A Micro-machining system based on electrochemical dissolution of material

Aiming at solving the problem of online fabrication of micro-tool electrode, a micromachining system based on electrochemical dissolution of material was constructed, which consisted of mechanical movement equipment, ultrashort pulse power supply, circulation system of electrolyte, and hall current sensor for detecting the process status. In the micro-ECM system, the micro tool-electrode and the micro-structures of workpiece can be sequentially machined by means of changing the machining condition. Applying the tungsten tool electrode with 8 μm diameter and the ultrashort voltage pulses, the micro-cross with a 30 μm width groove, which had the sharp edge, was obtained. Investigation results show the potential capability of electrochemical micromachining in the manufacture of micro-electromechanical parts.     

Modelling of micro-electrochemical machining parameters used for machining of holes on copper plate

The electrochemical machining is a non-conventional machining process based on the electrolysis principle. It is used to machine various features on conducting engineering materials with the required accuracy and precision. So an attempt has been made to machine micro-holes on a 300 μm thick copper plate as an anode and a hollow stainless steel tool electrode of 250 μm diameter as the cathode. The machining operation is performed on the in-house developed micro-ECM experimental setup with controlled machining parameters voltage, concentration, and duty factor varied in three levels. A full factorial experimental plan is used to study the output responses material removal rate (MRR), radial overcut (ROC), circularity, and taper angle (TA). Later an adaptive neuro-fuzzy inference system (ANFIS) model has been developed and shown the effectiveness of the developed model in the paper. The Sugeno fuzzy model has been used in ANFIS to generate the fuzzy rules required for the model. Out of 27 experiments, 22 machining data are used for training the model, and the remaining 5 machining data are used for testing the developed model. The average error observed between the ANFIS predicted values and experimental values of MRR is 12.56%, circularity is 43.09%, ROC is 13%, and TA is 27.53%, respectively.     

Three dimensional micromachining on aluminum surface by electrochemical wet stamping technique

We proposed an up–down working mode of electrochemical wet stamping technique (EC-WETS) for three dimensional (3D) micromachining on aluminum (Al) surface. 3D microstructures on a Si mold were transferred on to an agarose hydrogel containing 15% NaNO₃, 2% MgF₂, 1% NaOH and 5% glycerin, which acted as the quasi-solid electrolyte for the electrochemical micromachining. The transferred 3D microstructures on agarose hydrogel were then duplicated onto Al surface through anodic dissolution. The micromachining quality was improved by pulse-potential method dramatically with a machining tolerance lower than 200 nm and an average removal rate of 210 nm min^− 1 in the Z direction. This method was proved to be a highly efficient, low cost and green method for 3D micromachining on active metal surface, which would be valuable for the manufacture of microelectromechanical system (MEMS).     

Synthesis of spherical microcapsules by photopolymerization in aerosols

 The preparation of polymer microcapsules of well defined size in the range of 10–50 μm with different shell thickness to core diameter ratios is described. An aerosol of monodisperse droplets of a homogeneous ternary liquid system which contained a hydrophobic component and a hydrophilic component dissolved in a high-volatile mutual solvent, was produced by dispersing with a vibrating-orifice aerosol generator. After the evaporation of the solvent in a nitrogen atmosphere the particles demix and form a two-phase droplet of core-shell type. These droplets were illuminated with UV light and polymerized to highly monodisperse microcapsules with a solid polymer shell and a liquid core. The properties of the resulting particles (size, size distribution, shell thickness, shape and surface characteristics) were investigated by scanning electron microscopy, Raman spectroscopy on single optically levitated particles, and confocal Raman micro spectroscopy. The microcapsules were highly monodisperse and have spherical shape. Received: 24 July 1996 Accepted: 29 August 1996     

Influence of Variant Electrolyte in Electrochemical Micromachining of Micro Holes in SMA Using Taguchi Optimization

Russian Journal of Electrochemistry - Electrochemical micromachining (ECMM) is one of the commercially successful modern machining processes used in various manufacturing industries. Nitinol, a...     

LGS and GaPO4 piezoelectric crystals: New results

Theoretical and experimental results of two interesting piezoelectric crystals for vibrating sensors, the La₅Ga₃SiO₁₄ (also written LGS) and the GaPO₄, are presented. First a comparison of different piezoelectric crystals in terms of quality factor and temperature stability is given and shows the theoretical interest of the GaPO₄ and the LGS isomorphs (LGX). Then an experimental validation has been undertaken: a dedicated decoupling structure allowing high insulation of two flexural modes is described, as well as its micromachining by ultrasonic machining (USM). The experimental measurements of the LGS resonator gave disappointing results with very low measured quality factors of about 10,000 (under vacuum) for a beam working at 10 kHz. On the other hand, the GaPO₄ resonator behaves very well: a quality factor higher than 700,000 (beam frequency 9 kHz) at room temperature and under vacuum has been obtained, as well as a low temperature frequency dependence of ?12 ppm/K, in accordance with the theoretical predictions. The impact of the Au excitation/detection electrodes on the quality factor has also been studied in detail and it clearly explains why the measured quality factors are lower than the thermoelastic limit.     

Physicochemical Modelling of Solid/Liquid Interfacial Phenomena

Summary. The proposed modelling of solid/liquid interfacial phenomena consists in relating the main experimental parameter – contact angle θ for metals or alloys on different substrates to combinations of the interatomic interaction parameters of the phases in contact. Physically, these interatomic interaction parameters are analogous to the electronic density distribution in the first and second coordination spheres of the crystallographic lattice of the component, to the bond length, and to the electrochemical factors. The contact angle θ of some alloys on AlN substrates in the case of non-reactive or reactive wetting is calculated.     

The coupling effect of slow-rate mechanical motion on the confined etching process in electrochemical mechanical micromachining

By introducing the mechanical motion into the confined etchant layer technique (CELT), we have developed a promising ultra-precision machining method, termed as electrochemical mechanical micromachining (ECMM), for producing both regular and irregular three dimensional (3D) microstructures. It was found that there was a dramatic coupling effect between the confined etching process and the slow-rate mechanical motion because of the concentration distribution of electrogenerated etchant caused by the latter. In this article, the coupling effect was investigated systemically by comparing the etchant diffusion, etching depths and profiles in the non-confined and confined machining modes. A two-dimensional (2D) numerical simulation model was proposed to analyze the diffusion variations during the ECMM process, which is well verified by the machining experiments. The results showed that, in the confined machining mode, both the machining resolution and the perpendicularity tolerance of side faces were improved effectively. Furthermore, the theoretical modeling and numerical simulations were proved valuable to optimize the technical parameters of the ECMM process.     

Physicochemical Modelling of Solid/Liquid Interfacial Phenomena

The proposed modelling of solid/liquid interfacial phenomena consists in relating the main experimental parameter – contact angle θ for metals or alloys on different substrates to combinations of the interatomic interaction parameters of the phases in contact. Physically, these interatomic interaction parameters are analogous to the electronic density distribution in the first and second coordination spheres of the crystallographic lattice of the component, to the bond length, and to the electrochemical factors. The contact angle θ of some alloys on AlN substrates in the case of non-reactive or reactive wetting is calculated.     

Liquid–(Solid + Liquid) Transitions in a Two-Component System of (CH 3 )CCl 3 + CCl 4

Liquid–(solid + liquid) transitions are studied in (CH3)CCl3 + CCl4 by using the Landau phenomelogical model. The Gibbs energy is expanded in terms of the orientational disorder (OD) parameters for the transitions of the liquid–(rhombohedral + liquid) and liquid–(face-centered cubic + liquid) in a two component system of (CH3)CCl3 + CCl4. From the Gibbs energy, the phase line equations are derived for the transitions studied and they are fitted to the observed T–X phase diagram of (CH3)CCl3 + CCl4 for the concentration (X) CCl4. Temperature and concentration dependences of the OD parameters (Ψ and η) and the inverse susceptibility ($$\chi_{\psi }^{ - 1}$$ and $$\chi_{\eta }^{ - 1}$$) for the two transitions of interest, are predicted by using the melting curves of (CH3)CCl3 + CCl4 on the basis of the Landau phenomenological model. Our predictions, which can be compared with the experimental data, indicate that the first order transition of the liquid–(solid + liquid), in particular, for (CH3)CCl3 + CCl4 can be described satisfactorily by the Landau mean field model.     

Development of a pressure-driven nanofluidic control system and its application to an enzymatic reaction

A novel air-pressure-based nanofluidic control system was developed and its performance was examined. We found that the flow in a 100 nm scale nanochannel on a chip (called an extended nanospace channel) could be controlled within the pressure range of 0.003–0.4 MPa, flow rate range of 0.16–21.2 pL/min, and residence time range of 24 ms–32.4 s by using the developed nanofluidic control system. Furthermore, we successfully demonstrated an enzyme reaction in which the fluorogenic substrate TokyoGreen-β-galactoside (TG-β-gal) was hydrolyzed to the fluorescein derivative TokyoGreen (TG) and β-galactose by the action of β-galactosidase enzyme as a calalyst in a Y-shaped extended nanospace channel. The parameters for the reaction kinetics, such as K _m, V _max and k _cat, were estimated for the nanofluidic reaction, and these values were compared with the results of bulk and microfluidic reactions. A comparison showed that the enzyme reaction rate in the Y-shaped extended nanospace channel increased by a factor of about two compared with the rates in the bulk and micro spaces. We thought that this nanospatial property resulted from the activated protons of water molecules in the extended nanospace. This assumption was supported by the result that the pH dependence of the maximum enzyme activity in the Y-shaped extended nanospace channel was slightly different from that in the bulk and micro spaces. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Thermogravimetric investigation ofwastes from electrical and electronic equipment (WEEE)

Two components of electronic wastes (sample A – a mixture of three types of printed circuit boards, sample B – a mixture of electronic junctions with metal wires) were investigated using thermogravimetric analysis (TG). Thermogravimetric and derivative thermogravimetric data (TG and DTG) give information on the thermal stability of A and B samples and allows finding the correct conditions for their degradation using pyrolysis in an experimental system, built on the laboratory scale for utilization of hazardous wastes. X-ray fluorescence measurements prove that brominated flame retardant is present in sample A, whilst chlorinated flame retardant is a probable component of sample B. Preliminary liquid chromatography of oil products obtained as a result of thermal waste degradation shows that the hydrocarbons released during pyrolysis could be used as a fuel.     

Chemometrics in the assessment of the sustainable development rule implementation

The sustainable development rule implementation is tested by the application of chemometrics in the field of environmental pollution. A data set consisting of Cd, Pb, Cr, Zn, Cu, Mn, Ni, and Fe content in bottom sediment samples collected in the Odra River (Germany/Poland) is treated using cluster analysis (CA), principal component analysis (PCA), and source apportionment techniques. Cluster analysis clearly shows that pollution on the German bank is higher than on the Polish bank. Two latent factors extracted by PCA explain over 88 % of the total variance of the system, allowing identification of the dominant “semi-natural” and “anthropogenic” pollution sources in the river ecosystem. The complexity of the system is proved by MLR analysis of the absolute principal component scores (APCS). The apportioning clearly shows that Cd, Pb, Cr, Zn and Cu participate in an “anthropogenic” source profile, whereas Fe and Mn are “semi-natural”. Multiple regression analysis indicates that for particular elements not described by the model, the amounts vary from 4.2 % (Mn) to 13.1 % (Cr). The element Ni participates to some extent to each source and, in this way, is neither pure “semi-natural” nor pure “anthropogenic”. Apportioning indicates that the whole heavy metal pollution in the investigated river reach is 12510.45 mg·kg⁻¹. The contribution of pollutants originating from “anthropogenic sources” is 9.04 % and from “semi-natural” sources is 86.53 %.     

Determination of tributyltin in marine sediment: Comité Consultatif pour la Quantité de Matière (CCQM) pilot study P-18 international intercomparison

The capabilities of National Metrology Institutes (NMIs—those which are members of the Comité Consultatif pour la Quantité de Matière (CCQM)of the CIPM) and selected outside "expert" laboratories to quantitate (C₄H₉)₃Sn⁺ (TBT) in a prepared marine sediment were assessed. This exercise was sanctioned by the 7th CCQM meeting, April 4–6, 2001, as an activity of the Inorganic Analysis Working Group and was jointly piloted by the Institute for National Measurement Standards of the National Research Council of Canada (NRC) and the Laboratory of the Government Chemist (LGC), UK. A total of 11 laboratories submitted results (7 NMIs, and 4 external labs). Two external laboratories utilized a standard calibration approach based on a natural abundance TBT standard, whereas all NMIs relied upon isotope dilution mass spectrometry for quantitation. For this purpose, a species specific ¹¹⁷Sn-enriched TBT standard was supplied by the LGC. No sample preparation methodology was prescribed by the piloting laboratories and, by consequence, a variety of approaches was adopted by the participants, including mechanical shaking, sonication, accelerated solvent extraction, microwave assisted extraction and heating in combination with Grignard derivatization, ethylation and direct sampling. Detection techniques included ICP–MS (with GC and HPLC sample introduction), GC–MS, GC–AED and GC–FPD. Recovery of TBT from a control standard (NRCC CRM PACS-2 marine sediment) averaged 93.5±2.4% (n=14). Results for the pilot material averaged 0.680±0.015 µmol kg^–1 (n=14; 80.7±1.8 µg kg^–1) with a median value of 0.676 µmol kg^–1. Overall, performance was substantially better than state-of-the-art expectations and the satisfactory agreement amongst participants permitted scheduling of a follow-up Key comparison for TBT (K-28), a Pilot intercomparison for DBT (P-43), and certification of the test sediment for TBT content and its release as a new Certified Reference Material (HIPA-1) with a TBT content of 0.679±0.089 µmol kg^–1 (expanded uncertainty, k=2, as Sn) (80.5±10.6 µg kg^–1).Electronic Supplementary Material Supplementary material is available in the online version of this article at .     

Micro fluorescent analysis system integrating GaN-light-emitting-diode on a silicon platform

A micro fluorescent analysis system is proposed using silicon micromachining. GaN blue light-emitting diode (LED) monolithically integrated on a silicon substrate is used as a light source for the fluorescent analysis system. The blue light suits the excitation of several dyes used commonly in fluorescent analysis. Silicon photodiode (Si-PD) that matches the visible and near infrared fluorescent wavelengths of dyes is integrated on a silicon substrate. Polydimethylsiloxane (PDMS) micro-channels are also stacked for flowing dye-sensitized liquid. Therefore, the proposed system is an integrated system that can be composed on a silicon platform, i.e. a bottom layer of Si-PD, a middle layer of GaN-LED on silicon substrate and a top layer of micro PDMS channel. An aperture is opened into the GaN-LED layer by deep reactive ion etching to create a ring-shaped GaN-LED and a through-hole for detection. The light from the ring-shaped GaN-LED in the middle layer excites the dye-sensitized liquid in the top micro-channel layer. The fluorescence emitted from dye is detected by the Si-PD on the bottom layer at an angle larger than 90 degrees from the direction of excitation. Therefore, the detection optics consist basically of a dark-field illumination optical system. In order to evaluate the performance of the integrated system, fluorescence of fluorescein isothiocyanate (FITC) solution flowing in the micro channel is measured. From the measurement, the noise, sensitivity and limit of detection in the fabricated system are evaluated for FITC dye to be 0.57 pA, 1.21 pA μM(-1) and 469 nM, respectively. From these results, a compact fluorescence analysis system is demonstrated.     

Development of an on-line immobilized-enzyme reversed-phase HPLC method for protein digestion and peptide separation

This paper describes use of a novel glass bead-based immobilized-enzyme micro column for simple and swift on-line protein digestion then peptide separation by reversed-phase HPLC. The inexpensive and easily made immobilized-enzyme micro column was prepared from aminopropyl controlled-pore glass that was reacted first with glutaraldehyde then with trypsin in the presence of phosphate buffer. Tryptic digestion of bovine serum albumin (BSA) was achieved simply by passing pretreated protein solution through the laboratory made immobilized-trypsin column; the tryptic fragments were then separated by reversed-phase HPLC. The peptide separation was found to be identical to separation of a sample which had undergone conventional enzymatic protein digestion in solution. Digestion of BSA by the immobilized-trypsin column decreased with increasing flow rate of the solution through the column, and 1.0 μL min⁻¹ was found to be the optimum flow rate for on-line protein digestion with our system. It was also found that the sample required pretreatment with urea before injection, because of a change in the properties of the protein in the presence of urea, and the immobilized-trypsin column lost its function in the presence of acetonitrile. This on-line proteomics system enables simple and rapid protein digestion and was successfully applied to partially micro two-dimensional (2D) chromatographic separation of proteins.     

Development of a micro-mixer-settler for nuclear solvent extraction

Nuclear solvent extraction was traditionally performed with packed columns, pulse columns, mixer-settlers and centrifugal extractors. However for rapid separations at micro-flow level, micro mixer-settlers were desired and in the past, few of them were actually designed and operated in nuclear solvent extraction research. In the current era of micro-reactor and microchannel devices, there is a renewed interest for micro-mixer-settlers for costly solvents and specialty solutes where small flow-rate is not an issue. In this article, development of a simple but effective micro-mixer-settler for nuclear solvent extraction is reported. The developed unit was tested with 30% TBP/n-dodecane/nitric acid system and in both the regimes of mass transfer c → d (mass transfer from continuous phase to dispersed phase, also written as c → d) and d → c (mass transfer from dispersed phase to continuous phase, also written as d → c) nearly 100% efficiency was observed in extraction as well as stripping modes of operation.     

Application of temperature-controlled micro planar chromatography for separation and quantification of testosterone and its derivatives

Temperature-controlled micro thin-layer chromatography (TLC) was applied for separation and quantification studies of testosterone and its derivatives including methyltestosterone, testosterone propionate, isobutyrate, phenylpropionate, isocaproate, enanthate and caprate. Chromatographic studies were performed on silica-, octadecylsilica- and aluminum-coated plates working inside a small thermostated horizontal chamber unit allowing one-dimensional and two-dimensional developing modes with an elution distance of 45 mm. Retention properties of steroids were investigated across a whole range of binary mixtures such as methanol/water, acetonitrile/water, methanol/dichloromethane and acetone/hexane (0–100% v/v). Moreover, the effect of temperature ranging from −20 to +60 °C under saturated and unsaturated chamber conditions was also investigated. Our results revealed that depending on the mobile phase polarity the separation system based on the low carbon load wettable with water RP18W plates may work as a normal-phase (NP) or reversed-phase (RP) chromatographic system. It has been also demonstrated that micro TLC equipment can be applied as a fast retention screening device as well as simple and robust quantitative tool for determination of testosterone residue containing testosterone derivatives in complex samples. Figure 2D micro TLC separation and quantitative analysis of testosterone and its derivatives Presented at the 11th International Conference on Chemistry and the Environment, 9–12 September 2007, Torun, Poland     

Precision removal of ITO layer using plate-form tool design

An ITO layer is produced using semiconductor techniques, although the defect rate during production is easily seen. Current work presents a new modus of electrochemical machining using a ‘design recycle’ system offering faster performance in removing the color filter surface’s ITO layer. Higher electrical current is not required when an effective feeding electrode is used to reduce the response area. Through establishing an ultra-precise recycling process to remove the thin film microstructure, this helps the semiconductor optoelectronic industry to reduce both production costs and pollution. The design features of the removal processes for a thin film and the tool design of plate-form electrode are of major interest. In the current experiment, the author utilizes a 5th Generation TFT-LCD. The design of tool electrodes is used with continuous and pulsed direct current in the electrochemical machining experiment. High rotational speed of the tool electrodes and high flow velocity of the electrolyte elevates the discharge mobility and improves the removal effect. Pulsed direct current can improve the effect of dregs discharge and is advantageous to associate with the fast feed rate of the workpiece. A color filter with a fast feed rate is combined with enough electric power to provide highly effective removal. A smaller end radius and a thin plate-form positive-electrode provide a larger discharge space and better removal effect. A precision recycling process is presented using an effective plate-form positive-electrode in electrochemical machining. It only needs a short period of time to remove the ITO layer easily and cleanly.