Synthesis and characterization of fluorinated phosphonium ionic liquids

2007 ◽  
Vol 85 (10) ◽  
pp. 660-667 ◽  
Author(s):  
Jocelyn J Tindale ◽  
Chris Na ◽  
Michael C Jennings ◽  
Paul J Ragogna
Keyword(s):  
Thermal Decomposition ◽  
Ionic Liquids ◽  
Melting Point ◽  
Synthesis And Characterization ◽  
High Melting ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Phosphonium Ionic Liquids

A wide variety of phosphonium ionic liquids containing fluorous ponytails Rfn (Rfn = –(CF2)n–1CF3; n = 4, 6, 10) are synthesized by the reaction of Rfn-(CH2)2-I with trialkylphosphines (R3P; R = Me, nBu, nOct). The efficacy of multiple metathetical routes to anion exchange have been investigated, thus the corresponding BF4–, PF6–, tosylate (OTs–) and triflate (OTf–) derivatives have also been prepared. All compounds have been comprehensively characterized by multinuclear NMR spectroscopy, ESI-MS, DSC, and TGA/SDTA, and in the case of [Me3PCH2CH2Rf4][I] by single crystal X-ray diffraction. These materials range from high melting solids (e.g., [Me3P(CH2)2Rf4][I] Tm = 195 °C) to very low melting liquids (e.g., [nOct3P(CH2)2Rf4][OTf] Tg = –64 °C), and they all have high thermal decomposition points (295 to 394 °C). Incorporation of the more weakly coordinating BF4– and PF6– yielded a significant increase in the melting point of the materials, in contrast to OTf– and OTs– derivatives, which all exhibited significantly depressed melting points.Key words: phosphonium ionic liquids, alternative solvents, fluorine, phosphorus, fluorous ponytails.

Synthesis and Characterization of Co Nanoparticles by Solventless Thermal Decomposition

2007 ◽  
Vol 119 ◽  
pp. 71-74 ◽  
Author(s):  
Yan Li ◽  
Xiao Li Zhang ◽  
Young Hwan Kim ◽  
Young Soo Kang
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Synthesis And Characterization ◽  
Vibrating Sample Magnetometer ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Structure Of Nanoparticles ◽  
Co Nanoparticles

Co nanoparticles were synthesized via a solventless thermal decomposition of Co2+-oleate2. The crystalline structure is strongly affected by the thermal treatment of the Co nanoparticles. Further, the annealing also results in the decomposition of surfactant around Co particles. The size of nanoparticles was confirmed by transmission electron microscopy (TEM). The crystal structure of nanoparticles was characterized by X-ray diffraction pattern (XRD). The magnetic properties were characterized by vibrating sample magnetometer (VSM).

The Synthesis and Characterization of NiCo2O4 Nanoparticles

2012 ◽  
Vol 512-515 ◽  
pp. 2467-2470 ◽  
Author(s):  
Hong Xiao Zhao ◽  
Bao Ming He ◽  
Jing Li ◽  
Hui Min Jia ◽  
Li Wei Mi
Keyword(s):  
Thermal Decomposition ◽  
Hydrothermal Method ◽  
Physical Adsorption ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
Oxalate Precursor ◽  
X Ray ◽  
Scanning Electron

In this paper, NiCo2O4 nanoparticles were synthesized by three different methods. The applied preparation methods in this research are thermal decomposition of a mixed oxalate precursor, combustion synthesis and hydrothermal method. The crystalline phase, morphology and specific surface area (BET) of the resultant samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and nitrogen physical adsorption, respectively. The research found that the hydrothermal method is a promising method to prepare NiCo2O4 nanoparticles.

Synthesis and characterization of robust three-dimensional chiral metal sulfates

RSC Advances ◽  
2014 ◽  
Vol 4 (92) ◽  
pp. 50435-50442 ◽  
Author(s):  
J. N. Behera ◽  
Joydeep Bhattacharjee ◽  
Satoshi Horike ◽  
Subba R. Marri ◽  
Prem P. Dahiya
Keyword(s):  
Thermal Decomposition ◽  
High Temperature ◽  
First Principles ◽  
Three Dimensional ◽  
Ammonium Ion ◽  
Synthesis And Characterization ◽  
First Principles Calculations ◽  
X Ray Diffraction ◽  
X Ray

Chiral three-dimensional Mg(ii) and Mn(ii) sulfates have been synthesized, well characterized and studied from first-principles calculations. High temperature X-ray diffraction, thermogravimetric analysis and DFT calculations reveal that the structures of both the compounds remain intact even after the thermal decomposition of the ammonium ion.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

scholarly journals Synthesis and Characterization of Clay Polymer Nanocomposites of P(4VP-co-AAm) and Their Application for the Removal of Atrazine

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Nanocomposite Materials ◽  
Synthesis And Characterization ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
Numerous Species ◽  
X Ray ◽  
Different Types ◽  
Synthesized Materials

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.

scholarly journals High-pressure synthesis and characterization of the non-centrosymmetric scandium borate ScB6O9(OH)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Structure Solution ◽  
Temperature Experiment ◽  
Pressure Synthesis

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Composite ◽  
Transmission Electron ◽  
One Step ◽  
Ft Ir ◽  
Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

Synthesis and Characterization of Multiferroic NiFe2O4/BiFeO3 Nanocomposites by Modified Pechini Method

2011 ◽  
Vol 197-198 ◽  
pp. 456-459
Author(s):  
Xian Ming Liu ◽  
Wen Liang Gao
Keyword(s):  
Pechini Method ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Magnetic Bias ◽  
Field Frequency ◽  
Magnetic Field Frequency ◽  
X Ray ◽  
Structure And Morphology ◽  
Modified Pechini Method

Spinel-perovskite multiferroics of NiFe2O4/BiFeO3 nanoparticles were prepared by modified Pechini method. The structure and morphology of the composites were examined by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the composites consisted of spinel NiFe2O4 and perovskite BiFeO3 after annealed at 700°C for 2h, and the particle size ranges from 40 to 100nm. VSM and ME results indicated that the nanocomposites exhibited both tuning magnetic properties and a ME effect. The ME effect of the nanocomposites strongly depended on the magnetic bias and magnetic field frequency.

Hydrothermal Synthesis and Characterization of BiFeO3 Polyhedral Crystallites

2012 ◽  
Vol 174-177 ◽  
pp. 508-511
Author(s):  
Lin Lin Yang ◽  
Yong Gang Wang ◽  
Yu Jiang Wang ◽  
Xiao Feng Wang
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Electron

BiFeO3 polyhedrons had been successfully synthesized via a hydrothermal method. The as-prepared products were characterized by power X-ray diffraction (XRD) pattern, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The possible mechanisms for the formation of BiFeO3 polyhedrons were discussed. Though comparison experiments, it was found that the kind of precursor played a key role on the morphology control of BiFeO3 crystals.

Synthesis and Characterization of a Fluorescent Dianthraceno­indacene

Synlett ◽  
2018 ◽  
Vol 29 (19) ◽  
pp. 2562-2566 ◽  
Author(s):  
Michael Haley ◽  
Conerd Frederickson ◽  
Joshua Barker ◽  
Justin Dressler ◽  
Zheng Zhou ◽  
...  
Keyword(s):  
Neutral Molecule ◽  
Conical Intersection ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Irreversible Reduction ◽  
Inside Out

A freely soluble dianthracenoindacene derivative has been synthesized using an ‘inside-out’ Friedel–Crafts alkylation method and is the first fluorescent diacenoindacene reported. Linear fusion of the anthracenes is confirmed by X-ray diffraction studies on the neutral molecule as well as its dianion. Based on predictions from our previous studies, this is also the least antiaromatic diacenoindacene derivative yet to be prepared, which is reflected in its highly negative and irreversible reduction. With its paratropicity essentially eliminated, we posit that the molecule is no longer deactivated by a conical intersection, typical of antiaromatic molecules, and therefore fluorescence is restored. This follows the trend shown in the related dianthracenopentalenes, with the reappearance of fluorescence when the outer acene groups are extended to linearly-fused anthracene moieties.

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