scholarly journals New Volatile Perfluorinated Amidine–Carboxylate Copper(II) Complexes as Promising Precursors in CVD and FEBID Methods

Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3145
Author(s):  
Katarzyna Madajska ◽  
Iwona Barbara Szymańska

In the present study, we have synthesised and characterised newly copper(II) complexes with the general formula [Cu2(NH2(NH=)CC2F5)2(µ–O2CCRF)4], where RF = CF3, C2F5, C3F7, C4F9. Infrared spectroscopy, mass spectrometry with electron ionisation (EI MS), and density-functional theory (DFT) calculations were used to confirm compounds’ composition and structure. The volatility of the compounds was studied using thermal analysis (TGA), EI MS mass spectrometry, variable temperature infrared spectroscopy (VT IR), and sublimation experiments. Research has revealed that these compounds are the source of metal carriers in the gas phase. The thermal decomposition mechanism over reduced pressure was proposed. TGA studies demonstrated that copper transfer to the gaseous phase occurs even at atmospheric pressure. Two selected complexes [Cu2(NH2(NH=)CC2F5)2(µ–O2CC2F5)4] and [Cu2(NH2(NH=)CC2F5)2(µ–O2CC3F7)4] were successful used as chemical vapour deposition precursors. Copper films were deposited with an evaporation temperature of 393 K and 453 K, respectively, and a decomposition temperature in the range of 573–633 K without the use of hydrogen. The microscopic observations made to investigate the interaction of the [Cu2(NH2(NH=)CC2F5)2(µ–O2CC2F5)4] with the electron beam showed that the ligands are completely lost under transmission electron microscopy analysis conditions (200 keV), and the final product is copper(II) fluoride. In contrast, the beam energy in scanning electron microscopy (28 keV) was insufficient to break all coordination bonds. It was shown that the Cu-O bond is more sensitive to the electron beam than the Cu-N bond.

2021 ◽  
Author(s):  
Piero Ferrari ◽  
Hung Tan Pham ◽  
Jan Vanbuel ◽  
Andre Fielicke ◽  
Minh T. Nguyen ◽  
...  

The NbAl8H8+ cluster was formed in a molecular beam and characterized by mass spectrometry and infrared spectroscopy. Density functional theory calculations showed that its lowest-energy isomer is a high symmetry...


2022 ◽  
Vol 40 (2) ◽  
pp. 022601
Author(s):  
Austin M. Cano ◽  
Suresh Kondati Natarajan ◽  
Jonathan L. Partridge ◽  
Simon D. Elliott ◽  
Steven M. George

2005 ◽  
Vol 877 ◽  
Author(s):  
M. Wei ◽  
N. Khare ◽  
K. A. Yates ◽  
D. Zhi ◽  
J. L. MacManus-Driscoll

AbstractNanosized Co-doped ZnO samples were synthesized using an ultrasonic spray assisted chemical vapour deposition method. Microstructural and magnetic properties of these samples were studied. The room-temperature ferromagnetism was observed in the Co-doped ZnO. Also, x-ray analysis revealed a wurtzite ZnO structure with a small change of the lattice constants due to the doping of Co in ZnO. Raman spectroscopy of the Co-doped ZnO films indicated direct substitution of Co. Scanning electron microscopy showed nanostructured Co-doped ZnO with a ring or cup shape. Transmission electron microscopy analysis revealed nano grains within the rings of an average diameter of around 10 nm. Both energy dispersive spectroscopy and energy-filtered transmission electron microscopy indicated a uniform distribution of Co.


2019 ◽  
Vol 10 (1) ◽  
Author(s):  
Mollie A. Touve ◽  
Andrea S. Carlini ◽  
Nathan C. Gianneschi

Abstract We describe the observation of stimuli-induced peptide-based nanoscale assemblies by liquid cell transmission electron microscopy (LCTEM). LCTEM offers the opportunity to directly image nanoscale materials in liquid. Despite broad interest in characterizing biological phenomena, electron beam-induced damage remains a significant problem. Concurrently, methods for verifying chemical structure during or following an LCTEM experiment have been few, with key examples limited to electron diffraction or elemental analysis of crystalline materials; this strategy is not translatable to biopolymers observed in nature. In this proof-of-concept study, oligomeric peptides are biologically or chemically stimulated within the liquid cell in a TEM to assemble into nanostructures. The resulting materials are analyzed by MALDI-imaging mass spectrometry (MALDI-IMS) to verify their identity. This approach confirms whether higher-order assemblies observed by LCTEM consist of intact peptides, verifying that observations made during the in situ experiment are because of those same peptides and not aberrant electron beam damage effects.


2017 ◽  
Vol 296 ◽  
pp. 86-94
Author(s):  
Robert Bachliński ◽  
◽  
Małgorzata Galarda ◽  

The article presents a case involving an appearance of an atypical 3,4-methylenedioxymethamphetamine (MDMA) in the form of nitrate on the illicit drug market. This compound can be identified only by using such analytical methods as capillary electrophoresis (CE) or scanning electron microscopy (SEM), which are not routinely applied to forensic analyses of this type of substances. Therefore, particular caution should be exercised whenever a gas chromatography-mass spectrometry (GC-MS) method unambiguously identifies a substance, yet infrared spectroscopy fails to confirm this result.


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):  
J. G. Adams ◽  
M. M. Campbell ◽  
H. Thomas ◽  
J. J. Ghldonl

Since the introduction of epoxy resins as embedding material for electron microscopy, the list of new formulations and variations of widely accepted mixtures has grown rapidly. Described here is a resin system utilizing Maraglas 655, Dow D.E.R. 732, DDSA, and BDMA, which is a variation of the mixtures of Lockwood and Erlandson. In the development of the mixture, the Maraglas and the Dow resins were tested in 3 different volumetric proportions, 6:4, 7:3, and 8:2. Cutting qualities and characteristics of stability in the electron beam and image contrast were evaluated for these epoxy mixtures with anhydride (DDSA) to epoxy ratios of 0.4, 0.55, and 0.7. Each mixture was polymerized overnight at 60°C with 2% and 3% BDMA.Although the differences among the test resins were slight in terms of cutting ease, general tissue preservation, and stability in the beam, the 7:3 Maraglas to D.E.R. 732 ratio at an anhydride to epoxy ratio of 0.55 polymerized with 3% BDMA proved to be most consistent. The resulting plastic is relatively hard and somewhat brittle which necessitates trimming and facing the block slowly and cautiously to avoid chipping. Sections up to about 2 microns in thickness can be cut and stained with any of several light microscope stains and excellent quality light photomicrographs can be taken of such sections (Fig. 1).


Author(s):  
M. A. Hayat

Potassium permanganate has been successfully employed to study membranous structures such as endoplasmic reticulum, Golgi, plastids, plasma membrane and myelin sheath. Since KMnO4 is a strong oxidizing agent, deposition of manganese or its oxides account for some of the observed contrast in the lipoprotein membranes, but a good deal of it is due to the removal of background proteins either by dehydration agents or by volatalization under the electron beam. Tissues fixed with KMnO4 exhibit somewhat granular structure because of the deposition of large clusters of stain molecules. The gross arrangement of membranes can also be modified. Since the aim of a good fixation technique is to preserve satisfactorily the cell as a whole and not the best preservation of only a small part of it, a combination of a mixture of glutaraldehyde and acrolein to obtain general preservation and KMnO4 to enhance contrast was employed to fix plant embryos, green algae and fungi.


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