scholarly journals Experimental and Theoretical Study of the Covalent Grafting of Triazole Layer onto the Gold Surface

Materials ◽  
2020 ◽  
Vol 13 (13) ◽  
pp. 2927
Author(s):  
Nimet Orqusha ◽  
Sereilakhena Phal ◽  
Avni Berisha ◽  
Solomon Tesfalidet

Finding novel strategies for surface modification is of great interest in electrochemistry and material sciences. In this study, we present a strategy for modification of a gold electrode through covalent attachment of triazole (TA) groups. Triazole groups were electrochemically grafted at the surface of the electrode by a reduction of in situ generated triazolediazonium cations. The resulting grafted surface was characterized before and after the functionalization process by different electrochemical methods (cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS)) confirming the presence of the grafted layer. The grafting of TA on the electrode surface was confirmed using analysis of surface morphology (by atomic force microscopy), the thickness of the grafted layer (by ellipsometry) and its composition (by X-ray photoelectron spectroscopy). Density functional theory (DFT) calculations imply that the grafted triazole offers a stronger platform than the grafted aryl layers.

Sensors ◽  
2018 ◽  
Vol 18 (11) ◽  
pp. 3976 ◽  
Author(s):  
Matjaž Finšgar ◽  
David Majer ◽  
Uroš Maver ◽  
Tina Maver

In this work, unmodified screen-printed electrode (bare SPE) and Sb-film modified SPE (SbFSPE) sensors were employed for the analysis of trace amounts of Pb(II) in non-deaerated water solutions. The modified electrode was performed in situ in 0.5 mg/L Sb(III) and 0.01 M HCl. The methodology was validated for an accumulation potential of –1.1 V vs. Ag/AgCl and an accumulation time of 60 s. A comparative analysis of bare SPE and SbFSPE showed that the detection and quantification limits decrease for the bare SPE. The method with the bare SPE showed a linear response in the 69.8–368.4 µg/L concentration range, whereas linearity for the SbFSPE was in the 24.0–319.1 µg/L concentration range. This work also reports the reason why the multiple standard addition method instead of a linear calibration curve for Pb(II) analysis should be employed. Furthermore, the analytical method employing SbFSPE was found to be more accurate and precise compared to the use of bare SPE when sensors were employed for the first time, however this performance changed significantly when these sensors were reused in the same manner. Furthermore, electrochemical impedance spectroscopy was used for the first time to analyse the electrochemical response of sensors after being used for multiple successive analyses. Surface characterisation before and after multiple successive uses of bare SPE and SbFSPE sensors, with atomic force microscopy and field emission scanning electron microscopy, showed sensor degradation. The interference effect of Cd(II), Zn(II), As(III), Fe(II), Na(I), K(I), Ca(II), Mg(II), NO3–, Bi(III), Cu(II), Sn(II), and Hg(II) on the Pb(II) stripping signal was also studied. Finally, the application of SbFSPE was tested on a real water sample (from a local river), which showed high precision (RSD = 8.1%, n = 5) and accurate results.


Author(s):  
Matjaž Finšgar ◽  
David Majer ◽  
Uroš Maver ◽  
Tina Maver

In this work, unmodified screen-printed electrode (bare SPE) and Sb-film modified SPE (SbFSPE) sensors were employed for the analysis of trace amounts of Pb(II) in non-deaerated water solutions. The modified electrode was performed in situ in 0.5 mg/L Sb(III) and 0.01 M HCl. The methodology was validated for an accumulation potential of –1.1 V vs. Ag/AgCl and an accumulation time of 60 s. A comparative analysis of bare SPE and SbFSPE showed that the detection and quantification limits decrease for the bare SPE. The method with the bare SPE showed a linear response in the 69.8–368.4 µg/L concentration range, whereas linearity for the SbFSPE was in the 24.0–319.1 µg/L concentration range. This work also reports the reason why the multiple standard addition method instead of a linear calibration curve for Pb(II) analysis should be employed. Furthermore, the analytical method employing SbFSPE was found to be more accurate and precise compared to the use of bare SPE when sensors were employed for the first time, however this performance changed significantly when these sensors were reused in the same manner. Furthermore, electrochemical impedance spectroscopy was used for the first time to analyse the electrochemical response of sensors after being used for multiple successive analyses. Surface characterisation before and after multiple successive uses of bare SPE and SbFSPE sensors, with atomic force microscopy and field emission scanning electron microscopy, showed sensor degradation. The interference effect of Cd(II), Zn(II), As(III), Fe(II), Na(I), K(I), Ca(II), Mg(II), NO3– Bi(III), Cu(II), Sn(II), and Hg(II) on the Pb(II) stripping signal was also studied. Finally, the application of SbFSPE was tested on a real water sample (from a local river), which showed high precision (RSD = 8.1%, n = 5) and accurate results.


2013 ◽  
Vol 28 (2) ◽  
pp. 68-71 ◽  
Author(s):  
Thomas N. Blanton ◽  
Debasis Majumdar

In an effort to study an alternative approach to make graphene from graphene oxide (GO), exposure of GO to high-energy X-ray radiation has been performed. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) have been used to characterize GO before and after irradiation. Results indicate that GO exposed to high-energy radiation is converted to an amorphous carbon phase that is conductive.


2018 ◽  
Vol 115 (25) ◽  
pp. E5642-E5650 ◽  
Author(s):  
Matthias Meier ◽  
Jan Hulva ◽  
Zdeněk Jakub ◽  
Jiří Pavelec ◽  
Martin Setvin ◽  
...  

Determining the structure of water adsorbed on solid surfaces is a notoriously difficult task and pushes the limits of experimental and theoretical techniques. Here, we follow the evolution of water agglomerates on Fe3O4(001); a complex mineral surface relevant in both modern technology and the natural environment. Strong OH–H2O bonds drive the formation of partially dissociated water dimers at low coverage, but a surface reconstruction restricts the density of such species to one per unit cell. The dimers act as an anchor for further water molecules as the coverage increases, leading first to partially dissociated water trimers, and then to a ring-like, hydrogen-bonded network that covers the entire surface. Unraveling this complexity requires the concerted application of several state-of-the-art methods. Quantitative temperature-programmed desorption (TPD) reveals the coverage of stable structures, monochromatic X-ray photoelectron spectroscopy (XPS) shows the extent of partial dissociation, and noncontact atomic force microscopy (AFM) using a CO-functionalized tip provides a direct view of the agglomerate structure. Together, these data provide a stringent test of the minimum-energy configurations determined via a van der Waals density functional theory (DFT)-based genetic search.


2005 ◽  
Vol 20 (5) ◽  
pp. 1139-1145 ◽  
Author(s):  
Jeremiah T. Abiade ◽  
Wonseop Choi ◽  
Rajiv K. Singh

To understand the ceria–silica chemical mechanical polishing (CMP) mechanisms, we studied the effect of ceria slurry pH on silica removal and surface morphology. Also, in situ friction force measurements were conducted. After polishing; atomic force microscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy were used to quantify the extent of the particle–substrate interaction during CMP. Our results indicate the silica removal by ceria slurries is strongly pH dependent, with the maximum occurring near the isoelectric point of the ceria slurry.


2004 ◽  
Vol 811 ◽  
Author(s):  
Yingge Du ◽  
Surajit Atha ◽  
Robert Hull ◽  
James F. Groves ◽  
Igor Lyubinetsky ◽  
...  

ABSTRACTA method has been developed for specifying the growth location of Cu2O nanodotson SrTiO3 (100) substrates. Growth location has been specified by using a focused ion beam (FIB) to modify microscopic and nanoscopic regions of the SrTiO3substrate prior to Cu2O deposition. Deposition onto the modified regions under carefully selected process conditions has generated nanodot growth at the edge of microscopic FIB-induced features and on top of nanoscopic FIB-induced features. For this work, an array of evenly spaced FIB implants was first patterned into several regions of each substrate. Within each sub-division of the array, the FIB implants were identical in Ga+ energy and dosage and implant diameter and spacing. After FIB surface modification and subsequent in-situ substrate cleaning, Cu2O nanodots were synthesized on the patterned SrTiO3 substrates using oxygen plasma assisted molecular beam epitaxy. The substrates and nanodots were characterized using atomic force microscopy at various stages of the process; in-situ X-ray photoelectron spectroscopy and Auger electron spectroscopy analysis demonstrated that the final stoichiometry of the nanodots was Cu2O. The photocatalytic decomposition of water on Cu2O under visible light irradiation has been reported. If the Cu2O can be located in the form ofislands on a carefully selected substrate, then it could be possible to greatly enhance the efficiency of the photochemical process.


2021 ◽  
Author(s):  
Reshma P R ◽  
Anees Pazhedath ◽  
Ganesan Karuppiah ◽  
Arun Prasad ◽  
Sandip Dhara

Abstract Recently emerged transition metal oxide (TMO) based 2D nanostructures are gaining a foothold in advanced applications. Unlike, 2D transition metal dichalchogenides, it is strenuous to obtain high quality thin TMOs due to exotic surface reconstruction during synthesis. Herein, we report the synthesis of bilayer thin 2D-V2O5 nanosheets using chemical exfoliation. Synchrotron X-ray diffraction, X-ray photoelectron spectroscopy and atomic force microscopy substantiate the successful formation of bilayer thin 2D-V2O5. Ultraviolet-visible absorption spectra exhibit a thickness dependent blue shift in the optical band gap, signifying the emergence of electronic decoupling. Raman spectroscopy fingerprinting shows a thickness dependent vibrational decoupling of phonon modes. Further, it has been verified by computing the lattice vibrational modes using density functional perturbation theory. In this study, the manifestation of the electronic and vibrational decoupling is used as a novel probe to confirm the successful exfoliation of bilayer 2D-V2O5 from its bulk counterpart.


2020 ◽  
pp. 095400832094229
Author(s):  
Shifeng Wen ◽  
Jiacheng Ma

In this article, polyvinylpyrrolidone (PVP) was used for the noncovalent modification on the surface of graphene. Compared with covalent modification, this method maintained the original structure of graphene layers, thereby maximizing the original properties of graphene. The π–π noncovalent bond was formed between PVP and graphene by X-ray photoelectron spectroscopy analysis, indicating that PVP successfully modified graphene. The thickness of graphene layer was measured by atomic force microscopy, which showed that the distance between graphene layers was increased by 5–6 nm, and the stability of the modified graphene in N, N-dimethylformamide was remarkably improved. The obtained composite coating by combination of the modified graphene and the epoxy resin was subjected to electrochemical impedance test to obtain the best anticorrosive effect of the coating with the graphene content of 0.3 wt%. The results showed that the addition of graphene to the epoxy resin could effectively improve the anticorrosive effect. Meanwhile, the good electrical conductivity allowed the electrons which lost from the substrate to led to air or saline rapidly, thereby reducing the combination of iron ions with oxygen and the generation of corrosion products (iron oxides).


2019 ◽  
Vol 27 (06) ◽  
pp. 1950165
Author(s):  
IMENE BENMAHAMMED ◽  
TAHAR DOUADI ◽  
SAIFI ISSAADI ◽  
DJAMEL DAOUD ◽  
SALAH CHAFAA

The study of the corrosion inhibition of mild steel in acid medium 1 M HCl by the Schiff base compounds named {4,4′-Bis(pyrrole-2-carboxaldehyde) diphenyl diimino sulfide (L1) and 4,4′-Bis(thiophene-2-carboxaldehyde) diphenyl diimino sulfide (L2)} was carried out using various techniques: weight loss measurements, polarization curves, electrochemical impedance spectroscopy (EIS), atomic force microscopy (AFM), Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The influence of the concentration, immersion time and temperature was examined and the mode of adsorption of these inhibitors on the surface of the metal was highlighted by assigning the appropriate isotherm. The experimental results indicate that these compounds are effective corrosion inhibitors and the inhibitory competence rises with increasing inhibitor concentration. The adsorption of these compounds on the mild steel surface obeys the isotherm of Langmuir. The correlation between the molecular structures and the inhibitory properties of the compounds studied was performed using the Density Functional Theory (DFT) method. Furthermore, molecular dynamics (MD) simulation has been taken into account. The results indicate that the adsorption energy of L1 was less than L2, which is in accordance with the experimentally determined inhibition effect.


Sign in / Sign up

Export Citation Format

Share Document