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Title: Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control

Abstract

A phase transition, from orthorhombic Fe{sub 3}C to hexagonal Fe{sub 7}C{sub 3}, was observed using a wet synthesis mediated by hexadecyltrimethylammonium chloride (CTAC). In this study, CTAC has been shown to control carbide phase, morphology, and size of the iron carbide nanostructures. Fe{sub 7}C{sub 3} hexagonal prisms were formed with an average diameter of 960 nm, the thickness of 150 nm, and Fe{sub 3}C nanostructures with an approximate size of 50 nm. Magnetic studies show ferromagnetic behavior with M{sub s} of 126 emu/g, and H{sub c} of 170 Oe with respect to Fe{sub 7}C{sub 3} and 95 emu/g and 590 Oe with respect to Fe{sub 3}C. The thermal studies using high temperature x-ray diffraction show stability of Fe{sub 7}C{sub 3} up to 500 °C. Upon slow cooling, the Fe{sub 7}C{sub 3} phase is recovered with an intermediate oxide phase occurring around 300 °C. This study has demonstrated a simple route in synthesizing iron carbides for an in depth magnetic study and crystal phase transition study of Fe{sub 7}C{sub 3} at elevated temperatures.

Authors:
; ;  [1];  [1];  [2]
  1. Department of Chemistry, Virginia Commonwealth University, Richmond, Virginia 23284 (United States)
  2. (Egypt)
Publication Date:
OSTI Identifier:
22597817
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Applied Physics; Journal Volume: 120; Journal Issue: 3; Other Information: (c) 2016 Author(s); Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSICS; 75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; CONTROL; COOLING; CRYSTAL-PHASE TRANSFORMATIONS; CRYSTALS; IRON CARBIDES; MORPHOLOGY; NANOSTRUCTURES; ORTHORHOMBIC LATTICES; OXIDES; SYNTHESIS; TEMPERATURE RANGE 0400-1000 K; THICKNESS; X-RAY DIFFRACTION

Citation Formats

Williams, Brent, Clifford, Dustin, Carpenter, Everett E., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, El-Gendy, Ahmed A., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, and Nanotechnology and Nanometrology Laboratory, National Institute for Standards, Giza 12211. Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control. United States: N. p., 2016. Web. doi:10.1063/1.4958972.
Williams, Brent, Clifford, Dustin, Carpenter, Everett E., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, El-Gendy, Ahmed A., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, & Nanotechnology and Nanometrology Laboratory, National Institute for Standards, Giza 12211. Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control. United States. doi:10.1063/1.4958972.
Williams, Brent, Clifford, Dustin, Carpenter, Everett E., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, El-Gendy, Ahmed A., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu, and Nanotechnology and Nanometrology Laboratory, National Institute for Standards, Giza 12211. 2016. "Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control". United States. doi:10.1063/1.4958972.
@article{osti_22597817,
title = {Solvothermal synthesis of Fe{sub 7}C{sub 3} and Fe{sub 3}C nanostructures with phase and morphology control},
author = {Williams, Brent and Clifford, Dustin and Carpenter, Everett E., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu and El-Gendy, Ahmed A., E-mail: aelgendy@vcu.edu, E-mail: ecarpenter2@vcu.edu and Nanotechnology and Nanometrology Laboratory, National Institute for Standards, Giza 12211},
abstractNote = {A phase transition, from orthorhombic Fe{sub 3}C to hexagonal Fe{sub 7}C{sub 3}, was observed using a wet synthesis mediated by hexadecyltrimethylammonium chloride (CTAC). In this study, CTAC has been shown to control carbide phase, morphology, and size of the iron carbide nanostructures. Fe{sub 7}C{sub 3} hexagonal prisms were formed with an average diameter of 960 nm, the thickness of 150 nm, and Fe{sub 3}C nanostructures with an approximate size of 50 nm. Magnetic studies show ferromagnetic behavior with M{sub s} of 126 emu/g, and H{sub c} of 170 Oe with respect to Fe{sub 7}C{sub 3} and 95 emu/g and 590 Oe with respect to Fe{sub 3}C. The thermal studies using high temperature x-ray diffraction show stability of Fe{sub 7}C{sub 3} up to 500 °C. Upon slow cooling, the Fe{sub 7}C{sub 3} phase is recovered with an intermediate oxide phase occurring around 300 °C. This study has demonstrated a simple route in synthesizing iron carbides for an in depth magnetic study and crystal phase transition study of Fe{sub 7}C{sub 3} at elevated temperatures.},
doi = {10.1063/1.4958972},
journal = {Journal of Applied Physics},
number = 3,
volume = 120,
place = {United States},
year = 2016,
month = 7
}
  • In this paper, we report a solvothermal synthesis method that allows the crystallization of quartz to occur at a relatively low temperature of 300°C in the form of isolated nanosized euhedral crystals. Transmission electron microscopy (TEM) and small area electron diffraction (SAED) were used to confirm the phases present and their particle sizes, morphologies, and crystallinity of the products. In conclusion, the results show that it is possible to control the size and morphology of the nanoquartz from rough nanospheres to nanorods using fluoride, which templates the nanocrystals and moderates growth.
  • A variety of iron hydroxyl phosphate (NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2}OH.2H{sub 2}O) nanostructures such as solid microspheres, microspheres with the core in the hollow shell, and double-shelled hollow microspheres were synthesized by a simple one-step microwave-solvothermal ionic liquid method. The effects of the experimental parameters on the morphology and crystal phase of the resultant materials were investigated. Structural dependent photoluminescence was observed from the double-shelled hollow microspheres and the underlying mechanisms were discussed. - Graphical abstract: A variety of iron hydroxyl phosphate (NH{sub 4}Fe{sub 2}(PO{sub 4}){sub 2}OH.2H{sub 2}O) nanostructures were synthesized by a simple one-step microwave-solvothermal ionic liquid method. Structuralmore » dependent photoluminescence was observed from the double-shelled hollow microspheres.« less
  • No abstract prepared.
  • Novel rose-like three-dimensional Sn(HPO{sub 4}){sub 2}.H{sub 2}O nanostructures self-assembled by tightly stacked nanopetals were successfully synthesized by a simple cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol microemulsion system under solvothermal conditions for the first time. A series of compared experiments were carried out to investigate the factors that influence the morphology and size of the products. It was found that the molar ratio of water to CTAB and the concentration of SnCl{sub 4} aqueous solution play important roles in the formation of the rose-like nanostructures. A possible formation mechanism of rose-like nanostructures was proposed, which may be related to the crystal structure of Sn(HPO{submore » 4}){sub 2}.H{sub 2}O and the spherical micelles formed by the microemulsion. The electrochemical properties of Sn(HPO{sub 4}){sub 2}.H{sub 2}O were investigated through cyclic voltammetry (CV) measurements. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and field-emission scanning electron microscope (FE-SEM) were used to characterize the products.« less