Spectral emissivity modeling of steel 201 during the growth of oxidation film over the temperature range from 800 to 1100 K in air

This study explores the spectral emissivity modeling of steel 201 during the growth of oxidation film over the temperature range from 800 to 1100 K at 1.5 μm. The radiance coming from the specimen is received by an InGaAs photodiode detector. The specimen temperature is obtained by averaging the two platinum–rhodium thermocouples, which are tightly welded in the front surface of specimen near the measuring area viewed by the detector. The variation of spectral emissivity with the temperature is studied at a given heating time. The variation of spectral emissivity with the heating time is evaluated at a definite temperature. The strong oscillations of spectral emissivity are observed and discussed in detail, which originate from the interference effect between the radiation stemming from the oxidization film on the specimen surface and the radiation coming from the specimen surface. The measurement uncertainties of spectral emissivity contributed only by the surface oxidization are about 3.2–14.1%. At a given heating time, the variation of spectral emissivity with the temperature abides well by a simple analytic functional form. And at a definite temperature, the variation of spectral emissivity with the heating time can also be well reproduced by fitting except for the periodical oscillations.     

Effect of the surface oxidization and nitridation on the normal spectral emissivity of titanium alloys Ti–6Al–4V at 800–1100 K at a wavelength of 1.5 μm

This work strived to model the effect of surface oxidization and nitridation on the normal spectral emissivity of Ti–6Al–4V alloys at a temperature range of 800–1100 K and a wavelength of 1.5 μm. In experiments, the detector was as close to perpendicular to the surface of the specimens as possible so that only the normal spectral emissivity was measured. Two thermocouples were symmetrically welded near the measuring area for accurate measuring and monitoring of the temperature at the surface of the specimen. The specimens were heated for 6 h at a certain temperature. During this period, the normal spectral emissivity values were measured once every 1 min during the initial 180 min, and once every 2 min thereafter. The measurements were made at certain temperatures from 800 to 1100 K in intervals of 20 K. One strong oscillation in the normal spectral emissivity was observed at each temperature. The oscillations were formed by the interference between the radiation stemming from the oxidization and nitridation layer on the specimen surface and radiation from the substrate. The uncertainty in the normal spectral emissivity caused only by the surface oxidization and nitridation was found to be approximately 9.5–22.8%, and the corresponding uncertainty in the temperature generated only by the surface oxidization and nitridation was approximately 6.9–15.5 K. The model can reproduce well the normal spectral emissivity, including the strong oscillation that occurred during the initial heating period.     

Investigation of the effects of Ni-based alloy K465 on the normal spectral emissivity during oxidation

The normal spectral emissivity of Ni-based alloy K465 during oxidation is experimentally measured at 810, 914 and 998 °C for 12 h in air over the wavelength from 1.3 to 2.4 μm. The combined standard uncertainty of the normal spectral emissivity is less than 3%. The oscillations of the emissivity and the effects of oxidation temperature, heating time and wavelength on the emissivity are investigated. The oscillations of the emissivity are formed by the interference effect between the radiation from the surfaces of the substrate and the oxidation film. The oscillation extremums of the emissivity shift towards larger wavelengths as the oxidation process proceeds. The results show that the normal spectral emissivity increases as the temperature increases at the initial time. The normal spectral emissivity decreases as wavelength increases except for the occurrence of the oscillations of the emissivity. The normal spectral emissivity increases rapidly at the initial heating time, and the change of emissivity becomes slow when the oxidation tends to be saturated gradually. Besides, the emissivity fitting models versus heating time and wavelength are established, which fit the experimental results very well. The emissivity relative errors of the fitting models are less than 4%.     

Application of indium tin oxide (ITO) thin film as a low emissivity film on Ni-based alloy at high temperature

Indium tin oxide (ITO) films as the low emissivity coatings of Ni-based alloy at high temperature were studies. ITO films were deposited on the polished surface of alloy K424 by direct current magnetron sputtering. These ITO-coated samples were heat-treated in air at 600–900 °C for 150 h to explore the effect of high temperature environment on the emissivity. The samples were analyzed by X-ray diffraction (XRD), SEM and EDS. The results show that the surface of sample is integrity after heat processing at 700 °C and below it. A small amount of fine crack is observed on the surface of sample heated at 800 °C and Ti oxide appears. There are lots of fine cracks on the sample annealed at 900 °C and a large number of various oxides are detected. The average infrared emissivities at 3–5 μm and 8–14 μm wavebands were tested by an infrared emissivity measurement instrument. The results show the emissivity of the sample after annealed at 600 and 700 °C is still kept at a low value as the sample before annealed. The ITO film can be used as a low emissivity coating of super alloy K424 up to 700 °C.     

Multispectral pyrometry for surface temperature measurement of oxidized Zircaloy claddings

Non-contact temperature measurement in a nuclear reactor is still a huge challenge because of the numerous constraints to consider, such as the high temperature, the steam atmosphere, and irradiation. A device is currently developed at CEA to study the nuclear fuel claddings behavior during a Loss-of-Coolant Accident. As a first step of development, we designed and tested an optical pyrometry procedure to measure the surface temperature of nuclear fuel claddings without any contact, under air, in the temperature range 700–850 °C. The temperature of Zircaloy-4 cladding samples was retrieved at various temperature levels. We used Multispectral Radiation Thermometry with the hypothesis of a constant emissivity profile in the spectral ranges 1–1.3 µm and 1.45–1.6 µm. To allow for comparisons, a reference temperature was provided by a thermocouple welded on the cladding surface. Because of thermal losses induced by the presence of the thermocouple, a heat transfer simulation was also performed to estimate the bias. We found a good agreement between the pyrometry measurement and the temperature reference, validating the constant emissivity profile hypothesis used in the MRT estimation. The expanded measurement uncertainty (k = 2) of the temperature obtained by the pyrometry method was ±4 °C, for temperatures between 700 and 850 °C. Emissivity values, between 0.86 and 0.91 were obtained.     

A self-method for resolving the problem of apparent LWIR emissivity for quantitative thermography up to 130 °C

In a previous work, we succeeded in connecting normal LWIR apparent emissivity to the spectral one of an aluminum nitride ceramic plate. The key problem was the knowledge of the effective spectral bandwidth in use in the system. Hence we have developed an analyzer which permits to identify the spectral bandwidth of IR system using only its raw data. It proceeds by minimizing the dispersion from linearity of the characteristic thermosignals/integrated radiance over a temperature range of the IR system. The capacities of the analyzer are tested for five commercial cameras. Each of these systems exhibits a similar formatting process implemented during the thermogram recording. The effective spectral bandwidth shows plausible values. It varies significantly from one model to the other and the residual non-linearity is connected to the NETD of the IR system. The robustness of the apparent emissivity measurements is also tested with the aid of emissivity reference of 0.5. The overall accuracy of the method is less than 1%, depending on the specular or diffuse part of the reflected irradiation. Applied in field situation, the method is suitable to detect absolute variation of emissivity of less than 6 ⋅ 10⁻³. We use the analyzer to determine the spectral bandwidth of a commercial 320 × 240 microbolometer uncooled IRFPA camera which had already served to characterize the normal LWIR apparent emissivity of the aluminum nitride ceramic plate. By using the spectral response of the two major microbolometer sensor technologies, the general formulation of apparent emissivity matches our apparent emissivity measurements. An agreement better than 0.6% in absolute value and a less than 6 ⋅ 10⁻³%/°C dispersion are found over the entire temperature range [40–130 °C].     

Analysis of multi-band pyrometry for emissivity and temperature measurements of gray surfaces at ambient temperature

A multi-band pyrometry model is developed to evaluate the potential of measuring temperature and emissivity of assumably gray target surfaces at 300 K. Twelve wavelength bands between 2 and 60 μm are selected to define the spectral characteristics of the pyrometers. The pyrometers are surrounded by an enclosure with known background temperature. Multi-band pyrometry modeling results in an overdetermined system of equations, in which the solution for temperature and emissivity is obtained through an optimization procedure that minimizes the sum of the squared residuals of each system equation. The Monte Carlo technique is applied to estimate the uncertainties of temperature and emissivity, resulting from the propagation of the uncertainties of the pyrometers. Maximum reduction in temperature uncertainty is obtained from dual-band to tri-band systems, a small reduction is obtained from tri-band to quad-band, with a negligible reduction above quad-band systems (a reduction between 6.5% and 12.9% is obtained from dual-band to quad-band systems). However, increasing the number of bands does not always reduce uncertainty, and uncertainty reduction depends on the specific band arrangement, indicating the importance of choosing the most appropriate multi-band spectral arrangement if uncertainty is to be reduced. A reduction in emissivity uncertainty is achieved when the number of spectral bands is increased (a reduction between 6.3% and 12.1% is obtained from dual-band to penta-band systems). Besides, emissivity uncertainty increases for pyrometers with high wavelength spectral arrangements. Temperature and emissivity uncertainties are strongly dependent on the difference between target and background temperatures: uncertainties are low when the background temperature is far from the target temperature, tending to very high values as the background temperature approaches the target temperature.     

Preparation of cadmium stannate films by spray pyrolysis technique

Cadmium stannate thin films were prepared by spray pyrolysis technique using cadmium acetate and tin(II) chloride precursors at substrate temperatures 450 °C and 500 °C. XRD pattern confirms the formation of orthorhombic (1 1 1) cadmium stannate phase for the film prepared at substrate temperature of 500 °C, whereas, films prepared at 450 °C are amorphous. Film formation does not occur at substrate temperature from 300 to 375 °C. SEM images reveal that the surface of the prepared Cd₂SnO₄ film is smooth. The average optical transmittance of ∼86% is obtained for the film prepared at substrate temperature of 500 °C with the film thickness of 400 nm. The optical band gap value of the films varies from 2.7 to 2.94 eV. The film prepared at 500 °C shows a minimum resistivity of 35.6 × 10⁻⁴ Ω cm.     

Surface temperature measurement of the plasma facing components with the multi-spectral infrared thermography diagnostics in tokamaks

For the long-pulse high-confinement discharges in tokamaks, the equilibrium of plasma requires a contact with the first wall materials. The heat flux resulting from this interaction is of the order of 10 MW/m² for steady state conditions and up to 20 MW/m² for transient phases. The monitoring on surface temperatures of the plasma facing components (PFCs) is a major concern to ensure safe operation and to optimize performances of experimental operations on large fusion facilities. Furthermore, this measurement is also required to study the physics associated to the plasma material interactions and the heat flux deposition process. In tokamaks, infrared (IR) thermography systems are routinely used to monitor the surface temperature of the PFCs. This measurement requires an accurate knowledge of the surface emissivity. However, and particularly for metallic materials such as tungsten, this emissivity value can vary over a wide range with both the surface condition and the temperature itself, which makes instantaneous measurement challenging. In this context, the multi-spectral infrared method appears as a very promising alternative solution. Indeed, the system has the advantage to carry out a non-intrusive measurement on thermal radiation while evaluating surface temperature without requiring a mandatory surface emissivity measurement.In this paper, a conceptual design for the multi-spectral infrared thermography is proposed. The numerical study of the multi-channel system based on the Levenberg-Marquardt (LM) nonlinear curve fitting is applied. The numerical results presented in this paper demonstrate the design allows for measurements over a large temperature range with a relative error of less than 10%. Furthermore, laboratory experiments have been performed from 200 °C to 740 °C to confirm the feasibility for temperature measurements on stainless steel and tungsten. In these experiments, the unfolding results from the multi-channel detection provide good performance on temperature measurement, which supports our numerical evaluation and demonstrates the potential feasibility for metallic surface high temperature measurement with this method.     

Factors that influence the surface potential decay on a thin film of polyethylene terephthalate (PET)

The initial potential at the surface of the sample, as well as the temperature and the relative humidity of the ambient air are known to influence the surface-potential decay characteristics of corona-charged thin insulating films. The aim of the present work is to demonstrate the effectiveness of the Experimental Design methodology for evaluating the effects of these factors. Thus, a full factorial experimental design was carried out on a thin film of polyethylene terephthalate (thickness: 0.5 mm; surface: 50 mm × 50 mm). A negative corona discharge produced in a needle–grid–plate electrode system was employed to charge the surface of the film samples. The variation domains for the three factors were respectively: ?1000 V to ?1800 V; 25 to 55 °C; 50% to 80%. The surface-potential decay process was characterized by two output variables: the time needed for the potential to reduce to respectively 50% and 10% of the initial value. It was found that the former is more affected by the temperature, while the latter is more sensitive to the variation of the relative humidity.     

The synthesis and characterization of Al/Co3O4 magnetic composite pigments with low infrared emissivity and low lightness

The main challenge of low infrared emissivity coatings based on aluminum flake lies in finding an efficient method to synthesize the composite pigment with low infrared emissivity and low lightness simultaneously. In this work, we overcome this constraint to some extent, synthesizing a novel Al/Co₃O₄ magnetic composite pigments with low infrared emissivity and low lightness by thermal cracking and hot flowing method. The results show that the covering area of Co₃O₄ on the aluminum flake can be tuned by the amount of CoCO₃ adding in precursor and the reaction temperature of hot flowing, both of which pay a key factor on the VIS and IR spectral reflectance and magnetic properties. The magnetic Al/Co₃O₄ composite pigments with low lightness and low infrared emissivity can be obtained at 130 °C for 24 h in hot flowing liquid. The lightness L¹ can be decreased to 69.2, however the infrared emissivity (8–14 μm) is also low to 0.45. Compared with the single Al flakes, Al/Co₃O₄ magnetic composite pigments present stronger magnetic properties. Therefore, the Al/Co₃O₄ magnetic composite pigments have offered new choice for the pigments of low infrared emissivity coatings.     

A super-pixel QWIP focal plane array for imaging multiple waveband temperature sensor

The multi-waveband temperature sensor (MWTS) array, in which each super-pixel (2 × 2 pixel cell) operates at four distinct thermal infrared (IR) wavebands is being developed. Using this high spatial resolution, four-band thermal IR band detector array, accurate temperature measurements on the surface of an object can be made without prior knowledge of its exact emissivity. This multi-band detector involves intersubband transition in III–V semiconductor-based quantum layered structures. Each detector stack absorbs photons within the specified wavelength band while allowing the transmission of photons in other spectral bands, thus efficiently permitting multi-band detection. This produces multiple, spectrally resolved images of the scene that are recorded simultaneously in a single snapshot on the FPA. From the multispectral images and calibration information about the system, computational algorithms are used to evaluate the temperature on the surface of a target.     

Fabrication of Gd0.5Sr0.5CoO3 film for SOFC cathode by pulsed laser deposition

Gd_0.5Sr_0.5CoO₃ (GSCO) film has been fabricated by pulsed laser deposition (PLD) to be used as the cathode of the solid oxide fuel cell (SOFC). The GSCO thin film obtained has a columnar crystalline structure so that it will have a high permeation property. The PLD technique has been found suitable for growing a film of complex composition because of its good control of stoichiometry and thus for fabricating a GSCO film used as the cathode of the SOFC. The GSCO film has been studied for porosity electrical conductivity and power density. The GSCO film grown at a substrate temperature of 1100 K and oxygen gas pressure of 100 Pa has high electrical conductivity which is 820 S cm^− 1 at 973 K with post annealing at a rather low temperature (1000 K). This value is higher than that of the GSCO film prepared by RF-sputtering with post annealing at a higher temperature (1273 K).     

Quantum well earth science testbed

A thermal hyperspectral imager is underdevelopment which utilizes the compact Dyson optical configuration and the broadband (8–12 μm) quantum well infrared photodetector (QWIP) focal plane array technology. The Dyson configuration uses a single monolithic prism-like grating design which allows for a high throughput instrument (F/1.6) with minimal ghosting, stray light and large swath width. The configuration has the potential to be the optimal high resolution imaging spectroscopy solution for aerial and space remote sensing applications due to its small form factor and relatively low power requirements. The planned instrument specifications are discussed as well as thermal design trade-offs. The current design uses a single high power cryocooler which allows operation of the QWIP at 40 K with adequate temperature stability.Calibration testing results (noise equivalent temperature difference, spectral linearity and spectral bandwidth) and laboratory emissivity plots from samples are shown using an operational testbed unit which has similar specifications as the final airborne system. Field testing of the testbed unit was performed to acquire plots of emissivity for various known standard minerals (quartz, opal, alunite). A comparison is made using data from the ASTER spectral library. The current single band (8–9 μm) testbed utilizes the high uniformity and operability of the QWIP array and shows excellent laboratory and field spectroscopic results.     

Fourier transform measurements of SO2 absorption cross sections:: I. Temperature dependence in the 24 000–29 000 cm−1 (345–420 nm) region

Absorption cross sections of SO₂ have been obtained in the 24 000–29 000 cm^?1 spectral range (345–420 nm) with a Fourier transform spectrometer at a resolution of 2 cm^?1. Pure SO₂ samples were used and measurements were performed at room temperature (298 K) as well as at 318, 338 and 358 K. This is the first time that temperature effects in this spectral region are reported and investigated. This paper is the first of a series that will report on measurements of the absorption cross section of SO₂ in the UV/visible region at a higher than previously reported resolution and that will investigate temperature effects in support of tropospheric, stratospheric and astrophysical or planetary applications.     

Microstructures and nano mechanical properties of the metal tungsten film

The W film was prepared on 1045 steel by magnetron sputtering, with the thickness of 2 μm, its surface and cross-section morphologies were investigated with SEM, and the phase structure was analyzed with XRD. X-ray stress determinator was utilized to measure its residual stress, and the nano-hardness and elastic modulus of the film were surveyed by nano-indentation tester. The results show that the surface of W film is very compact and smooth; the particles arranged regularly, the granularity of the thin film is about 1 μm. The microcracks, cavities and desquamation were not found in the film and interface, and the bonding between the W film and substrate is well. The XRD results showed that the W film had a body-centered cubic structure, the lattice constant: a = 0.316 nm, the growth preferred orientations are (1 1 0) and (2 2 0). The compressive stress (−169 MPa) was found on the surface. The average nano-hardness and elastic modulus of W film are 15.22 GPa, 176.64 GPa, respectively, and the mechanical properties of W film are well.     

Irreversible nanoscale morphology transformation of an Fe film on Mo(1 1 0) induced by a magnetic STM tip

STM tip-induced surface roughening is reported for a 6 Å Fe film grown on vicinal Mo(1 1 0) at 760 ± 15 K. Using a STM tip of the antiferromagnetic alloy MnNi and tunneling parameters of 0.1 nA and 70 mV, the film morphology was completely transformed over a period of 1 h at room temperature. The results indicate that there is a strong promotion of surface diffusion and interlayer mass transport by the local electric field between the tip and sample and/or a magnetic interaction between the tip and the film. The strain state of the film plays a part in the propagation of this transformation across the scanned area.     

Effect of annealing temperature on the characteristics of ZnO thin films

Effect of annealing temperature on characteristics of sol–gel driven ZnO thin film spin-coated on Si substrate was studied. The UV–visible transmittance of the sol decreased with the increase of the aging time and drastically reduced after 20 days aging time. Granular shape of ZnO crystallites was observed on the surface of the films annealed at 550, 650, and 750 °C, and the crystallite size increased with the increase of the annealing temperature. Consequently nodular shape of crystallites was formed upon increasing the annealing temperature to 850 °C and above. The current–voltage characteristics of the Schottky diodes fabricated with ZnO thin films with various annealing temperatures were measured and analyzed. It is found that, ZnO films showed the Schottky characteristics up to 750 °C annealing temperature. The Schottky diode characteristics were diminished upon increasing the annealing temperature above 850 °C. XPS analysis suggested that the absence of oxygen atoms in its oxidized state in stoichiometric surrounding, might be responsible for the diminished forward current of the Schottky diode when annealed above 850 °C.     

Effect on thermoluminescence parameters of biotite mineral due to thermal quenching

The Thermally Stimulated Luminescence (TSL) at room temperature X-ray irradiated natural biotite in form of micro-grain powder was studied under various heating rates. TSL peaks showed at temperatures 393 K, 399.6 K, 403.5 K, 404.5 K, 406.9 K at their respective heating rates 2 K/s, 4 K/s, 6 K/s, 8 K/s and 10 K/s. The effect of thermal quenching on thermoluminescence parameters such as peak maximum temperature, peak area, FWHM, geometrical symmetry factor, the activation energy were investigated. From the symmetry factor it is clear that the TL glow curve follows the first order kinetics for the lowest heating rate, but as the heating rate increases it defers from the first order. The activation energies for each heating rates were calculated by using Chen peak shape methods for general order kinetics and found to be decreased for higher heating rates. When activation energy is calculated by variable heating rate method it is observed that the method overestimated the value of activation energy and pre-exponential frequency factor significantly due to thermal quenching.     

Ellipsometric detection of GaAs(0 0 1) surface hydrogenation in H2 atmosphere

Optical properties of MBE-grown GaAs(0 0 1) surfaces have been studied by spectroscopic ellipsometry under dynamic conditions of ramp heating and cooling after desorption of passivating As-cap-layer with low pressure H₂ atmosphere (14 Torr) applied to the surface. The temperature dependence of GaAs pseudo-dielectric function with atomically smooth (0 0 1) surface carrying the fixed Ga-rich (4 × 2) reconstruction was obtained for the temperature range of 160–600 °C. It is shown ellipsometrically that GaAs(0 0 1) heating in the molecular hydrogen atmosphere results in the formation of hydrogenated layer on the surface.