Iron substitution in aluminosilicate sols synthesized at low pH

Clay Minerals ◽  
1984 ◽  
Vol 19 (1) ◽  
pp. 1-8 ◽  
Author(s):  
M. B. McBride ◽  
V. C. Farmer ◽  
J. D. Russell ◽  
J. M. Tait ◽  
B. A. Goodman

AbstractThe procedure for synthesizing proto-imogolite (an acid-soluble hydroxy-aluminium orthosilicate complex) and imogolite (a tubular aluminosilicate mineral) was used to produce ferruginous aluminosilicates over a range of Al/Fe ratios to determine whether Fe3+ can be incorporated in the imogolite structure. Analysis of the synthesized products by transmission electron microscopy, electron diffraction, and IR spectroscopy indicated that, while imogolite was formed in the presence of iron, increased Fe3+ in the systems caused the formation of ferrihydrite and poorly-organized aluminosilicates resembling proto-imogolite allophane. Treatment of these materials with Na-citrate/dithionite/bicarbonate dissolved the ferrihydrite and poorly-organized aluminosilicate, and concentrated products with tubular morphology. Analysis of the structural Fe3+ by ESR spectroscopy suggested that little or no Fe3+ was incorporated in the structure of imogolite, although the less crystalline proto-imogolite allophane may have accommodated some structural Fe3+. A separate iron-rich product, identified as ferrihydrite, was formed at low Al/Fe ratios. Mössbauer spectroscopic analysis of 57Fe3+ doped at very low levels into proto-imogolite and imogolite indicated that the sites of substitution were better defined in the latter. At least part of this Fe3+ may have been incorporated in the structure of boehmite, an impurity formed during synthesis.

2020 ◽  
Vol 869 ◽  
pp. 28-39
Author(s):  
Danila Bakhtin ◽  
Leonid Kulikov ◽  
Alexander Malakhov ◽  
Stepan D. Bazhenov

Samples of nanoscale nano-PAF-10 and nano-PAF-24 porous aromatic framework-like polymeric materials were synthesized using the Suzuki reaction in a microemulsion. Monomers were tetrakis-(p-bromophenyl)methane and 1,4-phenylenediboronic acid. The main idea of the approach is to use 1,4-phenylenediboronic acid not only as a direct participant in the reaction, but also as a surfactant, which allows to stabilize the drops of the emulsion. Using this procedure, samples of PAF-like polymers were synthesized from the mixture, containing the mixture of tetrakis(p-bromophenyl)methane and 1,4-phenylenediboronic acid in ratio from 1:2 to 1:6; the reaction was conducted from 10 to 24 hours. The resulting materials were characterized by IR spectroscopy, NMR spectroscop. To estimate the particle size of the obtained materials, transmission electron microscopy was used. The object of the study were polymers, that were synthesized in 10-hour and 24-hour reactions. The particle size in the first material was in the range of 3-10 nm, in the second - from 30 to 100 nm.


2011 ◽  
Vol 239-242 ◽  
pp. 2839-2842
Author(s):  
Hong Mei Mu ◽  
Peng Fei ◽  
Bi Tao Su ◽  
Zi Qiang Lei

A series of Fe3+-dopped polyaniline (Fe3+/PANI) nanomaterials with different morphologies and a higher conductivity were successfully synthesized using a simple and static interfacial polymerization by using FeCl3 as both oxidant catalyst and dopant. The effect of surfactants CTAB and SDS and the concentration of FeCl3 on the morphology and conductivity of Fe3+/PANI nanomaterial were investigated. The samples were characterized by Transmission Electron Microscopy (TEM), SDY-4 probes conductivity meter, X-ray Diffractometry (XRD), Energy dispersive spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy techniques. TEM’s results showed that their morphologies changed with the type of the surfactant and the concentration of FeCl3. Introducing surfactants CTAB and SDS into Fe3+/PANI remarkably improved the conductivity of the material. The conductivities of CTAB/Fe3+/PANI and SDS /Fe3+/PANI nanomaterials were respectively about 4.8×10-2 and 1.3×10-2 S/cm while the conductivity of Fe3+/PANI was found to be 1.5×10-4 S/cm. The different morphology and high conductivity may be ascribed to the mutual effects of the surfactant and oxidant.


2021 ◽  
Vol 12 (2-2021) ◽  
pp. 207-213
Author(s):  
R. V. Saprykin ◽  
◽  
S. A. Semenov ◽  

Nickel (II) and cobalt (II) salts were synthesized with saturated monocarboxylic acids: butyric, valeric, nylon,enanthic, and caprylic. The obtained compounds were characterized by elemental analysis, IR spectroscopy,and differential scanning calorimetry. As a result of thermolysis of the synthesized carboxylates, nanocomposites were obtained, which were studied by scanning and transmission electron microscopy, elemental analysis, IR spectroscopy, energy dispersive X-ray spectroscopy, and X-ray phase analysis. The magnetic properties of the obtained nanocomposites have been studied.


Author(s):  
G. G. Shaw

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.


Author(s):  
R. W. Anderson ◽  
D. L. Senecal

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.


Author(s):  
S. Fujishiro

The mechanical properties of three titanium alloys (Ti-7Mo-3Al, Ti-7Mo- 3Cu and Ti-7Mo-3Ta) were evaluated as function of: 1) Solutionizing in the beta field and aging, 2) Thermal Mechanical Processing in the beta field and aging, 3) Solutionizing in the alpha + beta field and aging. The samples were isothermally aged in the temperature range 300° to 700*C for 4 to 24 hours, followed by a water quench. Transmission electron microscopy and X-ray method were used to identify the phase formed. All three alloys solutionized at 1050°C (beta field) transformed to martensitic alpha (alpha prime) upon being water quenched. Despite this heavily strained alpha prime, which is characterized by microtwins the tensile strength of the as-quenched alloys is relatively low and the elongation is as high as 30%.


Sign in / Sign up

Export Citation Format

Share Document