Μm Thick Samples Research Articles

Defect structure and strain reduction of 3C-SiC/Si layers obtained with the use of a buffer layer and methyltrichlorosilane addition

3C-SiC layers were deposited on Si substrates by using a low temperature buffer layer and the addition of methyltrichlorosilane (MTS) to the gas phase during the high temperature thick film growth. Several samples were grown by varying the deposition temperature and the MTS content in order to study how these parameters affect the layer quality and the lattice defects. All of the grown layers are single crystalline and epitaxial to the substrate. The formation of empty voids at the SiC/Si interface was successfully avoided. The surface of the layers grown with MTS addition was smoother and contained less residual strain. A 15 μm thick 3C-SiC sample was grown using an optimized process in order to evaluate its residual strain and bow.

Silver nanoparticles as a key feature of a plasma polymer composite layer in mitigation of charge injection into polyethylene under dc stress

The aim of this work is to limit charge injection from a semi-conducting electrode into low density polyethylene (LDPE) under dc field by tailoring the polymer surface using a silver nanoparticles-containing layer. The layer is composed of a plane of silver nanoparticles embedded in a semi-insulating organosilicon matrix deposited on the polyethylene surface by a plasma process. Size, density and surface coverage of the nanoparticles are controlled through the plasma process. Space charge distribution in 300 μm thick LDPE samples is measured by the pulsed-electroacoustic technique following a short term (step-wise voltage increase up to 50 kV mm−1, 20 min in duration each, followed by a polarity inversion) and a longer term (up to 12 h under 40 kV mm−1) protocols for voltage application. A comparative study of space charge distribution between a reference polyethylene sample and the tailored samples is presented. It is shown that the barrier effect depends on the size distribution and the surface area covered by the nanoparticles: 15 nm (average size) silver nanoparticles with a high surface density but still not percolating form an efficient barrier layer that suppress charge injection. It is worthy to note that charge injection is detected for samples tailored with (i) percolating nanoparticles embedded in organosilicon layer; (ii) with organosilicon layer only, without nanoparticles and (iii) with smaller size silver particles (<10 nm) embedded in organosilicon layer. The amount of injected charges in the tailored samples increases gradually in the samples ranking given above. The mechanism of charge injection mitigation is discussed on the basis of complementary experiments carried out on the nanocomposite layer such as surface potential measurements. The ability of silver clusters to stabilize electrical charges close to the electrode thereby counterbalancing the applied field appears to be a key factor in explaining the charge injection mitigation effect.

Refractive index measurements of poly(methyl methacrylate) (PMMA) from 0.4-1.6 μm.

Using a transmission-spectrum-based method, the refractive index of a 50 μm thick sample of poly(methyl methacrylate) (PMMA) was measured as a function of wavelength. To mitigate the effects of nonplane-parallel surfaces, the sample was measured at 16 different locations. The technique resulted in the measurement of index at several thousand independent wavelengths from 0.42 to 1.62 μm, with a relative RMS accuracy <0.5×10(-4) and absolute accuracy <2×10(-4).

Effect of the absorption coefficient of aluminium plates on their thermoelastic bending in photoacoustic experiments

The open-cell photoacoustic signal measured in the transmission configuration for aluminum thin plates with thicknesses of 280 μm, 197 μm, and 112 μm is experimentally and theoretically analyzed, in the 20 Hz–7 kHz modulation frequency range. It is shown that the observed differences between the predictions of the standard thermoelastic model and the experiment data of both the amplitude and phase of the photoacoustic signal can be overcome by considering the aluminum samples coated with a thin layer of black paint as volume-absorber materials. This new approach provides a quite good agreement with the obtained experimental data, in the whole frequency range, and yields an effective absorption coefficient of (16 ± 2) mm−1, for a 280 μm-thick sample. The introduction of the finite absorption coefficient led to the correct ratio between the thermal diffusion and thermoelastic components of the photoacoustic signal. Furthermore, it is found that the “volume-absorber” approach accurately describes the behavior of the amplitude, but not that of the phase recorded for a 112 μm-thick sample, due to its relatively strong thermoelastic bending, which is not considered by this theory. Within the approximation of the small bending, the proposed “volume-absorber” model provides a reliable description of the photoacoustic signal for Al samples thicker than 112 μm, and extends the applicability of the classical “opaque” approach.

High-resolution chemical depth profiling of solid material using a miniature laser ablation/ionization mass spectrometer.

High-resolution chemical depth profiling measurements of copper films are presented. The 10 μm thick copper test samples were electrodeposited on a Si-supported Cu seed under galvanostatic conditions in the presence of particular plating additives (SPS, Imep, PEI, and PAG) used in the semiconductor industry for the on-chip metallization of interconnects. To probe the trend of these plating additives toward inclusion into the deposit upon growth, quantitative elemental mass spectrometric measurements at trace level concentration were conducted by using a sensitive miniature laser ablation ionization mass spectrometer (LIMS), originally designed and developed for in situ space exploration. An ultrashort pulsed laser system (τ ∼ 190 fs, λ = 775 nm) was used for ablation and ionization of sample material. We show that with our LIMS system, quantitative chemical mass spectrometric analysis with an ablation rate at the subnanometer level per single laser shot can be conducted. The measurement capabilities of our instrument, including the high vertical depth resolution coupled with high detection sensitivity of ∼10 ppb, high dynamic range ≥10(8), measurement accuracy and precision, is of considerable interest in various fields of application, where investigations with high lateral and vertical resolution of the chemical composition of solid materials are required, these include, e.g., wafers from semiconductor industry or studies on space weathered samples in space research.

A New Ni-Based Metallic Glass with High Thermal Stability and Hardness

Glass forming ability (GFA), thermal stability and microhardness of Ni51−xCuxW31.6B17.4 (x = 0, 5) metallic glasses have been investigated. For each alloy, thin sheets of samples having thickness of 20 µm and 100 µm were synthesized by piston and anvil method in a vacuum arc furnace. Also, 400 µm thick samples of the alloys were synthesized by suction casting method. The samples were investigated by X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). Crystallization temperature of the base alloy, Ni51W31.6B17.4, is found to be 996 K and 5 at.% copper substitution for nickel increases the crystallization temperature to 1063 K, which is the highest value reported for Ni-based metallic glasses up to the present. In addition, critical casting thickness of alloy Ni51W31.6B17.4 is 100 µm and copper substitution does not have any effect on critical casting thickness of the alloys. Also, microhardness of the alloys are found to be around 1200 Hv, which is one of the highest microhardness values reported for a Ni-based metallic glass until now.

X-ray μ-Laue diffraction analysis of Cu through-silicon vias: A two-dimensional and three-dimensional study

Here, white X-ray μ-beam Laue diffraction is developed and applied to investigate elastic strain distributions in three-dimensional (3D) materials, more specifically, for the study of strain in Cu 10 μm diameter–80 μm deep through-silicon vias (TSVs). Two different approaches have been applied: (i) two-dimensional μ-Laue scanning and (ii) μ-beam Laue tomography. 2D μ-Laue scans provided the maps of the deviatoric strain tensor integrated along the via length over an array of TSVs in a 100 μm thick sample prepared by Focused Ion Beam. The μ-beam Laue tomography analysis enabled to obtain the 3D grain and elemental distribution of both Cu and Si. The position, size (about 3 μm), shape, and orientation of Cu grains were obtained. Radial profiles of the equivalent deviatoric strain around the TSVs have been derived through both approaches. The results from both methods are compared and discussed.

Magnetic Field Dependence of Critical Current in Sm1+xBa2Cu3+yO7−d Coated Conductors Fabricated by Reactive Co-evaporation Method

Sm 1+xBa 2Cu 3+yO7−d coated conductors were fabricated by reactive co-evaporation method in the evaporation using drum in dual chambers (EDDC) deposition chamber. The effect of substrate temperature on the superconducting properties was investigated. Three samples were prepared with different substrate temperatures of 740, 780, and 800 °C. In plane and out-of-plane texture were confirmed by X-ray patterns of 2 theta and phi scan and turned out to be almost the same. Angular dependences of critical currents of those samples were measured at 0.5 and 1 T. The magnetic field dependence of critical current with the magnetic field direction parallel to the c-axis of SmBCO film was measured in the range of 0.01–1.5 T. The critical current of the sample prepared at 740 °C was slightly lower than that of other samples in the range of 0.5–1.5 T. Also we investigated the effect of thickness of superconducting layer on the magnetic field dependence. Two samples with different SmBCO film thicknesses of 0.8 and 5 μm were prepared. The magnetic field dependence of critical current in the direction parallel to the c-axis of SmBCO film was measured in the range of 0.01–1.5 T. We found that the normalized critical current of a 5 μm thick sample was higher than that of 0.8 μm thick sample possibly due to the higher pinning force of thick film than that of thin film.

TH-C-19A-12: Two-Dimensional High Spatial-Resolution Dosimeter Using Europium Doped Potassium Chloride

Purpose: Recent research has shown that KCl:Eu2+ has great potential for use in megavoltage radiation therapy dosimetry because this material exhibits excellent storage performance and is reusable due to strong radiation hardness. This work reports our attempts to fabricate 2D KCl:Eu2+ storage phosphor films (SPFs) using both a physical vapor deposition (PVD) method and a tape casting method. Methods: A thin layer of KCl:Eu2+ was deposited on a substrate of borosilicate glass (e.g., laboratory slides) with a PVD system. For tape casting, a homogenous suspension containing storage phosphor particles, liquid vehicle and polymer binder was formed and subsequently cast by doctor-blade onto a polyethylene terephthalate substrate to form a 150 μm thick SPF. Results: X ray diffraction analysis showed that a 10 μm thick PVD sample was composed of highly crystalline KCl. No additional phases were observed, suggesting that the europium activator had completed been incorporated into the KCl matrix. Photostimulated luminescence and photoluminescence spectra suggested that F (Cl−) centers were the electron storage centers post x ray irradiation and that Eu2+ cations acted as luminescence centers in the photostimulation process. The 150 μm thick casted KCl:Eu2+ SPF showed sub-millimeter spatial resolution. Monte Carlo simulations further demonstrated that the admixture of 20% KCl:Eu2+ and 80% low Z polymer binder exhibited almost no energy dependence in a 6 MV beam. KCl:Eu2+ pellet samples showed a large dynamic range from 0.01 cGy to 60 Gy dose-to-water, and saturated at approximately 500 Gy as a Result of its intrinsic high radiation hardness. Conclusions: This discovery research provides strong evidence that KCl:Eu2+ based SPF with associated readout apparatus could Result in a novel electronic film system that has all the desirable features associated with classic radiographic film and, importantly, water equivalence and the capability of permanent identification of each detector. This work was supported in part by NIH Grant No. R01CA148853. The authors would like to thank Paul Leblans (AGFA Healthcare, Belgium) for many helpful discussions on this topic.

Development of positron annihilation spectroscopy for characterizing neutron irradiated tungsten

Tungsten samples (6 mm diameter and 0.2 mm thick) were irradiated to 0.025 and 0.3 dpa with neutrons in the High Flux Isotope Reactor at Oak Ridge National Laboratory as part of the US/Japan Tritium, Irradiation and Thermofluids for America and Nippon (TITAN) collaboration. Samples were then exposed to deuterium plasma in Idaho National Laboratory's Tritium Plasma Experiment at 100, 200 and 500 °C to a total fluence of 1 × 1026 m−2. Nuclear reaction analysis (NRA) and Doppler broadening positron annihilation spectroscopy (DB-PAS) were performed at various stages to characterize radiation damage and retention. We present the first results of neutron irradiated tungsten characterized by DB-PAS in order to study defect concentration. Two positron sources, 22Na and 68Ge, probe ∼58 μm and through the entire 200 μm thick samples, respectively. DB-PAS results reveal clear differences between the various irradiated samples. These results, and a correlation between DB-PAS and NRA data, are presented.

Two-dimensional high spatial-resolution dosimeter using europium doped potassium chloride: a feasibility study

Recent research has shown that KCl:Eu2+ has great potential for use in megavoltage radiation therapy dosimetry because this material exhibits excellent storage performance and is reusable due to strong radiation hardness. This work reports the authors’ attempts to fabricate 2D KCl:Eu2+ storage phosphor films (SPFs) using both a physical vapor deposition (PVD) method and a tape casting method. X-ray diffraction analysis showed that a 10 µm thick PVD sample was composed of highly crystalline KCl. No additional phases were observed, suggesting that the europium activator had been completely incorporated into the KCl matrix. Photostimulated luminescence and photoluminescence spectra suggested that F (Cl−) centers were the electron storage centers post x-ray irradiation and that Eu2+ cations acted as luminescence centers in the photostimulation process. The 150 µm thick casted KCl:Eu2+ SPF showed sub-millimeter spatial-resolution. Monte Carlo simulations further demonstrated that the admixture of 20% KCl:Eu2+ and 80% low Z polymer binder exhibited almost no energy-dependence in a 6 MV beam. KCl:Eu2+ pellet samples showed a large dynamic range from 0.01 cGy to 60 Gy dose-to-water, and saturated at approximately 500 Gy as a result of KCl's intrinsic high radiation hardness. Taken together, this work provides strong evidence that KCl:Eu2+-based SPF with associated readout apparatus could result in a novel electronic film system that has all the desirable features associated with classic radiographic film and, importantly, water equivalence and the capability of permanent identification of each detector.

Lambertian light trapping in thin crystalline macroporous Si layers

AbstractLambertian light trapping is a benchmark for efficient light trapping. In this Letter we experimentally quantify the degree of Lambertian light trapping in a macroporous silicon layer. The optical absorption of the effective (26.7 ± 5.5) µm thick sample with randomly arranged pores yields a photogeneration corresponding to a maximum current density of (40.8 ± 0.4) mA cm–2 and thus achieves a fraction of 0.985 ± 0.012 of the current density expected from a Lambertian light trapping scheme. The measured spectrum of the escape reflectance is well described with an analytic model assuming a complete randomization of the directions of light propagation. (© 2014 WILEY‐VCH Verlag GmbH &amp; Co. KGaA, Weinheim)

STRUCTURAL CHANGES IN PULSED LASER ABLATED CuInSe2 COMPOUND STRUKTURĀLĀS IZMAIŅAS IMPULSA LĀZERA ABLĒTAJĀ CuInSe2 SAVIENOJUMĀ

Abstract CuInSe2 (CISe) compound was produced by high-temperature synthesis. After mechanical milling, the average CISe particle size decreased to 10μm. The authors study structural changes of the compound after ablation in liquid by a 1064 nm pulsed laser. The SEM examination indicated the presence of spherical particles with the average size of ~ 450 nm. A nonlinear relationship was established between the laser radiation dose and the quantity of spherical particles. The XRD analysis has shown an improvement in the CISe crystalline structure and the absence of significant changes in its stoichiometry. The 3 μm thick experimental CISe samples were screen-printed on planar Ni electrodes, and improvement also was revealed in their photosensitivity. The conclusion is that the pulsed-laser ablation can be applied to chalcopyrite structures like CISe without destruction of their initial properties.

Optimized Anion Exchange Membranes for Vanadium Redox Flow Batteries

In order to understand the properties of low vanadium permeability anion exchange membranes for vanadium redox flow batteries (VRFBs), quaternary ammonium functionalized Radel (QA-Radel) membranes with three ion exchange capacities (IECs) from 1.7 to 2.4 mequiv g(-1) were synthesized and 55-60 μm thick membrane samples were evaluated for their transport properties and in-cell battery performance. The ionic conductivity and vanadium permeability of the membranes were investigated and correlated to the battery performance through measurements of Coulombic efficiency, voltage efficiency and energy efficiency in single cell tests, and capacity fade during cycling. Increasing the IEC of the QA-Radel membranes increased both the ionic conductivity and VO(2+) permeability. The 1.7 mequiv g(-1) IEC QA-Radel had the highest Coulombic efficiency and best cycling capacity maintenance in the VRFB, while the cell's voltage efficiency was limited by the membrane's low ionic conductivity. Increasing the IEC resulted in higher voltage efficiency for the 2.0 and 2.4 mequiv g(-1) samples, but the cells with these membranes displayed reduced Coulombic efficiency and faster capacity fade. The QA-Radel with an IEC of 2.0 mequiv g(-1) had the best balance of ionic conductivity and VO(2+) permeability, achieving a maximum power density of 218 mW cm(-2) which was higher than the maximum power density of a VRFB assembled with a Nafion N212 membrane in our system. While anion exchange membranes are under study for a variety of VRFB applications, this work demonstrates that the material parameters must be optimized to obtain the maximum cell performance.

A spectrometer on chemical vapour deposition-diamond basis for the measurement of the charge-state distribution of heavy ions in a laser-generated plasma

This article reports on the development and the first applications of a new spectrometer which enables the precise and time-resolved measurement of both the energy loss and the charge-state distribution of ion beams with 10 < Z < 30 at energies of 4-8 MeV/u after their interaction with a laser-generated plasma. The spectrometer is based on five 20 × 7 mm(2) large and 20 μm thick polycrystalline diamond samples produced via the Chemical Vapour Deposition (CVD) process and was designed with the help of ion-optical simulations. First experiments with the spectrometer were successfully carried out at GSI using (48)Ca ions at an energy of 4.8 MeV/u interacting with a carbon plasma generated by the laser irradiation of a thin foil target. Owing to the high rate capability and the short response time of the spectrometer, pulsed ion beams with 10(3)-10(4) ions per bunch at a bunch frequency of 108 MHz could be detected. The temporal evolution of the five main charge states of the calcium ion beams as well as the corresponding energy loss values could be measured simultaneously. Due to the outstanding properties of diamond as a particle detector, a beam energy resolution ΔEE ≈ 0.1% could be reached using the presented experimental method, while a precision of 10% in the energy loss and charge-state distribution data was obtained.

Sample thickness considerations for quantitative X‐ray fluorescence analysis of the soft and skeletal tissues of the human body – theoretical evaluation and experimental validation

A good estimation of the matrix composition and the areal mass of the sample is critical for quantitative X‐ray fluorescence (XRF) analysis. Integrated aspects of the XRF quantitative analysis of various human body organs are presented. Special emphasis is placed on the determination of the sample thicknesses at which the specimen can be regarded as thin, thick, or intermediate thickness depending on the element under consideration. Moreover, a method for a fully quantitative analysis allowing the determination of the masses per unit area of chemical elements in thin, thick, and intermediate thickness samples is discussed. It was found that for an incident beam of 17 keV energy, a 15 µm thick sample is of intermediate thickness for all elements between P and Ca and becomes thin from Fe for most human body tissues in a natural form. Dried samples of soft tissues excluding these of low water content can be regarded as thin for all elements from phosphorus to strontium. The use of thin sample approach in quantification of intermediate thickness specimen may result in about 30–45% discrepancy in areal mass (weight fraction) of phosphorus, 20–35% of sulfur, 15–25% of chlorine, 8–15% of potassium, and 5–10% of calcium. Theoretical evaluations presented in the work are verified experimentally. The analysis of human brain samples (white and gray matter) and bovine liver (National Institute of Standards and Technology standard reference materials 1577b) confirms high accuracy of the XRF quantification on the basis of the described procedures. Copyright © 2012 John Wiley &amp; Sons, Ltd.

Infrared Laser Ablation Sample Transfer for MALDI Imaging

An infrared laser was used to ablate material from tissue sections under ambient conditions for direct collection on a matrix assisted laser desorption ionization (MALDI) target. A 10 μm thick tissue sample was placed on a microscope slide and was mounted tissue-side down between 70 and 450 μm from a second microscope slide. The two slides were mounted on a translation stage, and the tissue was scanned in two dimensions under a focused mid-infrared (IR) laser beam to transfer material to the target slide via ablation. After the material was transferred to the target slide, it was analyzed using MALDI imaging using a tandem time-of-flight mass spectrometer. Images were obtained from peptide standards for initial optimization of the system and from mouse brain tissue sections using deposition either onto a matrix precoated target or with matrix addition after sample transfer and compared with those from standard MALDI mass spectrometry imaging. The spatial resolution of the transferred material is approximately 400 μm. Laser ablation sample transfer provides several new capabilities not possible with conventional MALDI imaging including (1) ambient sampling for MALDI imaging, (2) area to spot concentration of ablated material, (3) collection of material for multiple imaging analyses, and (4) direct collection onto nanostructure assisted laser desorption ionization (NALDI) targets without blotting or ultrathin sections.

Design of a new coplanar isolator made from YIG film operating in the X-frequency band

The miniaturization of devices and the increase of operating frequencies are two important issues for communication system development. This requires a high degree of integration, higher performance and lower cost. Isolator is an important non-reciprocal passive component for source protection. In most cases, the non-reciprocal effect is based on field displacement phenomenon induced by a magnetized ferrite material. In this paper we propose a new design of a coplanar isolator based on field displacement, composed of a non-symmetrical coplanar transmission line, made from a ferrite layer and ground plane below. Simulations were performed using HFSS software. Measurements were made on a first 1000 μm-thick YIG film sample giving 1 dB of insertion losses and 17 dB isolation and on a second sample made from a 150 μm-thick YIG ferrite sample giving an insertion loss lower than 2 dB. Interesting applications of this isolator structure are considered.

A new approach to grow C‐doped GaN thick epitaxial layers

AbstractIn this study we employ a new method for growth of carbon‐doped wurtzite crystalline GaN (GaN:C) based on vapour phase transport of Ga by the pseudohalide hydrogen cyanide HCN. GaN:C layers with a thicknesses from 10 to 100 μm and up to 19 mm in size were grown from gallium melt and ammonia as feeding materials in a carbon‐containing equipment. The properties of the GaN:C layers were characterized by low‐temperature photoluminescence (LTPL), High‐Resolution X‐ray Diffraction (HRXRD), Secondary Ion Mass Spectrometry (SIMS) and room‐temperature Hall effect and Raman spectroscopy measurements. HRXRD studies demonstrated good crystalline quality of the thick GaN layers (the Rocking curve FWHMs are 570 arcsec for the (0004) reflection and 561 arcsec for the (10‐14) reflection for 10 μm thick samples). The LTPL and Raman spectroscopy confirmed the good optical and structural quality of the material. The carbon concentration measured by SIMS was 6x1018 cm‐3, however, the room‐temperature Hall effect experiments showed n‐type conductivity. Carbon acceptor incorporation into GaN (from the transport agent) as well as the reason of its electrical overcompensation by unintentional impurities like oxygen and silicon is discussed. Ways of technological process improvement are proposed. (© 2011 WILEY‐VCH Verlag GmbH &amp; Co. KGaA, Weinheim)

Surface-type humidity sensor based on cellulose-PEPC for telemetry systems

Au/cellulose-PEPC/Au surface-type humidity sensors were fabricated by drop-casting cellulose and poly-N-epoxypropylcarbazole (PEPC) blend thin films. A blend of 2wt% of each cellulose and PEPC in benzol was used for the deposition of humidity sensing films. Blend films were deposited on glass substrates with preliminary deposited surface-type gold electrodes. Films of different thicknesses of cellulose and PEPC composite were deposited by drop-casting technique. A change in electrical resistance and capacitance of the fabricated devices was observed by increasing the relative humidity in the range of 0–95% RH. It was observed that the capacitances of the sensors increase, while their resistances decrease with increasing the relative humidity. The sensors were connected to op-amp square wave oscillators. It was observed that with increasing the relative humidity, the oscillator's frequencies were also increased in the range of 4.2–12.0 kHz for 65 μm thick film sample, 4.1–9.0 kHz for 88 μm thick film sample, and 4.2–9.0 kHz for 210 μm sample. Effects of film thickness on the oscillator's frequency with respect to humidity were also investigated. This polymer humidity sensor controlled oscillator can be used for short-range and long-range remote systems at environmental monitoring and assessment of the humidity level.