Experimental study of the relationships between the spectral emissivity of brass and the temperature in the oxidizing environment

Effect of surface oxidization on the spectral emissivity of brass is studied over the temperature range from 800 to 1070 K at the wavelength of 1.5 μm. The temperature of brass surface is measured by averaging the two R-type platinum–rhodium thermocouples. The radiant energy emitted by the brass surface is received by an InGaAs photodiode detector. Two kinds of relationships between the spectral emissivity and the temperature are investigated in the oxidizing environment at the elevated temperature. One is the variation of spectral emissivity with the heating-duration time at the given temperature. The other is the variation of spectral emissivity with the temperature at the given heating-duration time. The interference effect of radiation coming from the brass surface and coming from the oxidization film is discussed when the oxidation film on the surface is grown. The resonant structures of spectral emissivity are observed during the whole heating period, in particular at the early stage of heating duration. The analytic formula of spectral emissivity versus the temperature is derived at the heating-duration time of 30, 60, 90, 120, 150, 180, 210, 240, 270 and 300 min, respectively. The conclusion is obtained that coefficients of analytic expressions between the spectral emissivity and the temperature are different from each other for the experimental results obtained at the different heating-duration time, though the polynomial functional form is suitable to fit all the measurements obtained in the present work.     

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%.     

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.     

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.     

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].     

纯钨红外光谱发射率特性研究

光谱发射率是一个重要的热物性参数,在辐射测温、热传输计算等领域有着广泛的应用。钨作为一种重要的金属,关于其光谱发射率的研究报道较少。利用黑体炉、傅里叶红外光谱仪、加热装置和光学系统搭建了一套能量对比法光谱发射率测量装置,该装置能够测量3~20μm的光谱发射率,测量装置的整体不确定度优于5%。利用该装置测量了纯钨在4个温度点(573, 673, 773和873 K)的法向光谱发射率,重点探讨了氧化、温度、波长和加热时间对纯钨光谱发射率的影响。研究结果表明:纯钨在表面未氧化的情况下,光谱发射率在几个温度点的变化规律基本一致,且数值相差较小,而当其表面发生氧化后光谱发射率迅速增加,在某些波长处出现了强烈的振荡。表面未氧化时纯钨的光谱发射率受温度的影响较小,随着温度的增加仅出现微小的增加,但是当表面发生氧化后,随温度的升高而迅速增大。纯钨的光谱发射率整体上随着波长的增加而减小,但是当表面发生氧化后,由于表面氧化膜与钨金属基底发生干涉效应,在4, 9, 12.5和16.5μm处均出现了峰值。在573和673 K,纯钨的光谱发射率随着加热时间的增加无明显变化。然而,随着温度的升高,在773和873 K时,光谱发射率随着加热时间增加而增大,在773 K时光谱发射率随加热时间的增加增幅较大,因为在该温度点,纯钨表面刚开始发生氧化,氧化速率较大,在873 K时光谱发射率随加热时间的增加增幅较为平缓,并且随着加热时间的增长呈现稳定的趋势。综上,纯钨的光谱发射率在温度较低和表面未氧化时较为稳定。随着温度的升高,当表面发生氧化后,光谱发射率迅速增大,并且在多个波长位置出现了强烈的振荡。由此可见,纯钨光谱发射率受温度、波长、加热时间的影响较大,在实际应用过程中,特别是在辐射测温过程中,如果把纯钨的光谱发射率看做常数将会带来较大的测量误差。该研究将进一步丰富钨的光谱发射率数据,并为其在科学研究和应用中提供数据支持。     

Development and integration of near atmospheric N2 ambient sputtered Au thin film for enhanced infrared absorption

The exceedingly fragile nature of thermally grown Au-black coating makes handling and patterning a critical issue. Infrared absorption characteristics of near atmospheric, N₂ ambient DC sputtered Au thin films are studied for this purpose. The thin Au films are sputtered at different chamber pressures in Ar and N₂/Ar gas ambient from 4.5 to 8.0 mbar and optimized for enhanced infrared absorption. The absorber film sputtered in N₂/Ar ambient at 8.0 mbar chamber pressure offers significant absorption of medium to long wave infrared radiations. The micro-patterning of sputtered Au thin film is carried out by using conventional photolithography and metal lift off methods on a prefabricated µ-infrared detector array on Si (1 0 0) substrate. The steady state temperature response of sputtered film has been examined using nondestructive thermal imaging method under external heating of the detector array.     

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.     

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.     

Characteristics of silicon oxide thin films prepared by sol electrophoretic deposition method using tetraethylorthosilicate as the precursor

Silicon dioxide films were prepared on p-type Si (1 0 0) substrates by sol electrophoretic deposition (EPD) using tetraethylorthosilicate (TEOS) at low temperature. According to the variation of sol dipping conditions, we estimated the characteristics of SiO₂ films, such as composition, surface morphology, wet etch rate, breakdown voltage, etc. The growth rate of the film increased linearly with increasing TEOS quantity in solution. It increased exponentially with the increase in deposition time, and the film thickness was saturated at approximately 200 nm on hydrophilic Si surface after more than 6 days. The growth rate of the EPD SiO₂ films on the hydrophobic Si surface was much lower than that of the film on the hydrophilic Si surface.     

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.     

Spectral properties of an UV fused silica within 0.8 to 5 µm at elevated temperatures

A thermal radiative inverse method was used to determine the high-temperature spectral properties of an ultraviolet fused silica from transmittance data for wavelengths from 0.8 to 5 µm. A developed FTIR system used to measure apparent transmittances of the fused silica sample has been designed and built. In order to reduce the system error caused by detector emission and stray radiation, a measurement strategy at high temperatures was proposed. For deriving spectral transport properties from experimental transmittances, the parameter identification principle was described. The results show that spectral properties are both wavelength dependent and temperature dependent. Spectral refractive indexes rise with increasing temperature and decrease with wavelength. Three absorption peaks of spectral absorptive indices respectively at about 1.4 µm, 2.22 µm and 2.75 µm shift toward the far infrared region and vary differently with increasing temperature. In addition, three absorption bands all become broader for temperatures from 20 °C to 900 °C.     

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.     

Image quality of microns-thick specimens in the ultra-high voltage electron microscope

Image quality of MeV transmission electrons is an important factor for both observation and electron tomography of microns-thick specimens with the high voltage electron microscope (HVEM) and the ultra-HVEM. In this work, we have investigated image quality of a tilted thick specimen by experiment and analysis. In a 3 MV ultra-HVEM, we obtained transmission electron images in amplitude contrast of 100 nm gold particles on the top surface of a tilted 5 μm thick amorphous epoxy-resin film. From line profiles of the images, we then measured and evaluated image blurring, contrast, and the signal-to-noise ratio (SNR) under different effective thicknesses of the tilted specimen and accelerating voltages of electrons. The variation of imaging blurring was consistent with the analysis based on multiple elastic scattering. When the effective thickness almost tripled, image blurring increased from ～3 to ～20 nm at the accelerating voltage of 3 MV. For the increase of accelerating voltage from 1 to 3 MV in the condition of the 14.6 μm effective thickness, due to the reduction of multiple scattering effects, image blurring decreased from ～54 to ～20 nm, and image contrast and SNR were both obviously enhanced by a factor of ～3 to preferable values. The specimen thickness was shown to influence image quality more than the accelerating voltage. Moreover, improvement on image quality of thick specimens due to increasing the accelerating voltage would become less when it was further increased from 2 to 3 MV in this work.     

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.     

On the stability of the spectral responsivity of cryogenically cooled photoconductive HgCdTe infrared detectors

The spectral responsivity of cryogenically cooled HgCdTe detectors was observed to drift slowly with time. The magnitude of the drift was shown to be strongly dependent on wavelength. The origin of the drift was investigated and was shown to arise due to a thin film of water ice depositing on the active area of the cold detector. The presence of the ice film (which is a dielectric film) interacts with the detector structure thus altering its absorbance characteristics and gives rise to the observed drifts. The drifts were temporarily eliminated by evacuating the detector dewars while baking them at 50 °C for about 48 h. This work demonstrates that HgCdTe infrared detectors should be evacuated and baked at least annually and in some cases (depending on the quality of the dewar and the measurement uncertainty required) more frequently. These observations are particularly relevant to HgCdTe detectors mounted in dewars which utilise rubber O-rings, as the ingress of moisture was found to be particularly serious in this type of dewar. This paper also identified other sources of drift present in the output of cryogenically cooled photoconductive HgCdTe detectors whose origins are currently not understood.     

Electronic properties of the polycrystalline tin dioxide interface with conjugated organic layers

The results on the electronic structure of the unoccupied electronic states of the polycrystalline SnO₂ in the energy range from 5 eV to 25 eV above the Fermi level are presented. The modification of the electronic structure and of the surface potential upon deposition of the ultrathin films of copper phthalocyanine (CuPc) and of perylene tetracarboxylic acid dianhydride (PTCDA) film onto the SnO₂ surface were studied using the very low energy electron diffraction (VLEED) method and the total current spectroscopy (TCS) measurement scheme. A substantial attenuation of the TCS signal coming from the SnO₂ surface was observed upon formation of a 1.5–2 nm thick organic deposit layer while no new spectral features from the deposit were distinguishable. It was observed that the electronic structure typical for the organic films was formed within the organic deposit thickness range from 2 nm to 7 nm. The interfacial charge transfer was characterized by the formation of the polarization layer up to 5 nm thick in the organic films. The PTCDA deposition on SnO₂ was accompanied by the negative charge transfer onto the organic layer and to the 0.65 eV increase the surface work function. At the CuPc/SnO₂ interface, the negative charge was transferred to the SnO₂ surface and the overall surface work function decreased by 0.15 eV.     

Effect of sample temperature on laser-induced breakdown spectroscopy

The effect of initial sample temperature on spectral emission of laser-induced plasma has been investigated. The plasma has been produced on aluminum alloy surface at ambient air pressure. The sample has been uniformly heated by a heating element up to 150 °C. The spectral emission of aluminum at different initial sample temperature and gate delay times has been measured. A simple model has been improved in order to compare the analytical and experimental results. An increase in sample temperature leads to an increase in the area under spectral line profiles. The results suggest that increasing the sample temperature can improve the limits of detection (LOD).     

温度和加热时间对大气环境中纯铁光谱发射率的影响

纯铁的光谱发射率受温度的影响很大,尤其是在大气环境中,由于温度升高加剧了表面的氧化,导致其光谱发射率发生了“无规律”变化。基于基尔霍夫定理,利用研制的反射法光谱发射率测量装置对纯铁1.55μm波长的光谱发射率进行了系统的研究,探讨了温度、加热时间等因素对纯铁光谱发射率的影响。研究结果表明：纯铁的光谱发射率随着温度的升高而增大,并且在一定的温度下出现了峰值和谷值,通过分析有氧化层时金属的发射率模型,解释了这种现象的发生。恒温长时间测量结果表明,在不同的温度下,加热时间对光谱发射率的影响不同。研究结果将进一步丰富纯铁的光谱发射率数据,并为其光谱发射率在大气环境中的应用提供了实验依据。