkam

Abstract Nanocomposites of polystyrene (PS) was prepared with new styrenic ionic liquid, N-(4-vinyl benzyl)-(N,N-dimethylamino) pyridinium chloride[VBMAP], surfactants used as organic modifications for the clays. Sodium montmorillonite (Na-MMT) was successfully modified by [VBMAP] to become OMMT through cation exchange technique which is shown by the increase of basalspacing of clay by XRD. The composite material based on polystyrene and organo-modified montmorillonite (OMMT) was prepared by insitu polymerization and characterized. The morphology of the polymer/clay hybrids was evaluated by X-ray diffraction (XRD) ,transmission electron microscopy (TEM) and scanning electron microscopy (SEM), showing good overall dispersion of the clay. The thermal stability of the polymer/clay nanocomposites were enhanced, as evaluated by thermogravimetric analysis.


2013 ◽  
Vol 753 ◽  
pp. 279-284 ◽  
Author(s):  
Radomír Kužel ◽  
Zdeněk Matěj ◽  
Miloš Janeček

X-ray diffraction (XRD) studies of ECAP (equal-channel angular pressing) materials were performed after annealing and by in-situ measurements in XRD high-temperature chamber for samples prepared by different number of passes and number of revolutions, respectively. Main attention was given to Cu and Cu-Zr samples. Significant dependence on number of passes was found for ECAP samples. In-situ measurements were focused not only on temperature dependence but also on time evolution of the diffraction line profiles. Evaluation in terms of dislocation densities, correlation and crystallite size and its distribution was performed by our own software MSTRUCT developed for total powder diffraction pattern fitting. Abnormal growth of some grains with annealing is well-known for copper and leads to the creation of bimodal microstructure. Therefore a special care must be given to the evaluation and a model of two Cu components (larger and smaller crystallites) was fitted to the data if an indication of some crystallite growth appears either in the XRD line profile shape or in two-dimensional diffraction patterns.


2001 ◽  
Vol 703 ◽  
Author(s):  
Ann M. Viano ◽  
Sanjay R. Mishra

ABSTRACTNanocomposite iron nitride based powders are known to have enhanced magnetic and other physical properties. To further explore their potential for application in various fields, we have performed a systematic study of the iron nitride - alumina and iron nitride - silica systems. Iron nitride powder of composition FexN (2 < x < 4), containing both Fe3N and Fe4N phases, was mechanically milled with Al2O3 or SiO2 powder for 4, 8, 16, 32, and 64 hours at the following compositions; (FexN)0.2(Al2O3)0.8, (FexN)0.6(Al2O3)0.4, (FexN)0.2(SiO2)0.8, and (FexN)0.6(SiO2)0.4. Differential thermal analysis and X-ray diffraction were performed to investigate thermal and structural transitions as a function of milling time. As the milling time is increased, the thermal peak corresponding to Fe4N is diminished, while the one corresponding to Fe3N is enhanced. These transitions are correlated with X-ray diffraction patterns. All XRD peaks broaden as a function of milling time, corresponding to smaller particle size. Transmission electron microscopy also reveals a decrease in particle size as the milling time in increased.


2014 ◽  
Vol 904 ◽  
pp. 7-9
Author(s):  
Xiao Hua Gu ◽  
Xi Wei Zhang ◽  
Bao Yun Xu ◽  
Peng Zeng

In this paper, the diphenyl methane diisocyanate (MDI) was used to modify montmorillonoid (MMT) and got the organic montmorillonite (OMMT), which was used with the monomers of PET by in situ polymerization method to prepare PET/MMT nanocomposition. The OMMT was analyzed by the X ray diffraction (XRD) to test the change of the spacing layer. Dispersion of MMT in the PET/MMT nanocomposites were studied with XRD and SEM and by means of thermogravimetric analyzer (TGA) on the thermal stability of PET/MMT nanocomposites. The results showed that, MDI modified MMT successfully, and the compatibility of MMT and PET was increased .


2012 ◽  
Vol 182-183 ◽  
pp. 249-253
Author(s):  
Jun Qiao ◽  
Jia Wei Shen ◽  
Xiang Hong Huang ◽  
Qian Feng Zhang

PMMA/MMT nanocomposites has been prepared by using methyl methacrylate (MMA), montmorillonite (MMT) and ethanolamine as the raw materials via an in-situ free radical polymerization process. The as-prepared nanocomposites were characterized by Fourier transformation infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The results show that the poly(methyl methacrylate) and inorganic montmorillonite have been effectively combined. The structure and thermal stability of the as-prepared nanocomposites are different from the content of MMT in the nanacomposites.


2006 ◽  
Vol 21 (1) ◽  
pp. 112-118 ◽  
Author(s):  
A. Vadivel Murugan ◽  
Mathieu Quintin ◽  
Marie-Helene Delville ◽  
Guy Campet ◽  
Annamraju Kasi Viswanath ◽  
...  

Here we demonstrate the synthesis of a new type of layered poly(3,4-ethylenedioxy- thiophene) (PEDOT)/MoS2 nanocomposite via flocculation of delaminated MoS2 with subsequent in situ oxidative polymerization of 3,4-ethylenedioxythiophene. The resulting nanocomposite was characterized by Fourier transform infrared spectroscopy, powder x-ray diffraction, x-ray photoelectron spectroscopy, thermal analysis, transmission electron microscopy, and four-probe electrical conductivity measurements with respect to temperature. X-ray diffraction results indicated that the exfoliated MoS2 and PEDOT are restacked to produce a novel nanoscale composite material containing alternate nanoribbons of PEDOT in between MoS2 with a basal distance of ∼1.38 nm. The nanocomposite, which could be used as a cathode material for small power rechargeable lithium batteries, has also been demonstrated by the electrochemical insertion of lithium into the PEDOT/MoS2 nanocomposite, where a significant enhancement in the discharge capacity is observed, compared to that of respective pristine molybdenum disulfide.


2014 ◽  
Vol 1015 ◽  
pp. 688-691 ◽  
Author(s):  
Feng Wang ◽  
Qiang Zhang ◽  
Bai Qing Xiong ◽  
Yong An Zhang ◽  
Hong Wei Liu ◽  
...  

An innovative spray deposition technique has been applied to produce in situ TiB2/Zn-30Al-1Cu composites. The microstructures of the spray-deposited composite were studied using scanning electron microscopy, transmission electron microscope and X-ray diffraction. The results have shown that the TiB2particulates are formed in the microstructure. It was found that the TiB2particles were distributed in Zn-30Al-1Cu matrix uniformly, and the TiB2particles are about 2μm in size.


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