Synthesis and characterization of a silylated Brazilian clay mineral surface

2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Márcia Silva ◽  
Saloana Gomes ◽  
Maria Fonseca ◽  
Kaline Sousa ◽  
José Espínola ◽  
...  

AbstractClay mineral containing kaolinite, illite and montmorillonite was organofunctionalized with silylating agents: (3-aminopropyl)triethoxysilane, 3-[2-(2-aminoethylamino)ethylamino]propyl-trimethoxysilane and (3-mercaptopropyl)trimethoxy-silane, to yield three hybrids labelled Clay1, Clay2 and Clay3, respectively. These solids were characterized using elemental analysis, thermogravimetry, X-ray diffractometry, infrared spectroscopy, scanning electron micrograph, and 29Si and 27Al solid state NMR. Immobilized quantities of the organic groups were 0.66 mmol g−1, 0.48 mmol g−1 and 0.88 mmol g−1 for Clayx (x = 1–3), respectively. X-ray diffraction patterns confirmed the immobilization of silanes onto the surface without changes in the textural properties of the clay mineral as noted from the SEM images. Spectroscopic measurements were in agreement with the covalent bonding between the silanes and the hydroxyl groups deposited on the surface. The new hybrids were utilized as adsorbents of cobalt in aqueous solution, with retention values of 0.78 mmol g−1, 1.1 mmol g−1 and 0.70 mmol g−1 for Clayx (x = 1–3), respectively.

2012 ◽  
Vol 18-19 ◽  
pp. 291-297
Author(s):  
Priscila Anadão ◽  
Francisco Rolando Valenzuela-Díaz ◽  
Hélio Wiebeck

Poly(vinyl butyral)-polyaniline-sodium montmorillonite nanocomposites were prepared via polymerization of aniline between clay mineral platelets at two different pH levels (2.0 and 5.0), followed by dispersion of the polyaniline-sodium montmorillonite nanocomposite in a poly(vinyl butyral) solution. A comparison was made of the effect of the pH levels and the polyaniline-sodium montmorillonite nanocomposite precursor on the final structures of the poly(vinyl butyral) nanocomposites and their electrical conductivities. X-ray diffraction patterns revealed the formation of nanocomposites at both pH levels. UV-Vis spectra indicated that the polyaniline formed at both pH levels was conductive, with the UV-Vis spectra presenting a band at 420 nm corresponding to the polaronic form and the beginning of a new band at 600 nm indicating the presence of polaronic segments. FTIR spectra revealed the peaks of the groups present in polyaniline and poly(vinyl butyral) nanocomposites. The electrical conductivities of the polyaniline and poly(vinyl butyral) nanocomposites prepared at pH 2.0 were lower than those of the same nanocomposites prepared at pH 5.0, probably due to the lower formation of polyaniline chains in a more acidic dispersion and to the final configuration of polyaniline in the nanocomposites.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 931
Author(s):  
Ioana-Codruţa Mirică ◽  
Gabriel Furtos ◽  
Ondine Lucaciu ◽  
Petru Pascuta ◽  
Mihaela Vlassa ◽  
...  

The aim of this research was to develop new electrospun membranes (EMs) based on polycaprolactone (PCL) with or without metronidazole (MET)/nano-hydroxyapatite (nHAP) content. New nHAP with a mean diameter of 34 nm in length was synthesized. X-ray diffraction (XRD) and attenuated total reflectance Fourier transform infrared spectroscopy (FTIR-ATR) were used for structural characterization of precursors and EMs. The highest mechanical properties (the force at maximum load, Young’s modulus and tensile strength) were found for the PCL membranes, and these properties decreased for the other samples in the following order: 95% PCL + 5% nHAP > 80% PCL + 20% MET > 75% PCL + 5% nHAP + 20% MET. The stiffness increased with the addition of 5 wt.% nHAP. The SEM images of EMs showed randomly oriented bead-free fibers that generated a porous structure with interconnected macropores. The fiber diameter showed values between 2 and 16 µm. The fiber diameter increased with the addition of nHAP filler and decreased when MET was added. New EMs with nHAP and MET could be promising materials for guided bone regeneration or tissue engineering.


2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material


1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes

Author(s):  
Fikri Alatas ◽  
Fahmi Abdul Azizsidiq ◽  
Titta Hartyana Sutarna ◽  
Hestyari Ratih ◽  
Sundani Nurono Soewandhi

An effort to improve the solubility of albendazole (ABZ), an anthelmintic drug has been successfully carried out through the formation of multicomponent crystal with dl-malic acid (MAL). Construction of phase solubility curve of ABZ in MAL solution and crystal morphological observations after recrystallization in the acetone-ethanol (9:1) mixture were performed for initial prediction of multicomponent crystal formation. ABZ-MAL multicomponent crystal was prepared by wet grinding or also known as solvent-drop grinding (SDG) with acetone-ethanol (9:1) mixture as a solvent followed by characterization of the multicomponent crystal formation by powder X-ray diffraction and Fourier transform infrared (FTIR) methods. The solubility of ABZ-MAL multicomponent crystal was tested in water at ambient temperature and in pH 1.2, 4.5 and 6.8 of buffered solutions at 37°C. The phase solubility curve of the ABZ in the MAL solution showed type Bs. The ABZ-MAL mixture has a different crystalline morphology than pure ABZ and MAL after recrystallization in the acetone-ethanol mixture (9:1). The powder X-ray diffraction pattern and the FTIR spectrum of ABZ-MAL from SDG different from intact ABZ and MAL powder X-ray diffraction patterns and these results can indicate the ABZ-MAL multicomponent crystal formation. The ABZ-MAL multicomponent crystal has better solubility than pure ABZ in all media used. These results can be concluded that ABZ-MAL multicomponent crystal can be prepared by solvent-drop grinding method with acetone-ethanol (9:1) mixture as a solvent and can increase the solubility of albendazole.


2005 ◽  
Vol 03 (2) ◽  
pp. 24-29
Author(s):  
P.M. PIMENTEL ◽  
A.M.G. PEDROSA ◽  
H.K.S. SOUZA ◽  
C.N.S. JÚNIOR ◽  
R.C.A. PINTO ◽  
...  

Spinel oxides with the composition ZnCo2O4 and ZnCo2O4:Eu3+ have been synthesized by the Pechini method and characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures. The formation of monophase cubic spinel structure was confirmed by X-ray diffraction patterns. Extra lines corresponding to other phase has been observed in the powders calcined at 900 ºC. The results showed the extremely lower synthesis temperature than those presents in conventional methods.


2004 ◽  
Vol 831 ◽  
Author(s):  
Phanikumar Konkapaka ◽  
Huaqiang Wu ◽  
Yuri Makarov ◽  
Michael G. Spencer

ABSTRACTBulk GaN crystals of dimensions 8.5 mm × 8.5 mm were grown at growth rates greater than 200μm/hr using Gallium Vapor Transport technique. GaN powder and Ammonia were used as the precursors for growing bulk GaN. Nitrogen is used as the carrier gas to transport the Ga vapor that was obtained from the decomposition of GaN powder. During the process, the source GaN powder was kept at 1155°C and the seed at 1180°C. Using this process, it was possible to achieve growth rates of above 200 microns/hr. The GaN layers thus obtained were characterized using X-Ray diffraction [XRD], scanning electron microscopy [SEM], and atomic force microscopy [AFM]. X-ray diffraction patterns showed that the grown GaN layers are single crystals oriented along c direction. AFM studies indicated that the dominant growth mode was dislocation mediated spiral growth. Electrical and Optical characterization were also performed on these samples. Hall mobility measurements indicated a mobility of 550 cm2/V.s and a carrier concentration of 6.67 × 1018/cm3


2021 ◽  
Vol 12 (4) ◽  
pp. 2523-2529
Author(s):  
Daniel Sam N ◽  
Anish C I ◽  
Sabeena G ◽  
Rajaduraipandian S ◽  
Manobala ◽  
...  

Sol gel methods were used for the study of the antimicrobial activity of Cd-TiO2 against gram-negative and positive bacteria. These Cd-TiO2 have been characterized by various optical and techniques. They have been exhibited by X-ray diffraction, scanning electron microscopy, ultraviolet spectroscopy, and infrared spectroscopy. The structures of the various XRD patterns indicate that the product has a structure. The particle size of Cd-TiO2 is 35nm. The SEM images confirm the spherical appearance of the sample. The energy X-ray spectra have been confirmed as well and then C, O, Ti, Cd, Pt element are present in Cd-TiO2. The weight percentage of Cadmium is 5.8%, Ti is 51.03%, C is 5.13% and O is 31.75% in Cd-TiO2. BET image shows that the major pore size distribution of Cd-TiO2 is ranged from 2.24 nm. The Cd-TiO2 that the antibacterial activity when tested against the pathogens only gram-negative bacteria such as Pseudomonas. The zone of minimum inhibition concentration was measured in a range of 20mm in 25μl and 30mm in 100μl.


2021 ◽  
Vol 1039 ◽  
pp. 307-312
Author(s):  
Mohammad Malik Abood ◽  
Osama Abdul Azeez Dakhil ◽  
Aref Saleh Baron

Methyl ammonium lead iodide CH3NH3PbI3 Perovskite was synthesized by a new method mixing between one and two steps, in addition, the ethanol solvent was used to dissolve CH3NH3I and compared with isopropanol solvent. The characterizations of synthesized perovskite samples included the structural properties, morphological characteristics and optical properties. The intensity and orientation in X-ray diffraction patterns appear clearly in ethanol solvent while disappearing at a peak at 12o due to the speed reaction of perovskite in this solvent. Additionally, the ethanol solvent increasing the grain size of perovskite which homogeneity of the surface morphology. the ethanol solvent cause a decrease in the wavelength of absorbance edge in addition to an increase in the energy bandgap value. Keywords: Ethanol Solvent, Perovskite, Photovoltaic Technologies, X-ray diffraction.


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