Low temperature carbon nanotube and hexagonal diamond deposition with photo-enhanced chemical vapor deposition

Deposition of carbon nanotube and hexagonal diamond thin films at low substrate temperature with photo-enhanced chemical vapor deposition is described here. Extensive experimentation is conducted to optimize the catalyst layer utilized for deposition by varying Al/Ni/Al metal layer thicknesses on SiO₂ coated Si substrates. The coated substrates are annealed to transform the thin metal layers into nanoparticles. Suitable catalyst layer thicknesses obtained are 3/2/3, 5/1/5 and 5/3/5 nm for Al/Ni/Al sandwich metal layers. Suitable annealing conditions are in the range of 350–450 °C for substrate temperature and from 0.22 to 10 Torr for chamber pressure in ammonia ambient for 25 min. Carbon tetrachloride (CCl₄) is used as a carbon precursor in this work. Argon to CCl₄ flow ratio is varied in 1.5–19 range, chamber pressure is varied in 3–10 Torr range, and the substrate temperature is varied in 350–450 °C range. Carbon nanotubes (CNT) growth is observed at lower chamber pressure, lower partial pressure of CCl₄, lower substrate temperature and for thin Ni catalyst layer. The optimal CNT deposition condition observed is 5 Torr total chamber pressure, 9:1 partial pressure ratio of Ar to CCl₄, 400 °C substrate temperature and 5/1/5 nm thick Al/Ni/Al catalyst layers. The hexagonal diamond deposition is observed at a higher chamber pressure, higher partial pressure of CCl₄, higher substrate temperature and for a thicker Ni catalyst layer. The optimal condition for hexagonal diamond deposition observed is 10 Torr total chamber pressure, 7:3 partial pressure ratio of Ar to CCl₄, 450 °C substrate temperature and 5/3/5 nm thick Al/Ni/Al catalyst sandwich layers.     

The design and fabrication of a low-field NMR probe based on a multilayer planar microcoil

The nuclear magnetic resonance (NMR) probe has great influence on signal transmission and reception in NMR technology applications. In this paper, we present a design, fabrication, and test of an NMR probe comprised of a multilayer planar microcoil with a polydimethylsiloxane (PDMS) microchannel. First, geometric parameters of the probe are determined through theoretical analysis. Second, based on a glass substrate, the multilayer planar microcoil is manufactured using repeated photolithography and electroplating processes. During the fabrication process, the polyimide layer is used to package the coil, and the PDMS interlayer is used to adjust the distance from centerlines between the coil and the sample chamber. Third, the resistance and the quality factor of the coil are found to be 1.2158 Ω and 7.217, respectively, at a Larmor frequency of 28.1 MHz. Finally, the NMR probe is tested in an NMR experiment. The transverse relaxation time T₂ for the solid PDMS is 20.6 ± 0.4 ms, which is in agreement with 21.1 ± 0.2 ms obtained by a Bruker Minispec MQ60. Results show that the design and fabrication of this NMR probe are feasible for time-domain NMR applications.     

Electrical and morphological characterization of platinum thin-films with various adhesion layers for high temperature applications

In this paper we report on the morphological and electrical properties of platinum (Pt) thin-films with Titanium (Ti) and, alternatively, Titanium dioxide (TiO₂) as adhesion layers for high temperature applications. All films were sputter deposited on silicon substrates and afterwards annealed in air up to 800 °C. The results show that Ti diffuses into Pt grain boundaries forming oxide precipitates (TiO_x) in the Pt grain boundaries. The resistivity of Pt/Ti thin-films increased continuously with annealing temperature up to 500 °C and decreases again continuously above 500 °C. In contrast, TiO₂ demonstrates a dense stable oxide layer after annealing. Pt/TiO₂ thin-films show a continuous decrease in the sheet resistance with increasing the annealing temperature. Accordingly, TiO₂ thin-film is the preferable adhesive layer for Pt over Ti thin-films for high temperature applications.

     

Liquid metal microcoils for sensing and actuation in lab-on-a-chip applications

The use of metals and alloys with melting point near room temperature, called here as liquid metals, allows the integration of complex three-dimensional metallic micro structures in lab-on-chip devices. The process involves the injection molten liquid metal into microchannels and subsequent solidification at room temperature. The paper reports a technique for the fabrication of three-dimensional multilayer liquid-metal microcoils by lamination of dry adhesive films. The adhesive-based liquid metal microcoil could be used for magnetic resonance relaxometry (MRR) measurement in a lab-on-a-chip platform. Not only that the coil has a low direct-current resistance, it also has a high quality factor. In this paper, we investigate the sensing and actuating capabilities of the liquid metal microcoil. The sensing capability of the microcoil is demonstrated with the coil working as a blood hematocrit level sensor. In a MRR measurement, the transverse relaxation rate of the blood sample increases quadratically with the hematocrit level due to higher magnetic susceptibility. Furthermore, a vibrating adhesive membrane with the embedded coil was realized for electromagnetic actuation. A maximum deflection of approximately 50 μ at a low resonance frequency of 15 Hz can be achieved with a maximum driving current of 300 mA.     

Studies on contact resistance in graphene based devices

Contact resistance is an important limiting factor for the on-state current of graphene based devices. In this paper, both transmission line method and four-probe method are applied to measure the contact resistance in graphene-metal (Cr/Au and Ti/Au) interface. The calculated contact resistivity values by both methods are concentrated at 10⁴ Ωμm². These two methods are compared and four-probe method showed higher stability. At last, the graphene-Ti/Au devices are annealed at 400 °C with argon and hydrogen gas flow. After annealing, the contact resistivity values are reduced to 10³ Ωμm².     

Viable cell handling with high aspect ratio polymer chopstick gripper mounted on a nano precision manipulator

This paper presents the development of an optimized contact technique for viable cell manipulation utilizing a high aspect ratio polymer chopstick gripper. The gripper consists of a 2 μm thick metal heater layer and a 60 μm thick SU-8 layer and is fabricated by a typical UV-LIGA process using SiO₂ as sacrificial layer. The grippers were completely released, de-tethered and assembled as end-effectors on to a nano precision manipulator to perform cell manipulation. Successful pick-and-place of a suspended normal rat kidney cell in phosphate buffered saline solution was demonstrated. The major cell-damage mechanisms associated with contact techniques were identified and alleviated by optimizing the handling force and operating temperature of the polymer gripper. The viability of cells handled with this optimized contact technique was demonstrated by labeling cells with a fluorescent dye. The developed technique will enable incorporation of simple, viable, and repeatable cell handling capabilities into the generic micromanipulators used in the biological laboratories.     

Annealing temperature effect on structural,optical, morphological and electrical properties of CdS/Si(100) nanostructures

CdS nanostructures have grown on p-type silicon (Si) (100) substrates using sol–gel method. The crystalline quality, surface morphology, optical and electrical properties of the deposited CdS nanostructures have been characterized and analyzed using atomic force microscopy, scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, differential thermal analysis, UV–vis spectroscopy and electrical characterization, respectively. The effect of annealing temperature in the range 200–600 °C on the structural, morphological, optical and electrical properties has been elaborated. The XRD analysis shows that the crystalline quality can be improved by increasing the temperature to 400 °C, but further increase to 600 °C leads to degradation of crystalline quality. The bulk modulus is calculated and showed good agreement with experimental and theoretical results. The optical properties of absorption, reflection, energy band gap and extinction coefficient are obtained by UV–vis spectroscopy. The calculated refractive index and optical dielectric constant have shown good agreement with other results. The electrical and thermal properties are studied for antireflection coating applications.     

Modeling of Trivalent Chromium Sorption onto Commercial Resins by Artificial Neural Network

In this research, artificial neural network (ANN) model having three layers was developed for precise estimation of Cr(III) sorption rate varying from 17% to 99% by commercial resins as a result of obtaining 38 experimental data. ANN was trained by using the data of sorption process obtained at different pH (2–7) values with Amberjet 1200H and Diaion CR11 amount (0.01–0.1 g) dosage, initial metal concentration (4.6–31.7 ppm), contact time (5–240 min), and a temperature of 25°C. A feed-forward back propagation network type with one hidden layer, different algorithm (transcg, trainlm, traingdm, traincgp, and trainrp), different transfer function (logsig, tansig, and purelin) for hidden layer and purelin transfer function for output layer were used, respectively. Each model trained for cross-validation was compared with the data that were not used. The trainlm algorithm and purelin transfer functions with five neurons were well fitted to training data and cross-validation. After the best suitable coefficient of determination and mean squared error values were found in the current network, optimal result was searched by changing the number of neurons range from 1 to 20 in the current network hidden layer.     

Manufacture of microfluidic glass chips by deep plasma etching, femtosecond laser ablation, and anodic bonding

Two dry subtractive techniques for the fabrication of microchannels in borosilicate glass were investigated, plasma etching and laser ablation. Inductively coupled plasma reactive ion etching was carried out in a fluorine plasma (C₄F₈/O₂) using an electroplated Ni mask. Depth up to 100 μm with a profile angle of 83°–88° and a smooth bottom of the etched structure (Ra below 3 nm) were achieved at an etch rate of 0.9 μm/min. An ultrashort pulse Ti:sapphire laser operating at the wavelength of 800 nm and 5 kHz repetition rate was used for micromachining. Channels of 100 μm width and 140 μm height with a profile angle of 80–85° were obtained in 3 min using an average power of 160 mW and a pulse duration of 120 fs. A novel process for glass–glass anodic bonding using a conductive interlayer of Si/Al/Si has been developed to seal microfluidic components with good optical transparency using a relatively low temperature (350°C).     

Low power highly sensitive platform for gas sensing application

This paper reports a low power miniaturized MEMS based integrated gas sensor with 36.84 % sensitivity (ΔR/R₀) for as low as 4 ppm (NH₃) gas concentration. Micro-heater based gas sensor device presented here consumes very low power (360 °C at 98 mW/mm²) with platinum (Pt) micro-heater. Low powered micro-heater is an essential component of the metal oxide based gas sensors which are portable and battery operated. These micro-heaters usually cover less than 5 % of the gas sensor chip area but they need to be thermally isolated from substrate, to reduce thermal losses. This paper elaborates on design aspects of micro fabricated low power gas sensor which includes ‘membrane design’ below the microheater; the ‘cavity-to-active area ratio’; effect of silicon thickness below the silicon dioxide membrane; etc. using FEM simulations and experimentation. The key issues pertaining to process modules like fragile wafer handling after bulk micro-machining; lift-off of platinum and sensing films for the realization of heater, inter-digitated-electrodes (IDE) and sensing film are dealt with in detail. Low power platinum microheater achieving 700 °C at 267 mW/mm² are fabricated. Temperature calculations are based on experimentally calculated thermal coefficient of resistance (TCR) and IR imaging. Temperature uniformity and localized heating is verified with infrared imaging. Reliability tests of the heater device show their ruggedness and repeatability. Stable heater temperature with standard deviation (σ) of 0.015 obtained during continuous powering for an hour. Cyclic ON–OFF test on the device indicate the ruggedness of the micro-heater. High sensitivity of the device for was observed for ammonia (NH₃), resulting in 40 % response for ~4 ppm gas concentration at 230 °C operating temperature.     

A low-power,micromachined, double spiral hotplate for MEMS gas sensors

This paper presents the design, fabrication and reliability testing of a double spiral platinum-based MEMS hotplate for gas sensing applications. The structure of MEMS hotplate consists of a 0.7 µm-thick thermally grown SiO₂ membrane of size 120 µm × 120 µm over which a double spiral platinum resistor is laid out. The hotplate membrane is supported by its four arms connected to the Si-substrate. The design and simulation of the hotplate structure was carried out using MEMS-CAD Tool COVENTORWARE. Based on the design, a double spiral platinum resistor of 103 Ω is fabricated on SiO₂ membrane using lift-off technique. The platinum deposition is carried out using DC sputtering technique. Bulk micromachining of Si is done from front side of the structure to create the suspended SiO₂ membrane. The temperature coefficient of resistance (TCR) of platinum is measured and found to be 2.19 × 10^?3/ °C. The TCR value is used for temperature estimation of the hotplate. The test results show that the microhotplate consumes only 20 mW power when heated up to 500 °C. For reliability testing of fabricated structure, the hotplate is continuously operated at 300 °C for 1.8 h. Also, it can sustain at least 61 cycles pulse-mode operation at 530 °C with ultra-low resistance and temperature drifts. The structure can sustain a maximum temperature and current of 611 °C and 11.55 mA respectively without any damage.     

Simple fabrication of an uncooled Al/SiO2 microcantilever IR detector based on bulk micromachining

A simple microfabrication process to make an uncooled aluminum/silicon dioxide bi-material microcantilever infrared (IR) detector using silicon bulk micromachining technology is presented in this work. This detector is based on high banding of the microcantilever due to the large dissimilar in thermal expansion coefficients between the two materials. It consists of a 1 μm SiO₂ layer deposited by 200 nm thin Al layer. Since no sacrificial layer is used in this process, complexity related to releasing sacrificial layer is avoided. Moreover Al is protected in Si etchant using dual-doped tetramethyl ammonium hydroxide. The other advantage of this process is that only three masks are used with four photolithography process. Thermal and thermal mechanical behaviors of this structure are obtained using finite element analysis, and the maximum temperature and displacement at the end of cantilever at 100 pW/μm² absorbed IR power density on top surface are 7.82°K and 1.924 μm, respectively.     

Effects of ITO film annealing temperature on hybrid solar cell performance

The effects of indium tin oxide (ITO) film annealing temperature on the performance of organic solar cells are investigated. The roughness of the ITO film surface morphology increased with increasing annealing temperature. The optical penetration and rate of exciton generation both increased with increasing ITO film annealing temperature, enhancing the short-circuit current density. The maximum efficiency (2.62 %) was obtained with an annealing temperature of about 500 °C. The incident-photon-to-current efficiency value for a hybrid photovoltaic device with an ITO film annealed temperature at 500 °C was 45 % at 475 nm.     

Development of thin film based flexible current clamp sensor using screen-printed coil

This paper reports a novel flexible current clamp sensor with 480 turns silver paste coil (line/space = 50/50 μm) formed by through-holes and screen-printing technologies. Using screen-printing techniques, fine stripe patterns could be formed on a 50-mm-long and 10-mm-wide polyimide film in few seconds. Coil resistance between their contact pads is about 2.3 kΩ. When the value of a primary current was 20 A, the output voltage was 22.6 mV. Furthermore, the output voltage changed linearly with the changing of the primary current in the 0–20 A range. The sensor is developed using only coating, through-holes laser drilling, and screen-printing technologies. Therefore it can be fabricated by a reel-to-reel continuous film processing system.     

Properties of Sc<Subscript>x</Subscript>Al<Subscript>1-x</Subscript>N (x = 0.27) thin films on sapphire and silicon substrates upon high temperature loading

Scandium Aluminum Nitride thin films (Sc_xAl_1-xN) are attracting more and more attention for micro-electromechanical systems (MEMS) because of significantly increased piezoelectric constants compared to pure AlN. This work provides a comprehensive study of thermal annealing effects on Sc_xAl_1-xN (x = 27 %) films synthesized via DC magnetron sputter deposition at nominally unheated Silicon and Sapphire substrates. Compared to the “as deposited” state increasing c-axis orientation and crystalline quality upon annealing up to 1000 °C of films with mixed crystallographic orientation is observed via X-ray diffraction and transmission electron microscopy based analyses. Also the piezoelectric coefficient d ₃₃ of Sc_xAl_1-xN on Si shows increasing values at enhanced annealing temperatures. However, the improved piezoelectric properties are accompanied by both increased leakage currents and loss tangent values.     

Physiological strain of next generation combat uniforms with chemical and biological protection: importance of clothing vents

This study examined whether vents in the arms, legs and chest of new protective assault uniforms (PTAU) reduced heat strain at 35°C during a low dressed state (DS_low), and subsequently improved tolerance time (TT) after transitioning to DS_high compared with the battle dress uniform and overgarment (BDU+O). Small but significant reductions in rectal temperature (T _re), heart rate and vapour pressures over the thigh and shin were observed during DS_low with vents open (37.9 ± 0.2°C, 120 ± 10 b/min, 3.7 ± 0.4 and 3.5 ± 1.0 kPa) versus closed (38.0 ± 0.1°C, 127 ± 5 b/min, 4.3 ± 0.3 and 4.6 ± 0.5 kPa). During DS_high T _re was reduced and TT increased significantly with the PTAUs (1.1 ± 0.2°C/h and 46 ± 24 min) versus BDU+O (1.6 ± 0.2°C/h and 33 ± 16 min). The vents marginally reduced heat strain during DS_low and extended TT during DS_high compared with BDU+O.

Practitioner Summary: Clothing vents in chemical and biological protective uniforms can assist with heat transfer in situations where the uniforms must be worn for extended periods prior to exposure to a hazardous condition. Once the vents are closed, exposure time is increased and the increase in body temperature reduced.     

Device characteristics for Pt–Ti–O gate Si–MISFETs hydrogen gas sensors

A novel Pt–Ti–O-gate Si–metal–insulator–semiconductor field-effect transistor (MISFET) hydrogen gas sensor has been proposed by Usagawa and Kikuchi (2010) [1]. The sensors consist of unique gate structures composed of Ti and oxygen accumulated regions around Pt grains on top of a novel mixing layer of nanocrystalline TiO_x and superheavily oxygen-doped amorphous Ti formed on SiO₂/Si substrates. The optimum Pt/Ti thickness and annealing conditions for most hydrogen safety monitoring sensor systems are obtained by annealing Pt(15 nm)/Ti(5 nm)-gate Si–MOS structures in air around 400 °C for 2 h. One of the advantages of the Pt–Ti–O-gate Si–MISFETs after 10 min of air-diluted 1000-ppm hydrogen exposure at 115 °C are reproducible and uniform threshold voltage of V_th in addition to large sensing amplitudes at a practically important hydrogen concentration range between 100 ppm and 1%. The analysis of device characteristics of the Pt–Ti–O-gate Si–MISFETs hydrogen sensors concludes that the oxidation process of the Ti layer is consistently explained by an oxidation model that the oxygen invasion into Ti layer comes from open air through Pt grain boundaries and at the same time Ti will evacuate into the Pt surface through Pt grain boundaries. During the course of this process, the invading oxygen will be balanced with the evacuating Ti so that the Ti layer keeps nearly the same thickness with the as grown states. Ti and oxygen will remains around Pt grains named Ti and oxygen merged corridors.     

Stable electrical,morphological and optical properties of titanium dioxide nanoparticles affected by annealing temperature

Different TiO₂ synthesization processes give different properties. Most of researches in material studies only focus on the morphological and optical properties of TiO₂ while lacking in the effort of achieving stable electrical properties of the material. In engineering, stable electrical properties are vital in order to develop a device. Moreover, current technology needs more nanostructure application to enhance the performance of devices. In this paper, TiO₂ nanoparticle was synthesized by sol–gel method using 1:0.1:9 ratios of titanium isopropoxide:acetic acid:ethanol, respectively. This synthesized TiO₂ was able to respond in extremely small and consistent electrical reading (nanoampere). This metal oxide is good enough to be used as a material to develop ultra-high sensitive biosensor. Annealing process on the TiO₂ film was able to improve its’ electrical conductivity. The three layers TiO₂ coating were annealed at 400, 500, 600 and 700 °C and the surface morphologies, structural also electro-optical properties were studied using FESEM, XRD, UV–Vis and Keithley 6485 picoammeter. The XRD pattern shows the presence of stable anatase and rutile structures even at low temperature, whereas FESEM shows that annealing temperature affects the particle size. The optical band gap of TiO₂ thin films decreases from 3.74 to 3.34 eV as the annealing temperature increases. The current-to-voltage characteristics show that the conductivity decreases as the annealing temperature varies from 400to 700 °C. The output measurements indicated an improvement in electrical properties with annealing temperature.

     

John G. Fox (1931-2004)

The effectiveness of intermittent, microclimate cooling for men who worked in US Army chemical protective clothing (modified mission-oriented protective posture level 3; MOPP 3) was examined. The hypothesis was that intermittent cooling on a 2 min on–off schedule using a liquid cooling garment (LCG) covering 72% of the body surface area would reduce heat strain comparably to constant cooling. Four male subjects completed three experiments at 30°C, 30% relative humidity wearing the LCG under the MOPP 3 during 80 min of treadmill walking at 224 ± 5 W · m^?2. Water temperature to the LCG was held constant at 21°C. The experiments were; 1) constant cooling (CC); 2) intermittent cooling at 2-min intervals (IC); 3) no cooling (NC). Core temperature increased (1.6 ± 0.2°C) in NC, which was greater than IC (0.5 ± 0.2°C) and CC (0.5 ± 0.3°C) ( p < 0.05). Mean skin temperature was higher during NC (36.1 ± 0.4°C) than IC (33.7 ± 0.6°C) and CC (32.6 ± 0.6°C) and mean skin temperature was higher during IC than CC ( p < 0.05). Mean heart rate during NC (139 ± 9 b · min^?1) was greater than IC (110 ± 10 b · min^?1) and CC (107 ± 9 b · min^?1) ( p < 0.05). Cooling by conduction (K) during NC (94 ± 4 W · m^?2) was lower than IC (142 ± 7 W · m^?2) and CC (146 ± 4 W · m^?2) ( p < 0.05). These findings suggest that IC provided a favourable skin to LCG gradient for heat dissipation by conduction and reduced heat strain comparable to CC during exercise-heat stress in chemical protective clothing.     

Realization of an adaptive voltage driver for voice coil motor

In this paper we describe a head servo-positioning system for hard disk drives (HDDs), in which the usual current command for the voice coil motor has been replaced by a simpler voltage command. This solution has proven advantages in terms of cost, since the voltage driver does not require any resistive shunt for current measurement and phase-shaping passive networks for the current controller. Also, it requires a lower pin count and can be easily implemented with a PWM power stage. The voltage driver consists of a voltage-controlled power stage, with a pre-filter placed at its input, plus a back e.m.f. feed-forward compensator. The role of the pre-filter is to provide a transfer function between input signal and VCM current as close as possible to that of a standard current loop, so providing a one-to-one replacement to standard current drivers. To achieve this, it can be shown that the filter must cancel out the low-frequency pole of the VCM, located in a position which depends on the electrical impedance of the VCM itself. This, however, may change by ±30% during HDD operations, due to self-heating and consequent variation of the VCM resistance. Such variation may lead to an unsatisfactory performance of the voltage driver, so an adaptation mechanism, capable of tracking variations of VCM coil resistance, must be set up. This paper presents an on-line estimation procedure, based on an extended Kalman filter (EKF), capable of estimating the VCM coil resistance with a high degree of accuracy. EKF, however, usually brings a high computational load, making it unsuitable for real-time, low-cost embedded applications. The paper presents two reduced-order model of the VCM, for which the EKF can be implemented with 30 and 50% less computational effort, respectively, while maintaining a good estimate of the VCM coil resistance. The paper reports experimental results of VCM resistance estimation, obtained with the proposed algorithm, running in 30 μS on a 25 MHz, fixed-point DSP. Also, the on-line estimation is used to adapt the pre-filter. Experimental results show that the servo performance with adaptive voltage driver is not affected by resistance variation and equivalent to that of the standard current driver.