Graphene nanodots-encaged porous gold electrode fabricated via ion beam sputtering deposition for electrochemical analysis of heavy metal ions

All rights reserved. A graphene nanodots-encaged porous gold electrode via ion beam sputtering deposition (IBSD) for electrochemical sensing is presented. The electrodes were fabricated using Au target, and a composite target of Al and graphene, which were simultaneously sputtered onto glass substrates by Ar ion beam, followed with hydrochloric acid corrosion. The as-prepared graphene nanodots-encaged porous gold electrodes were then used for the analysis of heavy metal ions, e.g. Cu2+ and Pb2+ by Osteryoung square wave voltammetry (OSWV). These porous electrodes exhibited enhanced detection range for the heavy metal ions due to the entrapped graphene nanodots in 3-D porous structure. In addition, it was also found that when the thickness of porous electrode reached 40 nm the detection sensitivity came into saturation. The linear detection range is 0.009-4 μM for Cu2+ and 0.006-2.5 μM for Pb2+. Good reusability and repeatability were also observed. The formation mechanism and 3-D structure of the porous electrode were also investigated using scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray photoelectron spectra (XPS). This graphene entrapped 3-D porous structure may envision promising applications in sensing devices.

Focused ion beam milling as a universal template technique for patterned growth of carbon nanotubes

Focused ion beam (FIB) milling system has been used to create nanosized patterns as the template for patterned growth of carbon nanotubes on Si substrate surface without predeposition of metal catalysts. Carbon nanotubes only nucleate and grow on the template under controlled pyrolysis of iron phthalocyanine at 1000 °C. The size, growth direction, and density of the patterned nanotubes can be controlled under different growth conditions and template sizes. Atomic force microscopy and electron microscopy analyses reveal that the selective growth on the FIB template is due to its special surface morphology and crystalline structure.

Fabrication of nanoscale Ti honeycombs by focused ion beam

Ti honeycombs with the side of 800 and 400 nm were fabricated by focused ion beam (FIB), though the surfaces of the bottom and wall of the Ti honeycombs were rough, as compared with the surfaces of the bottom and wall of the Si honeycomb. It is demonstrated that the nanoscale Ti components can be fabricated in a short time by FIB.

Focused ion-beam (FIB) fabrication of micro-sized pillars for microcompression test

Pillars were fabricated by focused-ion beam (FIB) in a dual beam scanning electron microscope (SEM, FEI Quanta 3D). A multi-step milling procedure was adopted to prepare the pillars using Ga+ ion beam operated at 30 kV. The beam current was reduced from 5 nA for coarse milling down to 50 pA for fine milling, to minimize the surface damage induced by the Ga+ ion beam. The pillars were imaged at 52° tilt angle by SEM prior to the microcompression tests.

Synthesis and growth mechanism of Thin-film TiO2 nanotube arrays on focused-ion-beam micropatterned 3D isolated regions of titanium on silicon

In this paper, the fabrication and growth mechanism of net-shaped micropatterned self-organized thin-film TiO2 nanotube (TFTN) arrays on a silicon substrate are reported. Electrochemical anodization is used to grow the nanotubes from thin-film titanium sputtered on a silicon substrate with an average diameter of ?30 nm and a length of ?1.5 ?m using aqueous and organic-based types of electrolytes. The fabrication and growth mechanism of TFTN arrays from micropatterned three-dimensional isolated islands of sputtered titanium on a silicon substrate is demonstrated for the first time using focused-ion-beam (FIB) technique. This work demonstrates the use of the FIB technique as a simple, high-resolution, and maskless method for high-aspect-ratio etching for the creation of isolated islands and shows great promise toward the use of the proposed approach for the development of metal oxide nanostructured devices and their integration with micro- and nanosystems within silicon-based integrated-circuit devices.

Focused ion beam milling of carbon nanotube yarns and bucky-papers : correlating their internal structure with their macro-properties

Focused ion beam (FIB) milling through carbon nanotube (CNT) yarns and bucky-papers followed by scanning electron microscopy has recently emerged as a powerful tool for eliciting details of their internal structure. The internal arrangement of CNTs in bucky-papers and yarns directly affects their performance and characteristics. Consequently this information is critical for further optimisation of these structures and to tailor their properties for specific applications. This chapter describes in detail FIB milling of CNT yarns and bucky-papers and gives a range of examples where FIB milling has enabled a better understanding of how processing conditions and treatments affect the internal structure. Emphasis is placed on how FIB milling elucidates the influence of fabrication conditions on the internal arrangement of CNTs and how this influences the material's macroscopic properties.

Nanopatterning and electrical tuning of MoS2 layers with a subnanometer helium ion beam

We report subnanometer modification enabled by an ultrafine helium ion beam. By adjusting ion dose and the beam profile, structural defects were controllably introduced in a few-layer molybdenum disulfide (MoS2) sample and its stoichiometry was modified by preferential sputtering of sulfur at a few-nanometer scale. Localized tuning of the resistivity of MoS2 was demonstrated and semiconducting, metallic-like, or insulating material was obtained by irradiation with different doses of He(+). Amorphous MoSx with metallic behavior has been demonstrated for the first time. Fabrication of MoS2 nanostructures with 7 nm dimensions and pristine crystal structure was also achieved. The damage at the edges of these nanostructures was typically confined to within 1 nm. Nanoribbons with widths as small as 1 nm were reproducibly fabricated. This nanoscale modification technique is a generalized approach that can be applied to various two-dimensional (2D) materials to produce a new range of 2D metamaterials.

A novel graphene nanodots inlaid porous gold electrode for electrochemically controlled drug release

A uniform graphene nanodots inlaid porous gold electrode was prepared via ion beam sputtering deposition (IBSD) and mild corrosion chemistry. HRTEM, SEM, AFM and XPS analyses revealed the successful fabrication of graphene nanodots inlaid porous gold electrode. The as-prepared porous electrode was used as π-orbital-rich drug loading platform to fabricate an electrochemically controlled drug release system with high performance. π-orbital-rich drugs with amino mioety, like doxorubicin (DOX) and tetracycline (TC), were loaded into the graphene nanodots inlaid porous gold electrode via non-covalent π-π stacking interaction. The amino groups in DOX and TC can be easily protonated at acidic medium to become positively-charged NH3(+), which allow these drug molecules to be desorbed from the porous electrode surface via electrostatic repulsion when positive potential is applied at the electrode. The drug loading and release experiment indicated that this graphene nanodots inlaid porous gold electrode can be used to conveniently and efficiently control the drug release electrochemically. Not only did our work provide a benign method to electrochemically controlled drug release via electrostatic repulsion process, it also enlighten the promising practical applications of micro electrode as a drug carrier for precisely and efficiently controlled drug release via embedding in the body.

Graphene nanodots encaged 3-D gold substrate as enzyme loading platform for the fabrication of high performance biosensors

Herein, a uniform three-dimensional (3-D) graphene nanodots-encaged porous gold electrode was prepared via ion beam sputtering deposition (IBSD) and mild corrosion chemistry for efficient enzyme electrode fabrication. Enzymes, like glucose oxidase and catalase, were modified with pyrene functionalities and then loaded into the graphene nanodots encaged porous gold electrode via non-covalent π-π stacking interaction between pyrene and graphene. The fabricated enzyme electrodes showed profound reusability and repeatability, high sensitivity, inherent selectivity and enhanced detection range. As for glucose analysis a broad linear range from 0.05 to 100 mM was obtained and the linear range for hydrogen peroxide was 0.005 to 4 mM. Detection limits of 30 μM for glucose and 1 μM for hydrogen peroxide were achieved (S/N = 3), respectively. These electrodes can be applied to analyze the clinical samples with reliable results. The formation mechanism and 3-D structure of the porous electrode were investigated using high resolution transmission electron microscope (HRTEM), atomic force microscopy (AFM), scanning electron microscope (SEM) and electrochemical impedance spectroscopy (EIS). Most importantly, various other ideal biosensors can be fabricated using the same porous electrode and the same enzyme modification methodology.

Using polyatomic primary ions to probe an amino acid and a nucleic base in water ice

In this study on pure water ice, we show that protonated water species [H₂O]_nH⁺ are more prevalent than (H₂O)_n⁺ ions after bombardment by Au+ monoatomic and Au₃⁺ and C₆₀⁺ polyatomic projectiles. This data also reveals significant differences in water cluster yields under bombardment by these three projectiles. The amino acid alanine and the nucleic base adenine in solution have been studied and have been shown to have an effect on the water cluster ion yields observed using an Au₃⁺ ion beam.

TOF-SIMS analysis using C60. Effect of impact energy on yield and damage

C₆₀ has been shown to give increased sputter yields and, hence, secondary ions when used as a primary particle in SIMS analysis. In addition, for many samples, there is also a reduction in damage accumulation following continued bombardment with the ion beam. In this paper, we report a study of the impact energy (up to 120 keV) of C₆₀ on the secondary ion yield from a number of samples with consideration of any variation in yield response over mass ranges up to m/z 2000. Although increased impact energy is expected to produce a corresponding increase in sputter yield/rate, it is important to investigate any increase in sample damage with increasing energy and, hence, efficiency of the ion beams. On our test samples including a metal, along with organic samples, there is a general increase in secondary ion yield of high-mass species with increasing impact energy. A corresponding reduction in the formation of low-mass fragments is also observed. Depth profiling of organic samples demonstrates that when using C₆₀, there does not appear to be any increase in damage evident in the mass spectra as the impact energy is increased.

Exploring corrosion protection of Mg via ionic liquid pretreatment

We present the development of a 10–100 nanometer thick surface film upon pure Mg on exposure to an ionic liquid (IL) based on the bis(trifluoromethanesulfonyl)amide (TFSA) anion. This film formation is the result of the oxidative reactivity of the metal in the IL, with the subsequent effect of ultimately protecting the underlying metal from corrosion in aqueous chloride containing solution. Film formation was studied in the IL using an electrochemical droplet cell. It was seen that this film is adherent and subsequently facilitates appreciable protection against corrosion as judged by subsequent electrochemical testing in the form of potentiodynamic polarization and impedance spectroscopy, along with direct observation. The physical film morphology was studied by electron microscopy and focused ion beam.