Determination of dielectric constant and loss of high-K thin films in the microwave frequencies

A method to determine the dielectric constant and loss of high-K thin film dielectrics in the microwave frequency region using the extended cavity perturbation technique is presented. The feasibility of the technique is demonstrated by the determination of the dielectric constant and loss for reactively sputtered TiO₂ thin films on borosilicate glass substrates. The dielectric constant and loss is measured at 8.98, 9.96 and 10.97 GHz using a TE_10n rectangular cavity. Using this technique, the dielectric properties of TiO₂ films deposited under varying oxygen percentage in the sputtering atmosphere from 20% to 100% were measured. The dielectric constant and loss are found to be dependent on both the oxygen partial pressure as well as frequency of measurement. The film deposited at 50% of oxygen had a higher dielectric constant, ε_r = 44.35 at 8.98 GHz, where as the film deposited at 100% oxygen showed the lowest value of dielectric constant, ε_r = 21.36 at 10.97 GHz. The dielectric loss tangent varied from 0.004 to 0.019 depending on frequency and oxygen partial pressure. However this technique is applicable only for thin films coated on low K dielectric substrates.     

Analysis of composition dependence of some thermal transport properties in glassy Se80−xTe20Snx (0 ⩽ x ⩽ 10) alloys using transient plane source measurements

In the present work, we have studied simultaneous measurements of thermal transport properties (effective thermal conductivity, diffusivity, specific heat per unit volume, thermal inertia I_T) of glassy Se_80−xTe₂₀Sn_x (0 ? x ? 10) system using their twin pellets. The glassy system is prepared under a load of 5 tons and measurements have been made at room temperature using Transient Plane Source (TPS) technique. The composition dependence of the thermal transport properties of given glassy system is also discussed.     

Passive control of circular cylinder wake in shallow flow

The control of vortex shedding of a circular cylinder in shallow water using a splitter plate located in the downstream of the circular cylinder was studied by employing particle image velocimetry (PIV) technique. Experiments were carried out in a water channel having a test section of 8000 mm × 1000 mm × 750 mm dimensions at a Reynolds number of 6250. The length of the splitter plate (L) was varied within the range of 0.5 ? L/D ? 2 with an increment of 0.5. The plate was submerged into water at different height ratios (h_p/h_w) such as 0.25, 0.5, 0.75 and 1.0. Mean velocity vector field, corresponding vorticity contours, streamline topologies and turbulent quantities were calculated using 300 instantaneous velocity vector field measured by PIV. As the ratio of h_p/h_w increases, the effect of the splitter plate on the suppression of the vortex shedding increases. Flow characteristics and examination of spectra indicate that Karman vortex shedding is attenuated pronouncedly for the cases of L/D ? 1 and h_p/h_w ? 0.75. The transverse Reynolds normal stress is more effective on the attenuation of turbulent kinetic energy than the streamwise Reynolds normal stress. The value of peak transverse Reynolds normal stress is reduced to 90% of that of the bare cylinder at most.     

Grain boundary enrichment in the FePt polymorphic A1 to L10 phase transformation

A series of Fe_54±1Pt_46±1 thin films have been sputter-deposited and annealed at various times and temperatures to facilitate the A1 to L1₀ polymorphic phase transformation. The annealing times span one minute to tens of minutes over temperatures of 300–800 °C. The films were characterized by X-ray and electron diffraction and atom probe tomography. This time–temperature regime provides ‘snap-shots’ into the compositional segregation evolution at the grain boundaries during the polymorphic phase transformation. The as-deposited A1 phase showed a preferential segregation of Pt to the grain boundaries. The reduction of Pt enrichment at the boundaries was observed for all L1₀ ordered films.     

High load AFM friction and wear experiments on V2O5 thin films

High load friction and wear experiments by means of atomic force microscopy were carried out at the surface of highly (0 0 1) oriented vanadium oxide V₂O₅ thin films deposited on silicon by reactive magnetron sputtering. Microscopic friction coefficient was estimated for wide range of loads. The nature of surface wear due to multiple, high load scanning is presented and discussed.     

Column-by-column compositional mapping by Z-contrast imaging

A phenomenological method is developed to determine the composition of materials, with atomic column resolution, by analysis of integrated intensities of aberration-corrected Z-contrast scanning transmission electron microscopy images. The method is exemplified for InAs_xP_1−x alloys using epitaxial thin films with calibrated compositions as standards. Using this approach we have determined the composition of the two-dimensional wetting layer formed between self-assembled InAs quantum wires on InP(0 0 1) substrates.     

Characterization and mechanical/tribological properties of nano Au-TiO2 composite thin films prepared by a sol-gel process

Nano Au-TiO₂ composite thin films on Si(1 0 0) and glass substrates were successfully prepared with a facile sol-gel process followed by sintering. The morphology and mircostructure of the films were investigated via X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The Au particles, of diameter 14-22 nm depending on the sintering temperatures used, were found to be well dispersed in the TiO₂ matrix, with a small amount of the particles escaped from the film. The surfaces of the films were uniform, compact and crack-free. Hardness and elastic modulus of the films were measured by using the nanoindentation technique. Friction and wear properties were investigated by using a one-way reciprocating tribometer. It was found that the highest hardness and elastic modulus values were obtained for the films prepared with 500 °C sintering temperature. The films displayed superior antiwear and friction reduction performances in sliding against an AISI 52100 steel ball. With 5.0 mol% Au, the friction coefficient was only 0.09-0.10 and the wear life was more than 2000 sliding cycles. The friction coefficient and wear life decreased with increasing sliding speed and load. The failure mechanism of the Au-TiO₂ films was identified to be light scuffing and abrasion. Those films can be potentially applied as ultra-thin lubricating coatings.     

Electrostatic force microscopy study on the domain switching properties of the Pb(Zr0.2Ti0.8)O3 thin films with different crystallographic orientations for the probe-based data storage

The domain switching properties of the ferroelectric Pb(Zr_0.2Ti_0.8)O₃ (PZT) thin films with two types of crystallographic orientations were investigated by electrostatic force microscopy (EFM). The crystallographic orientations of the PZT thin films were random on the (1 1 1)Pt/MgO(1 0 0) and c-axis preferred on the (1 0 0)Pt/MgO(1 0 0), respectively. When dc bias was applied to the films for writing in micro-scale area, electrostatic force images showed that the domain switching was hard in the PZT thin films with random orientation, while the pattern could clearly be written in the PZT films with c-axis orientation. The differences in the domain switching properties of each PZT thin film were investigated in the crystallographic orientations point of view, and the domain switching dynamics were also measured by investigating the nano-sized dot switching behavior with respect to the width of the applied voltage pulse.     

“Magic size” effect in the packing of n-alkanes on Au(1 1 1): evidence of lowered sliding force for molecules with specific length

Molecular structure of monolayers formed at the interface between Au(1 1 1) surfaces and solutions containing n-alkanes has been studied by in situ scanning tunneling microscopy at room temperature. Increasing the C_nH_2n+2 length from n=10 up to 50 with even n numbers alternates rectangular and tilted arrangement of alkanes within the self-organized layers. This alternation is related to the dramatically lowered sliding force for molecules with a length close to mT (m-integer), where T is the period of commensurability between the CH₂-CH₂-CH₂ period along alkyl chains and the interatomic distance along Au〈1 1 0〉 direction.     

Development of high-precision micro-coordinate measuring machine: Multi-probe measurement system for measuring yaw and straightness motion error of XY linear stage

Today, with the development of microsystem technologies, demands for three-dimensional (3D) metrologies for microsystem components have increased. High-accuracy micro-coordinate measuring machines (micro-CMMs) have been developed to satisfy these demands. A high-precision micro-CMM (M-CMM) is currently under development at the National Metrology Institute of Japan in the National Institute of Advanced Industrial Science and Technology (AIST), in collaboration with the University of Tokyo. The moving volume of the M-CMM is 160 mm × 160 mm × 100 mm (XYZ), and our aim is to achieve 50-nm measurement uncertainty with a measuring volume of 30 mm × 30 mm × 10 mm (XYZ). The M-CMM configuration comprises three main parts: a cross XY-axis, a separate Z-axis, and a changeable probe unit. We have designed a multi-probe measurement system to evaluate the motion accuracy of each stage of the M-CMM. In the measurement system, one autocollimator measures the yaw error of the moving stage, while two laser interferometers simultaneously probe the surface of a reference bar mirror that is fixed on top of an XY linear stage. The straightness motion error and the reference bar mirror profile are reconstructed by the application of simultaneous linear equations and least-squares methods. In this paper, we have discussed the simulation results of the uncertainty value of the multi-probe measurement method using different intervals and standard deviations of the laser interferometers. We also conducted pre-experiments of the multi-probe measurement method for evaluating the motion errors of the XY linear stage based on a stepper motor system. The results from the pre-experiment verify that the multi-probe measurement method performs the yaw and straightness motion error measurement extremely well. Comparisons with the simulation results demonstrate that the multi-probe measurement method can also measure the reference bar mirror profile with a small standard deviation of 10 nm.     

Friction, wear and N2-lubrication of carbon nitride coatings: a review

Recent results of tribological properties of carbon nitride (CN_x) coatings are reviewed. CN_x coatings of 100 nm thickness were formed on Si-wafer and Si₃N₄ disks by the ion beam mixing method. Friction and wear tests were carried out against Si₃N₄ balls in the environments of vacuum, Ar, N₂, CO₂, O₂ or air by a ball-on-disk tribo-tester in the load range of 80-750 mN and in the velocity range of 4-400 mm/s.It was found that friction coefficient μ is high (μ=0.2-0.4) in air and O₂, and low (μ=0.01-0.1) in N₂, CO₂ and vacuum. The lowest friction coefficient (μ<0.01) was obtained in N₂. It was also found that N₂ gas blown to the sliding surfaces in air effectively reduced the friction coefficient down to μ≈0.017. Wear rate of CN_x coatings varied in the range 10⁻⁹-10⁻⁵ mm³/N m depending on the environment.The wear mechanisms of CN_x in the nanometer scale were studied by abrasive sliding of an AFM diamond pin in air. It was confirmed that the major wear mechanism of CN_x in abrasive friction was low-cycle fatigue which generated thin flaky wear particles of nanometre size.     

APT analyses of deuterium-loaded Fe/V multi-layered films

Interaction of hydrogen with metallic multi-layered thin films remains as a hot topic in recent days. Detailed knowledge on such chemically modulated systems is required if they are desired for application in hydrogen energy system as storage media. In this study, the deuterium concentration profile of Fe/V multi-layer was investigated by atom probe tomography (APT) at 60 and 30 K. It is firstly shown that deuterium-loaded sample can easily react with oxygen at the Pd capping layer on Fe/V and therefore, it is highly desired to avoid any oxygen exposure after D₂ loading before APT analysis. The analysis temperature also has an impact on D concentration profile. The result taken at 60 K shows clear traces of surface segregation of D atoms towards analysis surface. The observed diffusion profile of D allows us to estimate an apparent diffusion coefficient D. The calculated D at 60 K is in the order of 10⁻¹⁷ cm²/s, deviating 6 orders of magnitude from an extrapolated value. This was interpreted with alloying, D-trapping at defects and effects of the large extension to which the extrapolation was done. A D concentration profile taken at 30 K shows no segregation anymore and a homogeneous distribution at c_D=0.05(2) D/Me, which is in good accordance with that measured in the corresponding pressure–composition isotherm.     

Tribological properties of spark-plasma-sintered ZrO2(Y2O3)-CaF2-Ag composites at elevated temperatures

Spark-plasma sintering is employed to synthesize self-lubricating ZrO₂(Y₂O₃) matrix composites with different additives of CaF₂ and Ag as solid lubricants by tailoring the composition and by adjusting the sintering temperature. The friction and wear behavior of ZrO₂(Y₂O₃) matrix composites have been investigated in dry sliding against an alumina ball from room temperature to 800 °C. The effective self-lubrication at different temperatures depends mainly on the content of various solid lubricants in the composites. The addition of 35 wt.% Ag and 30 wt.% CaF₂ in the ZrO₂(Y₂O₃) matrix can promote the formation of a well-covered lubricating film, and effectively reduce the friction and wear over the entire temperature range studied. The friction coefficients at low temperatures were at a minimum value for the composite containing 35 wt.% of silver. At this silver concentration, low and intermediate temperature lubricating properties are greatly improved without affecting high-temperature lubrication by the calcium fluoride in ZrO₂(Y₂O₃) matrix composites. The worn surfaces and transfer films formed during wear process have been characterized to identify the synergistic lubrication behavior of CaF₂ and Ag lubricants at different temperatures.     

Characterization of nanoscale recording mark on Ge2Sb2Te5 film

We have fabricated nanoscale recording marks on Ge₂Sb₂Te₅ (GST) films with conductive atomic force microscope (AFM). GST films were deposited on glass or polyimide film with thickness of 150–200 nm by the rf–sputtering method. Through current–voltage (I–V) spectroscopy, good cantilevers for fabrication and characterization of nanoscale marks on GST were selected. A fresh and highly conductive tip showed voltage-switching characteristic in the I–V curve, where the threshold voltage was 1.6 V. Nanoscale dot and wire arrays of crystalline phases were successfully obtained by varying sample bias voltage from −10 to 10 V. With highly conductive tips, nanowires having full-width at half-maximum of 20 nm could be fabricated, whereas nanowires could not be fabricated with bias voltage below −2 V. The width of the nanoscale mark was increased by repetition of AFM lithography even with same applied voltage and lithography speed. For a thicker nanowire, the width measured in current-image (C-image) was observed to be 2 times of that measured in topography-image (T-image). This result supports that current sensing provides an image of phase-changed GST area with higher resolution than topography sensing.     

Process investigation on meso-scale hard milling of ZrO2 by diamond coated tools

This paper investigates the feasible machining of zirconium oxide (ZrO₂) ceramics, in the hard state, via milling by diamond coated miniature tools (from here on briefly indicated as meso-scale hard milling). The workpiece material is a fully sintered yttria stabilized tetragonal zirconia polycrystalline ceramic (Y-TZP). Diamond coated WC mills, 2 mm in diameter, four flutes and large corner radius (0.5 mm) are chosen as cutting tools, and experiments are conducted on a state-of-the-art micro milling machine centre. The influence of cutting parameters, including axial depth of cut (a_p) and feed per tooth (f_z), on the achievable surface quality is studied by means of a one-factor variation experimental design. Further tests are also conducted to monitor the process performance, including surface roughness, tool wear and machining accuracy, over the machining time. Mirror quality surfaces, with average surface roughness Ra below 80 nm, are obtained on the machined samples; the SEM observations of the surface topography reveal a prevailing ductile cutting appearance. Tool wear initiates with delamination of the diamond coating and progresses with the wear of the WC substrate, with significant effect on the cutting process and its performance. Main applications of this research include three dimensional surface micro structuring and superior surface finishing.     

Effect of pre-readout annealing treatments on TL mechanism in tellurite glasses at therapeutic radiation doses level

The higher sensitization for thermal annealing on TL mechanism in the region 550–600 °C for 80(TeO₂)–5(TiO₂)–(15 − x) (WO₃)–(x) A_nO_m where A_nO_m = Nb₂O₅, Nd₂O₃, Er₂O₃ and x = 5 mol% has been measured. The behavior of trap centers and luminescence centers has been investigated for tellurite glasses doped with rare earth oxides irradiated at 0.5 up to 2 Gy and annealed at different temperatures in the range 350–700 °C. The behavior of the three types of tellurite glasses is analyzed regarding to their kinetic parameters and luminescence emission which enhance the claim of tellurite glasses for use as TLD material at therapeutic radiation doses.     

Influence of Cr content on tribological properties of Ni3Al matrix high temperature self-lubricating composites

High temperature self-lubricating composites Ni₃Al-BaF₂-CaF₂-Ag-Cr were fabricated by powder metallurgy technique. In this paper the effect of Cr content on tribological properties at a wide temperature range starting from room temperature to 1000 °C was investigated. It was found that Ni₃Al matrix composite with 20 wt% Cr exhibited low friction coefficient of 0.24-0.37 and a wear rate of 0.52-2.32×10⁻⁴ mm³ N⁻¹ m⁻¹. Especially at 800 °C it showed the lowest friction coefficient of 0.24 and a favorable wear rate of 0.71×10⁻⁴ mm³ N⁻¹ m⁻¹. This implied that 20 wt% Cr was the optimal Cr content and its excellent tribological performance could be attributed to the balance between strength and lubricity.     

Simultaneous measurement of CO and CO2 at elevated temperatures by diode laser wavelength modulated spectroscopy

One single semiconductor distributed-feedback (DFB) laser is used to demonstrate the possibility of simultaneous measurements of CO and CO₂ at elevated temperatures. Wavelength modulation spectroscopy with second-harmonic detection is used to improve the detection sensitivity and accuracy. The concentrations of CO and CO₂ are determined from the WMS-1-normalized absorption-based WMS-2f signal peak heights of a proper line pair of CO and CO₂ near 6357.814 cm⁻¹ and 6357.312 cm⁻¹, which are selected using some line-selection criterions for the target temperature range of 300–1000 K. The CO and CO₂ concentrations measurements are within 2.86% and 2.69% of the expected values over the tested temperature range 300–1000 K. The minimum detectable concentrations of CO and CO₂ at 1000 K are 250 ppm m and 280 ppm m respectively.     

Effect of post-implantation annealing on the current-voltage characteristics of IR photodiodes based on <Emphasis Type="Italic">p</Emphasis>-HgCdTe

Current-voltage characteristics of IR photodiodes and distributions of charge carriers in n ⁺-n ⁻-p-structures based on vacancy p-doped Hg_{1 − x} Cd _x Te films with x = 0.22 are examined. Three-dimensional numerical modeling of the distribution of charge carriers and current-voltage characteristics during photodiode annealing is performed. The calculations predict that large tunnel currents in diodes after implantation can result from an elevated (more than 10¹⁵ cm⁻³) concentration of donors in the n ⁻-layer, which enhances tunneling by decreasing the thickness of the space charged region of the n-p-junction, and also from a small (less than 3 μm) depth of the p-n-junction.     

Polypyrrole-NiO hybrid nanocomposite: Structural,morphological, optical and electrical transport studies

Polypyrrole (PPy)-nickel oxide (NiO) hybrid nanocomposite thin films have been prepared by spin coating method. The PPy–NiO hybrid nanocomposites were characterized for structural, morphological, optical and electrical analysis, and the results were compared with the pure PPy films. The structural and optoelectronic properties of PPy–NiO hybrid nanocomposites are quite different from those of pure PPy and NiO nanoparticles, which were attributed to the strong interaction between the PPy and NiO nanoparticles. The XRD pattern shows that broad peak of PPy becoming weaker on increasing the content of NiO nanoparticles in the PPy–NiO hybrid nanocomposites. Also the diffraction peaks of NiO nanoparticles in PPy–NiO (10–50 wt%) nanocomposites were found to shift to lower 2θ values. The morphological studies revealed that the transformation of granular morphology of PPy to the nanospheres and clusters in the PPy–NiO hybrid nanocomposites. FTIR spectra of PPy–NiO hybrid nanocomposites, revealed that the main absorption at 1204 cm⁻¹ and 1559 cm⁻¹ are affected by the presence of NiO nanoparticle in pure PPy and get shifted to 1216 cm⁻¹ and 1570 cm⁻¹ respectively indicates, insertion of NiO nanoparticles in the PPy–NiO hybrid nanocomposite. UV–vis absorption spectrum of PPy corresponding to λ_max = 442 nm is blue shifted to λ_max = 375 nm in the PPy–NiO hybrid nanocomposites, reveals strong interaction between PPy and NiO nanoparticles. The room temperature dc electrical conductivity is increased from 8.66 × 10⁻⁹ to 4.08 × 10⁻⁷ (Ω/cm)⁻¹ as the content of NiO nanoparticles increased from 10 to 50 in wt% in the PPy–NiO hybrid nanocomposites.