Machinability improvement in Inconel-718 by enhanced tribological and thermal environment using textured tool

Journal of Thermal Analysis and Calorimetry - Machinability of Inconel-718 superalloy in conventional approach is poor—this fact necessitates advanced technological adoption such as improved...     

Evolution of isolated streamwise vortices in the late stages of boundary layer transition

Experiments were conducted with two, smooth hills, lying well within the boundary layer over a flat plate mounted in a wind tunnel. One hill was shallow, with peak height 1.5 mm and width 50 mm; the other, steep, 3 mm high and 30 mm wide. Since the hills occupied one-half of the tunnel span, streamwise vorticity formed near the hills’ edge. At a freestream speed of 3.5 m/s, streaks formed with inflectional wall-normal and spanwise velocity profiles but without effecting transition. Transition, observed at 7.5 m/s, took different routes with the two hills. With the steep hill, streamwise velocity signals exhibited the passage of a wave packet which intensified before breakdown to turbulence. With the shallow hill there was a broad range of frequencies present immediately downstream of the hill. These fluctuations grew continuously and transition occurred within a shorter distance. Since the size of the streamwise vorticity generated at the hill edge is of the order of the hill height, the shallow hill generates vorticity closer to the wall and supports an earlier transition, whereas the steep hill creates a thicker vortex and associated streaks which exhibit oscillations due to their own instability as an additional precursor stage before transition.     

Flow cytometry-based evaluation and enrichment of multiwalled carbon nanotube dispersions

The uniform aqueous dispersion of carbon nanotubes (CNTs) is a vital but challenging task required for their utilization in most technologies. We propose and demonstrate a technique based on forward- and side-scatter analysis on a flow cytometer to characterize the components in a dispersion of multiwalled CNTs (MWCNTs). The method simultaneously distinguishes various MWCNT components such as short and long CNTs, nanotube bundles, and particulates. It also detects the emergence of new CNT populations as a result of centrifugation. We use this method, together with classical methods such as UV and Raman spectroscopy, to observe and study the multistep MWCNT dispersion process in various surfactants (Pluronic, Triton X-100, sodium dodecyl sulfate, and cetyl trimethylammonium bromide). On the basis of the distinct scatter patterns obtained, we confirm and elaborate the surfactant-assisted unzipping mechanism of MWCNT dispersion. We also show that the ultrasonic energy spent after MWCNT unbundling and unwinding can be minimized and the process optimized for each surfactant by correct end point detection through scatter analysis. The ability to enrich nanotube population in dispersion by using the sorting mode of a flow cytometer is confirmed by electron microscopy and Raman spectroscopy. This method can thus be used for observing and enriching MWCNT components and as a complementary technique to UV spectroscopy for studying and optimizing MWCNT dispersion in surfactants.     

Separation of chelating agents as copper complexes by capillary zone electrophoresis using quaternary ammonium bromides as additives in N-methylformamide

This study presents the use of quaternary ammonium bromides as additives in N-methylformamide (NMF) for the separation and quantification of chelating agents as copper complexes by capillary zone electrophoresis (CZE). The new quaternary ammonium bromides were synthesized in our laboratory and used for the first time for CZE applications performed in NMF media. The methods were developed and optimized for determination of six chelating agents (trans-1,2-diaminocyclohexane-N,N,N′,N′-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N′,N′-triacetic acid (HEDTA), nitrilotriacetic acid (NTA) and triethylenetetraaminehexaacetic acid (TTHA)) as copper complexes. Among the tested electrolyte additives in NMF media (pH_app 10.2) dimethyldioctylammonium bromide (DMDOAB), dimethyldinonylammonium bromide (DMDNAB) and dimethyldidecylammonium bromide (DMDDAB), at a concentration of 20 mmol L⁻¹ improved the separation of the copper complexes. The optimized methods require only 12 min for one analysis, and the detection limits for copper complexes of DMDNAB, the best-performing additive, were ≤24 μmol L⁻¹. Relative standard deviations (R.S.D.) for migration times were ≤2.5, ≤2.1, ≤3.1% and for peak areas, ≤3.1, ≤3.0, ≤3.2% for DMDOAB, DMDNAB and DMDDAB used as additives, respectively. All three methods were successfully applied to the analysis of natural and wastewater samples. No matrix effects from these samples were observed. The interaction between quaternary ammonium bromides and copper complexes is discussed.     

Thermal and X‐ray powder diffraction studies of aliphatic polyester dendrimers

The syntheses and thermal and X‐ray powder diffraction analyses of three sets of aliphatic polyester dendrimers based on 2,2‐bis(hydroxymethyl)propionic acid as a repeating unit and 2,2‐dimethyl‐1,3‐propanediol, 1,5‐pentanediol, and 1,1,1‐tris(hydroxymethyl)ethane as core molecules are reported. These dendritic polyesters were prepared in high yields with the divergent method. The thermal properties of these biodendrimers were evaluated with thermogravimetric analysis and differential scanning calorimetry. The thermal decomposition of the compounds occurred around 250 °C for the hydroxyl‐ended dendrimers and around 150 °C for the acetonide‐protected dendrimers. In addition, the crystallinity of the lower generation dendrimers was evaluated with X‐ray powder diffraction. The highest crystallinity and the highest melting points were observed for the first‐generation dendritic compounds. The higher generation dendrimers showed weaker melting transitions during the first heating scan. Only the glass‐transition temperatures were observed in subsequent heating scans. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5574–5586, 2004     

X‐ray Absorption Near‐Edge Structure and Nuclear Magnetic Resonance Study of the Lithium–Sulfur Battery and its Components

Understanding the mechanism(s) of polysulfide formation and knowledge about the interactions of sulfur and polysulfides with a host matrix and electrolyte are essential for the development of long‐cycle‐life lithium–sulfur (Li–S) batteries. To achieve this goal, new analytical tools need to be developed. Herein, sulfur K‐edge X‐ray absorption near‐edge structure (XANES) and ^6,7Li magic‐angle spinning (MAS) NMR studies on a Li–S battery and its sulfur components are reported. The characterization of different stoichiometric mixtures of sulfur and lithium compounds (polysulfides), synthesized through a chemical route with all‐sulfur‐based components in the Li–S battery (sulfur and electrolyte), enables the understanding of changes in the batteries measured in postmortem mode and in operando mode. A detailed XANES analysis is performed on different battery components (cathode composite and separator). The relative amounts of each sulfur compound in the cathode and separator are determined precisely, according to the linear combination fit of the XANES spectra, by using reference compounds. Complementary information about the lithium species within the cathode are obtained by using ⁷Li MAS NMR spectroscopy. The setup for the in operando XANES measurements can be viewed as a valuable analytical tool that can aid the understanding of the sulfur environment in Li–S batteries.     

Self-assembly properties of bile acid derivatives of l-cysteine,l-valine and l-serine alkyl esters

Comprehensive self-assembly studies for nine bile acid amides of amino acid esters are reported. The number of the hydroxyl groups attached to the steroidal skeleton and the character of the amino acid ester moiety were used as variables when examining the self-assembly properties of the compounds. Two of the compounds were shown to undergo self-assembly leading to organogelation. In addition, preliminary self-assembly studies in aqueous mixtures of polar organic solvents were conducted. Microscopic methods (optical microscopy and scanning electron microscopy) were utilised in order to gain a deeper insight into the self-assembled structures. Furthermore, single-crystal X-ray structures for three of the compounds were solved.     

The advantageous way of getting the lowest uncertainty values of elemental concentration by INAA

Analysts in a NAA accredited laboratory bear full responsibility for the report on the material they investigated. The document has to contain the most accurate values that can be, as confidence to further use of the material on the market. To this end, analysts are expected to use the standardization method providing the lowest element concentration uncertainty and carefully quantify every factor that may contribute to the validity of the results. The question is which method is the most advantageous one from this perspective and in what conditions. This paper presents a comparison between results of the elemental analysis of a CRM sample by INAA, as obtained through two standardization methods and three calculations variants applied to the same experimental data. The results were discussed in terms of uncertainty and of the E _n statistical criterion recommended for inter-comparison exercises. The influence of the nuclear reaction and decay data was studied in several cases.