Use of a higher order Heydemann–Welch model to characterize a controlled clearance piston gauge

We present a new method for characterizing a controlled-clearance piston gauge as a primary pressure standard. This method requires operating the piston gauge to jacket pressures of over 80% of the system pressure. We present measurements on a hydraulic piston gauge with a 290 MPa maximum pressure and a nominal piston diameter of 3.27 mm. Measurements showed that the cylinder becomes stiffer as the jacket pressure increases, and that non-linear models of the Heydemann–Welch parameters improve the determination of the effective area. The relative standard uncertainty in the effective area of the piston gauge ranges from 16.0 × 10⁻⁶ to 17.6 × 10⁻⁶, and the agreement to the present NIST pressure scale is within the standard uncertainty.     

A DOE nano-tribological study of thin amorphous carbon-based films

A design of experiment (DOE) matrix of 150 nm non-hydrogenated amorphous C and Cr doped amorphous C films was produced to investigate the effect of four key coating process parameters (use of an adhesion layer, Cr magnetron current, cathodic substrate bias voltage and Ar flow to the chamber) using a new rapid method of nano-scale wear test under conditions relevant to MEMS and similar devices. The condition of nano-wear was produced by controlled oscillation of the sample mounting within a nanoindentation system under ultra-low normal load. Specific wear rates were low, typically in the range 6-24×10⁻¹⁷ m³ N⁻¹ m⁻¹. The results were processed using an analysis of variance (ANOVA) procedure which showed that: hardness was reduced in the Cr containing films whilst specific wear rate and data scatter increased, increasing the cathodic substrate bias voltage reduced the specific wear rate due to increased coating hardness, the use of a Cr adhesion layer reduced the specific wear rate and scatter of results with Cr doped films but had no effect on pure a-C films, and Ar flow rate had no significant effect on specific wear rate but strongly interacted with the effect of the cathodic bias voltage.     

A study on fretting fatigue characteristics of Inconel 690 at high temperature

Inconel 690 alloy is used in nuclear power plant steam generator tubes. Fretting fatigue experiments were performed on Inconel 690 specimens at room temperature and at the nuclear power plant operating temperature of 320 °C. By comparing the fretting fatigue test data at room temperature and 320 °C, this study analyzed the change in characteristics related to the fatigue limit at 10⁷ cycles. In addition, this study attempted to measure changes in the friction force for repetitive cycles in fretting fatigue tests, and analyzed the mechanism of fretting fatigue by observing the fracture surfaces and performing spectrum analysis.     

Study of tribological performance of ECR-CVD diamond-like carbon coatings on steel substrates: Part 2. The analysis of wear mechanism

This paper describes the tribological performance of diamond-like carbon (DLC) coatings deposited on AISI 440C steel substrates by electron cyclotron resonance chemical vapor deposition (ECR-CVD) process. A variety of analytic techniques were used to characterize the coatings, such as Raman spectroscopy, atomic force microscopy (AFM) and nano-indentation. The sliding wear and friction experiments were carried out by the conventional ball-on-disk tribometry against 100Cr6 steel counterbody at various normal loads (1-10 N) and sliding speeds (2-15 cm/s). All the wear tests were conducted under dry sliding condition in ambient air for a total rotation cycle of 1 × 10⁵ (sliding distance ∼2.2 km). Surfaces of the coatings and the steel balls were examined before and after the sliding wear tests. The DLC coatings that had been tested all showed relatively low values of friction coefficient, in the range of 0.1-0.2 at a steady-state stage, and low specific wear rates (on the order of 10⁻⁸ mm³/Nm). It was found that higher normal loads or sliding speeds reduced the wear rates of the coatings. Plastic deformation became more evident on the coating surface during the sliding wear test at higher contact stresses. The friction-induced transformation of the coating surface into a graphite-like phase was revealed by micro-Raman analysis, and the flash temperature of the contact asperities was estimated. It was suggested that the structural transformation taking place within the wear tracks was mainly due to the formation of compact wear debris layer rather than the frictional heating effect. On the other hand, an adherent transfer layer (tribolayer) was formed on the counterface, which was closely related to the steady-state friction during sliding and the wear mechanisms. Fundamental knowledge combined with the present tribological study led to the conclusion that adhesive wear along with abrasion was probably the dominant wear mechanism for the DLC/steel sliding systems. Additionally, fatigue processes might also be involved in the wear of the coatings.     

Improved system for the automatic calibration of standard resistors in the meg-ohm range

An automated measuring system has been developed to improve the calibration of high value standard resistors in the meg-ohm range at the National Institute for Standards (NIS), Egypt. This system is suitable for the calibration of the standard resistors from 100 kΩ to 100 MΩ using the DMM-based method by the substitution technique where the unknown resistor and the standard resistor are indirectly compared in the same position using a dummy resistor as a short-term reference standard. The system operation is automatically controlled by using a Lab VIEW program which is especially developed for this purpose. The uncertainty for the high value standard resistors measurement of this system is estimated. The performance of this system is also evaluated by comparing the measurement results obtained from this technique with those obtained by the direct comparison DMM-based method. It is found that the measurement uncertainty of with this method spans from 4.1 × 10⁻⁶ to 27 × 10⁻⁶, while it spans from 40 × 10⁻⁶ to 110 × 10⁻⁶ for the direct comparison method. The relative differences of the deviation from nominal values of the working standards resistors measured by the two methods are found to be within their expanded uncertainties.     

Thermal sensors based on p-Pb0.925Yb0.075Te:Te and n-Pb0.925Yb0.075Se0.2Te0.8 thin films grown using thermal evaporation method

We utilize p-Pb_0.925Yb_0.075Te:Te and n-Pb_0.925Yb_0.075Se_0.2Te_0.8 ingots in a standard solid-state microwave synthesis route to fabricate thermally evaporated thin films. The nanostructure and composition of the films were studied through X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and energy dispersive X-ray spectroscopy (EDX). The Seebeck coefficient and electrical conductivity were measured at a temperature range of 298–523 K. The micro-thermoelectric devices were composed of 20 pairs and 10 pairs of p-Pb_0.925Yb_0.075Te:Te and n-Pb_0.925Yb_0.075Se_0.2Te_0.8 thin films on glass substrates, respectively. The dimensions of the thin films thermoelectric generators which comprised of 10-pair were 12 mm × 10 mm, whereas, 20-pair were 23 mm × 20 mm, respectively of legs connected through aluminum electrodes. The serial 20-pair p–n thermocouples generated a maximum output open-circuit voltage of 275.3 mV and a maximum output power of 54.37 nW at a temperature difference of ΔT = 162 K; the values are 109.4 mV and 16.68 nW at ΔT = 162 K for the 10-pair thermocouples, respectively.     

Research on the fretting wear behavior of silicon wafers before and after carbon ions implantation

Carbon ions with different doses of 2×10¹⁵ and 2×10¹⁶ ions/cm² were implanted into single crystal silicon wafers under an energy level of 80 keV. The nanohardness and elastic modulus of silicon wafers were studied on the nano-mechanical testing system. The fretting wear tests were performed on the UMT-2 Micro-tribometer to evaluate the fretting wear resistance of C⁺ implanted silicon wafer and to investigate its micro-tribological properties. The results demonstrate that the nanohardness and elastic modulus of silicon wafer with dose of 2×10¹⁵ ions/cm² decreased and those of 2×10¹⁶ ions/cm² changed little. Implanted silicon wafer with dose of 2×10¹⁶ ions/cm² had much lower coefficient of friction and wear volume under low loads, which suggests a significant effect of friction-reducing and anti-wear. The results also indicate that abrasive wear was the main wear mechanism for both virgin silicon and C⁺ implanted silicon with dose of 2×10¹⁵ ions/cm². However, adhesive wear played a significant role in the wear mechanism of the C⁺ implanted silicon with dose of 2×10¹⁶ ions/cm² under the low loads, while the abrasive wear dominated the wear mechanism under high loads.     

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.     

A Josephson voltage-traceable DC high-voltage divider evaluation using the binary step-up method

An evaluation technique and traceability for a DC-resistive high-voltage divider was established based on 1 kV, which was traceable to a Josephson voltage standard at the Korea Research Institute of Standards and Science. To do this, the binary step-up method was used to evaluate the voltage-dividing ratio and the voltage coefficient of the divider up to 100 kV. The expanded relative uncertainty for the dividing ratio up to 100 kV was 16 × 10⁻⁶ level. To confirm the validity of the method, the ratio at 1 kV was compared with the resistance ratio of the divider, and the two results agreed to within 5.3 × 10⁻⁶.     

Distributed amplified ultra-stable signal quartz oscillator based

The aim of this communication is to present the performances of 5 MHz distributed ultra-stable system, based on ultra-stable Boitiers à Vieillissement Amélioré (BVA) oscillator. We demonstrated flicker frequency modulation (FFM) floor better than 4.5 × 10⁻¹⁴ ± 2.5 × 10⁻¹⁵ at 12 s with an intrinsic noise floor about 6 × 10⁻¹⁵ at 1 s with a τ^−1/2 time integration dependence slope.     

INRIM primary standard for microgas-flow measurements with reference to atmospheric pressure

Primary standard flowmeters are developed for the calibration of leak devices used in many applications in which is necessary to detect and quantify gas leakage from a material, a component or a system. At INRIM, a primary standard was designed and realized for the measurement of molar gas flow from 4 × 10⁻¹⁰ mol/s to 2 × 10⁻⁷ mol/s with reference to atmospheric pressure. It is based on the constant-pressure–variable-volume method and is able to work with any tracer gas.     

1–15,000 Pa Absolute mode comparisons between the NIST ultrasonic interferometer manometers and non-rotating force-balanced piston gauges

The National Institute of Standards and Technology (NIST) Low Pressure Manometry Project maintains and operates primary standard ultrasonic interferometer manometers (UIMs) over the pressure range of 1 mPa to 360 kPa. Over the past decade a new type of customer gauge, the non-rotating force-balanced piston gauge or FPG (model 8601, DH Instruments, a Fluke Company¹) has been introduced to the standards community that covers the range of ≈1–15,000 Pa and is capable of both absolute and differential measurement modes. Since 2002, NIST customers² have requested that four different FPG units be compared to the NIST primary pressure ultrasonic interferometer manometer standards (UIMs). The results of the comparisons were that all four FPG units were within manufacturers stated uncertainty (0.008 Pa + 30 × 10⁻⁶ × P for absolute mode) when compared against the NIST UIMs at pressures between 10 Pa and 15,000 Pa (absolute mode). At pressures between 5 Pa and 10 Pa, the results were generally within manufacturer’s specifications. Below 5 Pa some of the FPG units were outside of manufacturer’s uncertainty specifications. The use of an isolating capacitance diaphragm gauge (CDG) was necessary during the comparisons to prevent humidified gas from the FPG from entering the NIST 160 kPa mercury UIM primary pressure standard. The results of these four different comparison tests will be discussed in detail, along with test conditions, equipment set-up, and test uncertainty analysis.     

Measurement uncertainty estimation of health risk from exposure to natural radionuclides in soil

Cancer mortality risk were estimated due to external exposure to ⁴⁰K in soil. Uncertainty estimation was performed for the risk considered as a measurand. It was presented uncertainty estimation using two methods. One method is based on the Guide to the Expression of Uncertainty in Measurement Framework (GUF) and other represents Monte Carlo method. For the Monte Carlo method, the mean of the obtained distribution that represents mortality cancer risk estimation, due to one year exposure to ⁴⁰K with mean activity concentration of 708 Bq/kg in soil, is 12.9 × 10⁻⁶ with 90% confidential interval (k ≈ 1.64) of (4.7–25.5) × 10⁻⁶. According to GUF the mean value is estimated as 10.9 × 10⁻⁶, with 90% confidential interval of (0.9–20.8) × 10⁻⁶. Uncertainty of assessed risk obtained by numerical simulation is slightly different with asymmetrical boundaries related to the mean value, comparing to the uncertainty estimated using GUF.     

Study of structures at the boundary and defects in organic thin films of perchlorocoronene by high-resolution and analytical transmission electron microscopy

Both the periodic and non-periodic structures of perchlorocoronene (C₂₄Cl₁₂) crystals were characterized by high-resolution transmission electron microscopy (HRTEM), electron diffraction (ED), electron energy-loss spectroscopy (EELS), and energy-filtered transmission electron microscopy (EFTEM). The HRTEM images at the boundary of the C₂₄Cl₁₂ crystals exhibit the flexibility of defect structures, where molecules align to compensate for the discontinuity between two different domains. Emphasized by the filtered images, it was found that the non-periodic regions are created everywhere with a small electron beam irradiation (∼10⁶ electrons nm⁻²) and then spread over the entire regions to completely destroy the periodic structures after a higher electron dose (∼2×10⁶ electrons nm⁻²). The effect of the electron beam irradiation was monitored by ED, EELS, and EFTEM, where periodic structures and content elements are well preserved up to 10⁶ electrons nm⁻², but chlorine atoms decreased with a much higher electron dose. This is explained by the breakage of the C–Cl bond to detach chlorine atoms, confirmed by energy-loss near the edge structures (ELNES) of carbon π? peaks and chlorine loss at the edge of the specimen, as well as by theoretical simulation. The detachment of chlorine is localized at the peripheral edge around a hole confirmed by core-loss EFTEM imaging.     

The effect of fretting on the fatigue behaviour of plasma nitrided stainless steels

The plain fatigue and fretting fatigue behaviour of a plasma nitrided dual phase stainless steel known as 3CR12 and an AISI 316 austentic stainless steel have been studied in the present work, using a modified Wohler rotating-bending configuration. Test specimens were produced at two nitriding temperatures, namely 400 and 520 °C, representing low temperature and conventional nitriding temperature, respectively. The test results demonstrate that both nitriding processes can enhance the plain fatigue limit of these steels by approximately 10-25%, with the high temperature process being slightly more effective. Under fretting fatigue conditions, the beneficial effect of plasma nitriding is even more significant and the fretting fatigue limit is increased between 50 and 100% for 3CR12 and at least 50-150% for the AISI steel as the nitriding temperature is raised from 400 to 520 °C.     

Electroanalysis of ascorbic acid using poly(bromocresol purple) film modified glassy carbon electrode

We report a simple method for determination of ascorbic acid (AA) by using a glassy carbon electrode (GCE) modified with poly(bromocresol purple) (poly(BCP)/GCE). Compared with a bare GCE, the poly(BCP) film exhibited the obvious electrocatalytic effect towards ascorbic acid oxidation, which reduced the oxidation overpotential about 240 mV with obviously increased current response. Under the optimized conditions, the catalytic current increased linearly with the concentration of AA in the range of 2.0 × 10⁻⁵–7.0 × 10⁻⁴ M with the detection limit of 6.5 × 10⁻⁶ M (S/N = 3) in 0.1 M phosphate buffer solution (pH 6.5). The interferences from different species and the repeatability of the poly(BCP)/GCE for the determination of AA were also investigated. The proposed method has been successfully applied to the determination of AA in vitamin C injection and tablet with satisfactory results.     

Metrological characterization of the new 1 MN force standard machine of NPL India

Since November 2010, NPL India’s force scale has been complemented in the range from 10 kN to 1 MN by a further force standard machine. This automatically working 1 MN force standard machine utilizes a lever amplification of a 100 kN mass stack and enables low relative expanded uncertainties of smaller than 9 × 10⁻⁵ on the lever, and 2 × 10⁻⁵ on the deadweight side. In this paper, the constructional design of the machine is described. According to the new EURAMET Calibration Guide, a model for the uncertainties is developed.Supplementary to this, results from comparison measurements of the new NPL India machine with PTB´s force standard machines are presented.     

Hamon 10 × 100 MΩ resistor based traceable source for calibration of picoammeters in the range 100 pA–100 nA

This paper describes a measurement method developed at National Institute of metrological Research (INRIM) to calibrate picoammeters in dc current from 100 pA to 100 nA. The current source is based on a traceable to the dc resistance national standard 10 × 100 MΩ Hamon resistor developed at INRIM and on a traceable to the dc voltage national standard high precision dc voltage calibrator. The expanded uncertainties of the method for the calibration of picoammeters span from 9.4 × 10⁻⁴ for the gain of a picoammeter at 100 pA to 4.0 × 10⁻⁴ for the gain at 100 nA. A detailed uncertainties budget at 10 nA level and the results of a comparison with a different technique are also reported.     

Thermal diffusivity measurement of Au nanofluids of very low concentration by using photoflash technique

In this paper, the application of photoflash technique to measuring the thermal diffusivity of gold nanofluids of very low concentration at room temperature was presented. The nanofluid samples were prepared from the pulse laser ablation procedure. The thermal diffusivity was obtained by fitting the theoretical temperature signal to the experimental data, and it was found to increase linearly from 1.47 × 10⁻³ cm² s⁻¹ to 1.68 × 10⁻³ cm² s⁻¹ as the concentration increased from 1.11 mg/L to 3.18 mg/L. The increase in thermal diffusivity in these multidispersed nanofluids was attributed to the higher nanoparticle concentration as well as to the increasing presence of the smaller size nanoparticles.