A dual analyzer for real-time impedance and noise spectroscopy of nanoscale devices

This paper introduces a simple portable dual analyzer which allows real-time ac-impedance measurements and noise spectroscopic analysis simultaneously, employing one or two data acquisition systems together with a low noise current-to-voltage preamplifier. The input signal composed of numerous selected frequencies of sinusoidal voltages with a dc bias was applied to a device under the test (DUT): single walled carbon nanotube field effect transistors (SWCNT-FETs). Each frequency component, ranging from 1 to 46.4 kHz, was successfully mapped to a Nyquist plot using the background of the electrical noise power spectrum. It is, thus, clearly demonstrated that this dual analyzer enables the real-time ac-impedance analysis and the frequency response of the carrier transport in the SWCNT-FETs as a DUT.     

Characterization of thermoelectric generators by measuring the load-dependence behavior

Solid-state thermoelectric generators (TEGs) based on the Seebeck effect to convert temperature gradients, ΔT [K], into electrical energy are being used in an increased number of stand-alone microsystems applications. These generators are composed by at least one pair of p- and n-type thermoelectric elements with high figures-of-merit, ZT, to perform such a conversion. The exact behavior knowledge of generators is mandatory in order to decide the most suitable for the target application. The focus of this paper is to present a methodology to characterize thermoelectric generators, by measuring their behavior for different types of loads. The measurements were done with the help of commercial thermoelectric generators (thermoelectric modules TEC1-12707) and a measurement setup composed by a controlled hot-plate, a controlled cooling fan (above an heat dissipator), a set of two thermistors for measuring the temperature, a personal computer with the data acquisition board model NI USB-6009 and the LabView software from National Instruments for acquiring the measures and for controlling both the hot-plate and the cooling fan. The thermoelectric modules TEC1-12707 was selected due to its compact size (e.g., 40 mm × 40 mm) and because it can withstand temperatures up to 450 K without degrading the quality of measurements. A SPICE model for thermoelectric modules TEC1-12707 was also obtained: an open-circuit voltage of V_open = 53.17 × ΔT [mV] and an internal resistance of R₀ = 3.88 Ω with a tolerance of ΔR_int = 0.13 Ω such that R_int = R₀ ± ΔR_int = 3.88 ± 0.13 Ω. The measurements done under the maximum output power delivery condition (for the maximum temperature gradient of ΔT = 51 °C) resulted in the maximum output power of P_out = 500 mW, as well as in the output current and voltage of I_out = 357 mA and V_out = 1.40 V, respectively. The load resistance of 3.92 Ω (V_out/I_out) is also in accordance with the measurements because it is located in the range [μ − σ, μ + σ] Ω, where μ = R₀ = 3.88 Ω and σ = ΔR_int = 0.13 Ω. An Agilent multimeter model 34410A with 6½ digits was used for measuring the voltages at the TEG’s output and the respective currents.     

An accurate new method to measure the dimensionless figure of merit of thermoelectric devices based on the complex impedance porcupine diagram

The heat diffusion related f(-1/2) slow decay in the frequency domain transfer function of thermoelectric devices introduces a bias in figure of merit measurement methods that do not take it into account. The bias can range from less than 1% to more than 20% depending on the device. Harman type methods are not immune. Neither is the simple single measurement procedure proposed here on the basis of a complex thermal impedance analysis of the device, but in this case the supporting theory allows evaluating and correcting for the bias with documented accuracy. To this aim, both a theoretical approach based on a priori knowledge of the device and an experimental one based on theory guided measurements are possible and are described in the paper. Typical residual Type B uncertainties after correction can be below 10% of the bias.     

Assessing the tribocorrosion behaviour of Cu and Al by electrochemical impedance spectroscopy

This study is focused on the interests and limits of Electrochemical Impedance Spectroscopy, to establish the electrochemical behaviour of a tribosystem between Cu and Al, in acid solution. The calculated capacitance, in high-frequency range, partially allows understanding the double layer state of body in the contact. The Potential of Zero Charge (PZC) was calculated for Cu sample and it was associated with a potential range for Al. PZC value of each material is discussed as a key parameter of sliding contact. During tests of wear, the EIS results are related to the evolution of adsorbed water molecules.     

Four-contact impedance spectroscopy of conductive liquid samples

We present an improved approach to the impedance spectroscopy of conductive liquid samples using four-electrode measurements. Our method enables impedance measurements of conductive liquids down to the sub-Hertz frequencies, avoiding the electrode polarization effects that usually cripple standard impedance analysers. We have successfully tested our apparatus with aqueous solutions of potassium chloride and gelatin. The first substance has shown flat spectra from ~100 kHz down to sub-Hz range, while the results on gelatin clearly show the existence of two distinct low frequency conductive relaxations.     

Alternating current impedance spectroscopy measurement under high pressure

A microcircuit was designed and fabricated on a diamond anvil cell for alternating current impedance spectroscopy measurement under high pressure. Sputtered molybdenum film on a diamond anvil was used as an electrode, maintained the contact between the sample and the electrode stable, and reduced the electrode effect on the impedance measurement. By the empty cell and short circuit tests, the parasitic capacitive impedance from the sample chamber wall was observed to be larger than 10(5) Ω at a frequency lower than 1.0 MHz and could be ignored for samples with higher conductivity. The wire inductance was only 1.0 μH and just appeared at frequency higher than 20 kHz, which could be subtracted from measured impedance for the samples with higher impedance than several hundred ohms. Using this apparatus, the impedances of the II-VI group cadmium sulfide were measured. The pressure dependence of the grain interior conductance of CdS crystal was obtained, which reflected that the phase transitions of CdS under high pressure are the same as the single crystal measurement results.     

The elusive half-pole in the frequency domain transfer function of Peltier thermoelectric devices

A half-pole can be expected in the transfer function of a Peltier device because proportionality between the diffusion length and the square root of the diffusion time is intrinsic in the diffusion equation. The resulting -1∕2 bilogarithmic slope (10 dB∕dec) is, however, easily masked by the thermal time constant of the load, which makes it elusive. The goal of this work is to identify the arrangements which can reveal and make usable the half-pole, because the latter can be instrumental in a servo control to increase the open-loop gain without risking instability. The diffusion equation was solved in a sine wave regime for a one-dimensional model of a Peltier device. The Laplace transform method was used, and the periodic solution was obtained using Cauchy's theorem and the method of residues. The -1∕2 slope of the half-pole appeared observable in a frequency range which can be several decades wide, depending on details of device configuration and considered position within. Amplitude and phase of temperature and heat flux in various spots are discussed with emphasis on the physical meaning, and a comparison is provided with solutions yielded by the lumped model, which cannot show the half-pole. An experimental check of the theoretical approach and analysis was made taking into account the deviations from one-dimensionality occurring in a real Peltier device. Given a constant amplitude sine wave injected current, the quadrature component of the Seebeck voltage across the whole series of junctions was identified as the most easily measurable quantity related to the thermal response of the device. Experimental results for the latter turned out in good agreement with analytical solutions.     

Characterization of biological macromolecules by combined mass mapping and electron energy-loss spectroscopy

The combination of scanning transmission electron microscopy (STEM) and parallel-detection energy-loss spectroscopy (EELS) was used to detect specific bound elements within macromolecules and macromolecular assemblies prepared by direct freezing. After cryotransferring and freeze-drying in situ, samples were re-cooled to liquid nitrogen temperature and low-dose (about 10³ e/nm²) digital dark-field images were obtained with single-electron sensitivity using a beam energy of approximately 100 keV and a probe current of approximately 5 pA. These maps provided a means of characterizing the molecular weights of the structures at low dose. The probe current was subsequently increased to about 5 nA in order to perform elemental analysis. The 320 copper atoms in a keyhole limpet haemocyanin molecule (mol.wt = 8 MDa) were detected with a sensitivity of ± 30 atoms in an acquisition time of 200 s. Phosphorus was detected in an approximately 10-nm length of single-stranded RNA contained in a tobacco mosaic virus particle (mol.wt = 130 kDa/nm) with a sensitivity of ± 25 atoms. Near single-atom sensitivity was achieved for the detection of iron in one haemoglobin molecule (mol.wt = 65 kDa, containing four Fe atoms). Such detection limits are only feasible if special processing methods are employed, as is demonstrated by the use of the second-difference acquisition technique and multiple least-squares fitting of reference spectra. Moreover, an extremely high electron dose (about 10¹⁰ e/nm²) is required resulting in mass loss that may be attributable to ‘knock-on’ radiation damage.     

Progress in multilayer devices as X-ray optical elements

A new kind of mirror based on multilayering techniques gives the possibility of preparing artificial Bragg reflectors over all the X-UV range. The possibility to choose most of the parameters governing the reflectivity opens the possibility to get a very good efficiency, even under normal incidence. Main parameters, evaporating techniques and tests are described. Some example of recent results are compared to the theoretical predictions.     

Two-channel impedance spectroscopy for the simultaneous measurement of two samples

We describe a dielectric relaxation technique, which allows one to obtain a very accurate comparison of the behavior of two different samples. The key feature is the simultaneous impedance measurement on two capacitors that can share a common center electrode, implying that the same voltage is applied to both samples and that only a single gain/phase analyzer is required. The capabilities of this technique have been examined by comparing the dynamics of protonated and deuterated 1-propanol samples using this dual-channel analyzer in the frequency range of 10(-2)-10(6) Hz and in the temperature range of 110-160 K, after calibrating the system using the same sample in both, channel 1 and channel 2. For many supercooled liquids, the high sensitivity of the dielectric relaxation behavior on temperature prevents a meaningful comparison of nearly identical dynamics on the basis of two separate measurements. Based on this dual-channel method, we observe that a deuterated 1-propanol sample displays small but systematic deviations from the relaxation spectra of its protonated counterpart, which would not be observable in separate dielectric measurements. Many other applications can be envisioned where simultaneous or differential impedance measurements are advantageous.     

Characterization of nanophase Al-oxide/Al powders by electron energy-loss spectroscopy

Al nanoparticles were prepared by the inert gas condensation method. After passivation with oxygen and air exposure we obtained a powdered sample of an Al-oxide/Al nanocomposite material. In the present paper we describe the use of the electron energy-loss spectroscopy (EELS) technique in a transmission electron microscope to characterize such nanostructured powders compared with a microcrystalline commercial aluminium foil. Energy-filtered images showed the presence of an alumina overlayer of ≈ 4 nm covering the aluminium nanoparticles (23 nm in diameter). EELS analysis enabled us to determine the total amount of Al₂O₃ and metallic Al and the structure of the alumina passivation overlayer in the sample. In particular, the extended energy-loss fine structure analysis of the data showed a major presence of Al tetrahedrally coordinated with oxygen in the alumina passivation layer of Al nanoparticles instead of the octahedral coordination found for a conventional Al foil. This surprising effect has been attributed to the nanoscopic character of the grains. The analysis of the electron-loss near-edge structure also determines the presence of a certain degree of aggregation in this kind of powdered sample as result of the coalescence of the nanocrystalline grains. The procedure presented here may have the potential to solve other problems during characterization of nanostructured materials.     

Note: electrode polarization of Galinstan electrodes for liquid impedance spectroscopy

Electrode polarization is a significant obstacle in the impedance measurements of ionic liquids. An atomically smooth electrode surface could potentially reduce unwanted impedance contributions from electrode polarization. Liquid metal electrodes were formed by adhering Galinstan to acrylic plates in a parallel-plate capacitor arrangement. Electrode polarization was compared to a similar cell with stainless steel electrodes. The impedance of salt and protein solutions (β-lactoglobulin) was measured from 40 Hz to 110 MHz. Because of oxide layer formation, the performance of the Galinstan electrode is significantly different than the theoretical ideal.     

Characterization of chevron-shaped permalloy magnetic memory elements by four magnetic imaging techniques

Scanning auger microscopy (SAM) and the recently developed scanning electron microscopy with polarization analysis (SEMPA) are easily combined analytical techniques which provide quantitative submicrometer images of X-, Y-, and Z-axis spin polarization components of magnetization. SAM/SEMPA, along with three established magnetic imaging techniques (Bitter colloidal, longitudinal magneto-optic Kerr microscopy, and the Fresnel mode of Lorentz microscopy), was used to characterize a chevron-shaped permalloy magnetic memory element. Reflected light and secondary electrons were used to image the topography. Auger electrons identified and imaged the elemental composition. Reflected light, transmitted electrons, and secondary electrons were used to image the magnetic microstructure. The Bitter colloidal images showed only the delineation of the domain walls, and the longitudinal magneto-optic Kerr microscopy images produced similar results. The Lorentz microscopy images provided the most qualitative magnetization information. SAM/SEMPA was the only technique to combine elemental information and quantitative magnetization information with images having submicrometer resolution.     

Characterization of tribofilms derived from zinc dialkyl dithiophosphate and serpentine by X-ray absorption spectroscopy

The tribological performance of serpentine in combination with ZDDP as additive for base oil was investigated by a Plint high frequency friction tester at room temperature and 100 °C. The tribofilms formed by serpentine and ZDDP were analyzed using the scanning electron microscopy technique equipped with energy dispersive X-ray spectroscopy. X-ray absorption spectroscopy at phosphorus K- and L_3,2-edges, sulfur K- and L_3,2-edges, silicon K-edge, magnesium K-edge, oxygen K-edge, and zinc L_3,2-edge were recorded to determine the chemistry of the tribofilms. It is found that a combination of serpentine with ZDDP helps reduce the friction of oil blend and exhibits better antiwear properties than base oil.     

Single HeLa and MCF-7 cell measurement using minimized impedance spectroscopy and microfluidic device

This study presents an impedance measurement system for single-cell capture and measurement. The microwell structure which utilizes nDEP force is used to single-cell capture and a minimized impedance spectroscopy which includes a power supply chip, an impedance measurement chip and a USB microcontroller chip is used to single-cell impedance measurement. To improve the measurement accuracy of the proposed system, Biquadratic fitting is used in this study. The measurement accuracy and reliability of the proposed system are compared to those of a conventional precision impedance analyzer. Moreover, a stable material, latex beads, is used to study the impedance measurement using the minimized impedance spectroscopy with cell-trapping device. Finally, the proposed system is used to measure the impedance of HeLa cells and MCF-7 cells. The impedance of single HeLa cells decreased from 9.55 × 10(3) to 3.36 × 10(3) Ω and the impedance of single MCF-7 cells decreased from 3.48 × 10(3) to 1.45 × 10(3) Ω at an operate voltage of 0.5 V when the excitation frequency was increased from 11 to 101 kHz. The results demonstrate that the proposed impedance measurement system successfully distinguishes HeLa cells and MCF-7 cells.     

Characterization of an ultraviolet irradiation chamber to monitor molecular photodegradation by Raman spectroscopy

A homemade ultraviolet chamber is reported to induce photochemical changes with characterization by Raman spectroscopy. The equipment has compartments for ultraviolet-A (UV-A) (8 lamps of 8 W) and for UV-A + ultraviolet-B (UV-B) irradiation (4 lamps of 26 W and 1 lamp of 15 W). The irradiance was measured 3, 5, and 10 cm from the light sources. The maximum irradiance was obtained at 3 cm (UV-A: 2.66 mW/cm² and UV-A + UV-B: 4.30 mW/cm²). The chamber internal temperature was stabilized at 30°C after 1 hr of operation with an internal relative humidity of approximately 45%. 10% Collagen was irradiated with UV-A at 2.0 mW/cm² for 3 hr with changes in Raman peaks at 1253, 1271, 1453, and 1660 cm^?1 indicating changes in conformation. 5% Atenolol was irradiated with UV-A + UV-B at 4.30 mW/cm² for 8 hours with changes to Raman peaks at 822, 1186, 1206, 1248, and 1618 cm^?1. A commercial insect repellent was irradiated with UV-A + UV-B at 4.30 mW/cm² for 8 hr and decreases in Raman intensity were observed at 526, 690, 1003, and 1606 cm^?1 due to degradation of N, N-diethyl-m-toluamide. The results demonstrate proper operation of the irradiation chamber with Raman spectroscopic monitoring.     

Characterization of human ovarian teratoma hair by using AFM, FT-IR, and Raman spectroscopy

The structural, physical, and chemical properties of hair taken from an ovarian teratoma (teratoma hair) was first examined by atomic force microscopy (AFM), Fourier transform infrared (FT-IR), and Raman spectroscopy. The similarities and differences between the teratoma hair and scalp hair were also investigated. Teratoma hair showed a similar morphology and chemical composition to scalp hair. Teratoma hair was covered with a cuticle in the same manner as scalp hair and showed the same amide bonding modes as scalp hair according to FT-IR and Raman spectroscopy. On the other hand, teratoma hair showed different physical properties and cysteic acid bands from scalp hair: the surface was rougher and the adhesive force was lower than the scalp hair. The cystine oxides modes did not change with the position unlike scalp hair. These differences can be understood by environmental effects not by the intrinsic properties of the teratoma hair.     

Study on carrier mobility measurement using electroluminescence in frequency domain and electrochemical impedance spectroscopy

In this paper, the two methods, electroluminescence in frequency domain and electrochemical impedance spectroscopy, have been applied to investigate the carrier mobility in single layer polymer light-emitting diode employing the polymer MEH-PPV (Poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) as the light-emitting layer. The carrier mobility μ is 1.64 × 10⁻⁶ cm²/V s under the electric field 8.3 × 10⁵ V/cm measured by the method of electroluminescence in frequency domain. The electrochemical impedance spectroscopy results indicate that the carrier mobility μ is 1.08 × 10⁻⁶ cm²/V s under the electric field 7.5 × 10⁵ V/cm. A significant advantage of the two methods is that both of them can be applied to measure the carrier mobility in the thin film.     

Characterization of the calcification of cardiac valve bioprostheses by environmental scanning electron microscopy and vibrational spectroscopy

Bioprosthetic heart valve tissue and associated calcification were studied in their natural state, using environmental scanning electron microscopy (ESEM). Energy dispersive X‐ray micro‐analysis, X‐ray diffraction, Fourier‐transform infrared and Raman spectroscopy were used to characterize the various calcific deposits observed with ESEM. The major elements present in calcified valves were also analyzed by inductively coupled plasma–optical emission spectroscopy. To better understand the precursor formation of the calcific deposits, results from the elemental analyses were statistically correlated. ESEM revealed the presence of four broad types of calcium phosphate crystal morphology. In addition, two main patterns of organization of calcific deposits were observed associated with the collagen fibres. Energy dispersive X‐ray micro‐analysis identified the crystals observed by ESEM as salts containing mainly calcium and phosphate with ratios from 1.340 (possibly octacalcium phosphate, which has a Ca/P ratio of 1.336) to 2.045 (possibly hydroxyapatite with incorporation of carbonate and metal ion contaminants, such as silicon and magnesium, in the crystal lattice). Raman and fourier‐transform infrared spectroscopy also identified the presence of carbonate and the analyses showed spectral features very similar to a crystalline hydroxyapatite spectrum, also refuting the presence of precursor phases such as β‐tricalcium phosphate, octacalcium phosphate and dicalcium phosphate dihydrate. The results of this study raised the possibility of the presence of precursor phases associated with the early stages of calcification.     

基于浓厚分散系 HANAI 理论的血液温度生物 电阻抗特性量化表征研究

温度是人体的重要机能,血液温度变化监测对人体健康评估尤为重要。本文提出拓展的浓厚分散系HANAI理论,结合生物电阻抗谱,量化表征温度对血液生物电阻抗特性的影响规律,为监测血液温度及相关血液疾病的演变过程提供基础。试验结果表明,随着温度T不断上升,血液的生物电阻抗参数Z~*持续下降;奈奎斯特峰值电阻参数R_c和峰值电抗参数X_c与温度T有良好的线性关系,可描述为R_c=-0.3T+24.14和X_c=0.08T-5.78。将传统HANAI方程进行拓展,并进行多物理场数值模拟,其数值分析、模拟结果与试验结果较好吻合,揭示了血浆电导率σ_p和细胞质电导率σ_c是温度对血液生物电阻抗特性的主要影响因素。本文展示了一种潜在的血液温度监测方法,在临床医学领域或有一定的科研与应用价值。