Pyroelectric detector-based method for low uncertainty spectral irradiance and radiance responsivity calibrations in the infrared using tunable lasers.

The standard uncertainty of detector-based radiance and irradiance responsivity calibrations in the short-wave infrared (SWIR) traditionally has been limited to around 1% or higher by the poor spatial uniformity of detectors used to transfer the scale from radiant power. Pyroelectric detectors offer a solution that avoids the spatial uniformity uncertainty but also introduces additional complications due to alternating current (AC) measurement techniques. Herein, a new, to the best of our knowledge, method for low uncertainty irradiance responsivity calibrations in the SWIR is presented. An absolute spectral irradiance responsivity scale was placed on two pyroelectric detectors (PED) at wavelengths λ from 500 to 3400 nm. The total combined uncertainty (k=1) was ≈0.28% (>1000nm), 0.44% (900 nm), and 0.36% (≈950nm and <900nm) for PED #1 and 0.34% (>1000nm), 0.48% (900 nm), and 0.42% (≈950nm and <900nm) for PED #2. This was done by utilizing a demodulation technique to digitally analyze the time-dependent AC waveforms, which obviates the use of lock-in amplifiers and avoids associated additional uncertainty components.

Developmental changes in the reflectance spectra of temperate deciduous tree leaves and implications for thermal emissivity and leaf temperature.

Leaf optical properties impact leaf energy balance and thus leaf temperature. The effect of leaf development on mid-infrared (MIR) reflectance, and hence thermal emissivity, has not been investigated in detail. We measured a suite of morphological characteristics, as well as directional-hemispherical reflectance from ultraviolet to thermal infrared wavelengths (250 nm to 20 µm) of leaves from five temperate deciduous tree species over the 8 wk following spring leaf emergence. By contrast to reflectance at shorter wavelengths, the shape and magnitude of MIR reflectance spectra changed markedly with development. MIR spectral differences among species became more pronounced and unique as leaves matured. Comparison of reflectance spectra of intact vs dried and ground leaves points to cuticular development - and not internal structural or biochemical changes - as the main driving factor. Accompanying the observed spectral changes was a drop in thermal emissivity from about 0.99 to 0.95 over the 8 wk following leaf emergence. Emissivity changes were not large enough to substantially influence leaf temperature, but they could potentially lead to a bias in radiometrically measured temperatures of up to 3 K. Our results also pointed to the potential for using MIR spectroscopy to better understand species-level differences in cuticular development and composition.

Direct method of extracting broadband complex refractive index from spectrophotometric measurements: an application to polydimethylsiloxane for passive radiative cooling.

We describe an algorithm to extract the complex refractive index of a material from broadband reflectance and transmittance measurements taken by spectrophotometers. The algorithm combines Kramers-Kronig analysis with an inversion of Fresnel's equations to provide a direct method of solving for the refractive index which is accurate, even for weakly absorbing materials, and easily applicable to radiative heat transfer calculations. The algorithm is validated by extracting the complex refractive index of polydimethylsiloxane between 0.25 µm and 100 µm and comparing against existing literature. We also discuss the importance of broadband optical properties to passive radiative cooling and details of the uncertainty analysis of the algorithm.

Measurement Uncertainty of Surface Temperature Distributions for Laser Powder Bed Fusion Processes.

This paper describes advances in measuring the characteristic spatial distribution of surface temperature and emissivity during laser-metal interaction under conditions relevant for laser powder bed fusion (LPBF) additive manufacturing processes. Detailed descriptions of the measurement process, results, and approaches to determining uncertainties are provided. Measurement uncertainties have complex dependencies on multiple process parameters, so the methodology is demonstrated on one set of process parameters and one material. Well-established literature values for high-purity nickel solidification temperature and emissivity at the solidification temperature were used to evaluate the predicted uncertainty of the measurements. The standard temperature measurement uncertainty is found to be approximately 0.9% of the absolute temperature (16 AC), and the standard relative emissivity measurement uncertainty is found to be approximately 8% at the solidification point of high-purity nickel, both of which are satisfactory. This paper also outlines several potential sources of test uncertainties, which may require additional experimental evaluation. The largest of these are the metal vapor and ejecta that are produced as process by-products, which can potentially affect the imaging quality, reflectometry results, and thermal signature of the process, while also affecting the process of laser power delivery. Furthermore, the current paper focuses strictly on the uncertainties of the emissivity and temperature measurement approach and therefore does not detail a variety of uncertainties associated with experimental controls that must be evaluated for future generation of reference data.

Methods for quantitative infrared directional-hemispherical and diffuse reflectance measurements using an FTIR and a commercial integrating sphere.

We have developed methods to measure the directional-hemispherical (ρ) and diffuse (ρd) reflectances of powders, liquids, and disks of powders and solid materials using a commercially available, matte gold-coated integrating sphere and Fourier transform infrared spectrometer. To determine how well the sphere and protocols produce quantitative reflectance data, measurements were made of three diffuse and two specular standards prepared by the National Institute of Standards and Technology (NIST), LabSphere Infragold and Spectralon standards, hand-loaded sulfur and talc powder samples, and water. Relative to the NIST measurements of the NIST standards, our directional hemispherical reflectance values are within ±4% for four of the standards and within ±7% for a low reflectance diffuse standard. For the three diffuse reflectance NIST standards, our diffuse reflectance values are within ±5% of the NIST values. For the two specular NIST standards, our diffuse reflectance values are an order of magnitude larger than those of NIST, pointing to a systematic error in the manner in which diffuse reflectance measurements are made for specular samples using our methods and sphere. Sources of uncertainty are discussed in the paper.

Optical design and Initial Results from The National Institute of Standards and Technology's AMMT/TEMPS Facility.

The National Institute of Standards and Technology's (NIST) Physical Measurement and Engineering Laboratories are jointly developing the Additive Manufacturing Measurement Testbed (AMMT)/ Temperature and Emittance of Melts, Powders and Solids (TEMPS) facilities. These facilities will be co-located on an open architecture laser-based powder bed fusion system allowing users full access to the system's operation parameters. This will provide users with access to machine-independent monitoring and control of the powder bed fusion process. In this paper there will be emphasis on the AMMT, which incorporates in-line visible light collection optics for monitoring and feedback control of the powder bed fusion process. We shall present an overview of the AMMT/TEMPS program and its goals. The optical and mechanical design of the open architecture powder-bed fusion system and the AMMT will also be described. In addition, preliminary measurement results from the system along with the current status of the system will be described.

Report on the CCT Supplementary Comparison S1 of Infrared Spectral Normal Emittance/Emissivity.

The National Measurement Institutes (NMIs) of the United States, Germany, France, Italy and Japan, have joined in an inter-laboratory comparison of their infrared spectral emittance scales. This action is part of a series of supplementary inter-laboratory comparisons (including thermal conductivity and thermal diffusivity) sponsored by the Consultative Committee on Thermometry (CCT) Task Group on Thermophysical Quantities (TG-ThQ). The objective of this collaborative work is to strengthen the major operative National Measurement Institutes' infrared spectral emittance scales and consequently the consistency of radiative properties measurements carried out worldwide. The comparison has been performed over a spectral range of 2 µm to 14 µm, and a temperature range from 23 °C to 800 °C. Artefacts included in the comparison are potential standards: oxidized inconel, boron nitride, and silicon carbide. The measurement instrumentation and techniques used for emittance scales are unique for each NMI, including the temperature ranges covered as well as the artefact sizes required. For example, all three common types of spectral instruments are represented: dispersive grating monochromator, Fourier transform and filter-based spectrometers. More than 2000 data points (combinations of material, wavelength and temperature) were compared. Ninety-eight percent (98%) of the data points were in agreement, with differences to weighted mean values less than the expanded uncertainties calculated from the individual NMI uncertainties and uncertainties related to the comparison process.

Goniometric and hemispherical reflectance and transmittance measurements of fused silica diffusers.

Fused silica diffusers, made by forming scattering centers inside fused silica glass, can exhibit desirable optical properties, such as reflectance or transmittance independent of viewing angle, spectrally flat response into the ultraviolet wavelength range, and good spatial uniformity. The diffusers are of interest for terrestrial and space borne remote sensing instruments, which use light diffusers in reflective and transmissive applications. In this work, we report exploratory measurements of two samples of fused silica diffusers. We will present goniometric bidirectional scattering distribution function (BSDF) measurements under normal illumination provided by the National Institute of Standards and Technology (NIST)'s Goniometric Optical Scatter Instrument (GOSI), by NIST's Infrared reference integrating sphere (IRIS) and by the National Aeronautics and Space Administration (NASA)'s Diffuser Calibration Laboratory. We also present hemispherical diffuse transmittance and reflectance measurements provided by NIST's Double integrating sphere Optical Scattering Instrument (DOSI). The data from the DOSI is analyzed by Prahl's inverse adding-doubling algorithm to obtain the absorption and reduced scattering coefficient of the samples. Implications of fused silica diffusers for remote sensing applications are discussed.

Experimental observation of extremely weak optical scattering from an interlocking carbon nanotube array.

We experimentally demonstrate a nearly wavelength-independent optical reflection from an extremely rough carbon nanotube sample. The sample is made of a vertically aligned nanotube array, is a super dark material, and exhibits a near-perfect blackbody emission at T=450 K-600 K. No other material exhibits such optical properties, i.e., ultralow reflectance accompanied by a lack of wavelength scaling behavior. This observation is a result of the lowest ever measured reflectance (R=0.0003) of the sample over a broad infrared wavelength of 3 µm < λ < 13 µm. This discovery may be attributed to the unique interlocking surface of the nanotube array, consisting of both a global, large scale and a short-range randomness.

Very black infrared detector from vertically aligned carbon nanotubes and electric-field poling of lithium tantalate.

Vertically aligned multiwall carbon nanotubes were grown by water-assisted chemical vapor deposition on a large-area lithium tantalate pyroelectric detector. The processing parameters are nominally identical to those by which others have achieved the "world's darkest substance" on a silicon substrate. The pyroelectric detector material, though a good candidate for such a coating, presents additional challenges and outcomes. After coating, a cycle of heating, electric field poling, and cooling was employed to restore the spontaneous polarization perpendicular to the detector electrodes. The detector responsivity is reported along with imaging as well as visible and infrared reflectance measurements of the detector and a silicon witness sample. We find that the detector responsivity is slightly compromised by the heat of processing and the coating properties are substrate dependent. However, it is possible to achieve nearly ideal values of detector reflectance uniformly less than 0.1% from 400 nm to 4 microm and less than 1% from 4 to 14 microm.

Standard reference material 2036 near-infrared reflection wavelength standard.

Standard Reference Material 2036 (SRM 2036) is a certified transfer standard intended for the verification and calibration of the wavelength/wavenumber scale of near-infrared (NIR) spectrometers operating in diffuse or trans-reflectance mode. SRM 2036 Near-Infrared Wavelength/Wavenumber Reflection Standard is a combination of a rare earth oxide glass of a composition similar to that of SRM 2035 Near-Infrared Transmission Wavelength/Wavenumber Standard and SRM 2065 Ultraviolet-Visible-Near-Infrared Transmission Wavelength/Wavenumber Standard, but is in physical contact with a piece of sintered poly(tetrafluoroethylene) (PTFE). The combination of glass contacted with a nearly ideal diffusely reflecting backing provides reflection-absorption bands that range from 15% R to 40% R. SRM 2036 is certified for the 10% band fraction air wavelength centroid location, (10%)B, of seven bands spanning the spectral region from 975 nm to 1946 nm. It is also certified for the vacuum wavenumber (10%)B of the same seven bands in the spectral region from 10 300 cm(-1) to 5130 cm(-1) at 8 cm(-1) resolution. Informational values are provided for the locations of thirteen additional bands from 334 nm to 804 nm.

Monte Carlo modeling of an integrating sphere reflectometer.

The Monte Carlo method has been applied to numerical modeling of an integrating sphere designed for hemispherical-directional reflectance factor measurements. It is shown that a conventional algorithm of backward ray tracing used for estimation of characteristics of the radiation field at a given point has slow convergence for small source-to-sphere-diameter ratios. A newly developed algorithm that substantially improves the convergence by calculation of direct source-induced irradiation for every point of diffuse reflection of rays traced is described. The method developed is applied to an integrating sphere reflectometer for the visible and infrared spectral ranges. Parametric studies of hemispherical radiance distributions for radiation incident onto the sample center were performed. The deviations of measured sample reflectance from the actual reflectance as a result of various factors were computed. The accuracy of the results, adequacy of the reflectance model, and other important aspects of the algorithm implementation are discussed.