Photothermal Radiometry Signal Research Articles

Sizing the depth and width of ideal delaminations using modulated photothermal radiometry

Delaminations, buried defects parallel to the sample surface, reduce the material stiffness and the structure reliability. Photothermal methods, based on exciting the surface by a light beam and analyzing the resulting temperature rise, have been extensively used for detecting delaminations and sizing their depth. However, less attention has been paid to the sizing of the delamination width. In this work, we use modulated photothermal radiometry (PTR) to size the depth and width of narrow delaminations by fitting the theoretical temperature expression to the experimental frequency spectrum of the PTR signal. We have established a detectability limit: for good thermal conductors, submicronic delaminations can be sized down to 10 mm, whereas for thermal insulators, it is difficult to go below 0.5 mm. Experiments on calibrated delaminations confirm these predictions.

Investigations of the possibility of determination of thermal parameters of Si and SiGe samples based on the Photo Thermal Radiometry technique

This paper presents results of investigations of the possibility of determination of thermal parameters (thermal conductivity, thermal diffusivity) of silicon and silicon germanium crystals from the frequency characteristics of the Photo Thermal Radiometry (PTR) signal. The theoretical analysis of the influence of the mentioned parameters on the PTR signal has been presented and discussed. The values of the thermal and recombination parameters have been extracted from the fittings of the theoretical to experimental data. The presented approach uses the reference Si sample whose thermal and recombination parameters are known.

Investigation of Thermal Properties of High-Density Polyethylene/Aluminum Nanocomposites by Photothermal Infrared Radiometry

In this study, thermal properties of high-density polyethylene (HDPE) filled with nanosized Al particles (80 nm) were investigated. Samples were prepared using melt mixing method up to filler volume fraction of 29 %, followed by compression molding. By using modulated photothermal radiometry (PTR) technique, thermal diffusivity and thermal effusivity were obtained. The effective thermal conductivity of nanocomposites was calculated directly from PTR measurements and from the measurements of density, specific heat capacity (by differential scanning calorimetry) and thermal diffusivity (obtained from PTR signal amplitude and phase). It is concluded that the thermal conductivity of HDPE composites increases with increasing Al fraction and the highest effective thermal conductivity enhancement of 205 % is achieved at a filler volume fraction of 29 %. The obtained results were compared with the theoretical models and experimental data given in the literature. The results demonstrate that Agari and Uno, and Cheng and Vachon models can predict well the thermal conductivity of HDPE/Al nanocomposites in the whole range of Al fractions.

Comment on “Photothermal radiometry parametric identifiability theory for reliable and unique nondestructive coating thickness and thermophysical measurements” [J. Appl. Phys. 121, 095101 (2017)

A recent paper [Guo et al., J. Appl. Phys. 121, 095101 (2017)] intends to demonstrate that from the photothermal radiometry signal obtained on a coated opaque sample in 1D transfer, one should be able to identify separately the following three parameters of the coating: thermal diffusivity, thermal conductivity, and thickness. In this comment, it is shown that, in the considered experiment arrangement, these three parameters are correlated, the identifiability criterion is in error, and the thickness inferred therefrom is not trustable.

Photothermal, Structural, and Microstructural Characterization of SAE4320H Automotive Steel

SAE4320H steel was characterized by photothermal radiometry spectroscopy, scanning electron microscopy, x-ray diffraction, and Vickers microhardness, to study metallurgical property changes as a result of the annealing heat treatment. Photothermal radiometry (PTR) images of hot forged and annealed SAE4320H steel were obtained to study the thermal changes, as a consequence of metallurgical microstructure changes that were produced by the heat treatment conditions. X-ray diffraction showed that the annealing process improves the crystalline quality of the SAE4320H steel and releases of any thermal stress. Widmanstatten microstructure was identified as a typical structure after the forging process. The Widmanstatten is a metallographic microstructure transformation to ferrite and pearlite which affected SAE4320H steel hardness and thermal properties. Vickers test showed that the hardness decreases as a result of the annealing process. A positive correlation between Vickers microhardness and PTR amplitude images was found, indicating that the annealing process increases the PTR signal. This methodology allows the determination of the changes in the Vickers microhardness from a non-contact and remote method as in PTR.

Kapitza thermal resistance studied by high-frequency photothermal radiometry

Kapitza thermal resistance is determined using high-frequency photothermal radiometry (PTR) extended for modulation up to 10 MHz. Interfaces between 50 nm thick titanium coatings and silicon or stainless steel substrates are studied. In the used configuration, the PTR signal is not sensitive to the thermal conductivity of the film nor to its optical absorption coefficient, thus the Kapitza resistance is directly determined from single thermal parameter fits. Results of thermal resistances show the significant influence of the nature of the substrate, as well as of the presence of free electrons at the interface.

Simulation and experimental investigation of tooth tissue in photothermal radiometry dynamic response induced by modluated laser

The photon-density wave is generated in tooth tissue due to the scattering induced by modulated laser beams, and furthermore, thermal-wave will form because of photothermal effect. A one-dimensional thermal-wave model for three-layer tooth tissue using modulated laser stimulation is developed based on 1D diffusion approximation of the radiative transfer theory in combination with 1D heat conduction equation. Effects of photothermal properties (i.e. light absorption coefficient, scattering coefficient and thermal diffusivity coefficient), enamel depth and caries depth on the photothermal radiometry (PTR) dynamic responses are investigated based on the 1D thermal wave model coupling with photon-density wave. The PTR amplitude and phase delay (the phase difference between the PTR signal and reference signal) are strongly dependent on the photothermal parameters of the dental enamel caries layers (DECLs). PTR amplitude and phase delay increase with increasing DECL absorption coefficient, scattering coefficient and thermal diffusivity. Additionally, PTR amplitude may also increase due to the larger thickness of caries layer, and the PTR phase peak value is generated at low frequencies. The inhomogeneous photothermal properties of dental enamel healthy layer (DEHL) also have obviously influenced PTR amplitude and phase. Increasing DEHL scattering coefficient leads to the increase of PTR amplitude, but has no apparent effect on the PTR phase. While the PTR phase delay increases with increasing DEHL absorption coefficient. The delay of PTR amplitude and phase is enlarged at the high value of DEHL thermal diffusivity. However, the DEHL layer thickness has no apparent effect on the PTR amplitude and phase.The PTR signal of tooth tissue induced by the 808 nm diode laser is monitored using an infrared detector (HgCdTe, spectral width 2.012.0 m), and the PTR amplitude and phase response are obtained using lock-in amplifier (SR830). Through frequency-scanning experiments of dental tissue, PTR dynamic responses can be measured and employed to characterize the inhomogeneity and caries of the tooth tissue. The photothermal parameters and caries characteristic of the tooth issue can be simultaneously obtained by multi-parameters statistic best-fit.Simulation and experimental results show that the PTR dynamic response has the advantages of high sensitivity and high contrast for inhomogeneity and caries of the tooth tissue.

Defects of a-Si Thin-Film Solar Cells Detected by Transmission Photothermal Radiometric Imaging

The photothermal radiometry (PTR) technique is an effective non-destructive testing technique for detecting defects in materials. In this paper, a piece of commercial amorphous silicon (a-Si) thin-film solar cells with some artificial mechanical defects has been investigated by the transmission PTR imaging system. Firstly, a simplified analytical expression of a normalized transmission PTR signal was employed to characterize defects. Secondly, the corresponding experimental system has been set-up for obtaining several thermal images of the sample. Thirdly, different kinds of defects have been analyzed and identified by the thermal images. The results show that not only the artificial mechanical defects on the sample can be detected, but also some defects occurring in the manufacturing process can be detected by the transmission PTR imaging system.

Noncontact measurement of the thermal diffusivity of IR semi-transparent and semiconducting n-CdMgSe mixed crystals by means of the photothermal radiometry

In this paper we present results of noncontact measurements of the thermal diffusivity of infrared semi-transparent n-CdMgSe mixed semiconductor crystals by means of the photothermal radiometry (PTR) in a transmission configuration. In order to overcome an influence of the infrared semi-transparency and plasma waves on the PTR signal from n-CdMgSe mixed crystals the samples were covered by thin aluminum foils on both sides. The thermal diffusivities of n-CdMgSe mixed crystals were estimated from PTR phase frequency characteristics using a well-known formula. It was found that the obtained results are underestimated in comparison to thermal diffusivities estimated from the PPE (photopyro-electric) measurements. A three layer model of a PTR signal was applied in order to estimate an error in determination of the thermal diffusivity of a sample caused by aluminum foils.

Correlation Between Chemical Composition of Silver Alloys and Photothermal Radiometry Signals

The development of nondestructive and noncontact techniques for evaluation of metallic materials is invaluable to metal characterization. The photothermal radiometry (PTR) amplitude and phase images of silver alloys were used to study the silver distribution in alloys rich in silver and copper for Ag concentrations between 37 mass% and 92 mass%. The silver concentration was determined using inductively coupled plasma. It was found that for Ag concentrations lower than 50 mass%, the PRT signals are governed by the thermal and optical properties of copper and vice versa. It was possible to establish a good correlation between the PTR amplitude and phase signal with the Ag concentration. This means that after calibration it is possible to determine the Ag concentration using nondestructive evaluation.

Photothermal Evidence of Laterally Inhomogeneous Interfacial Thermal Resistance in Copper-Coated Carbon Samples

In this study, the heat transport in copper–carbon flat model systems was studied by frequency-dependent photothermal radiometry (PTR). The samples consist of Cu films of about 1 μm thickness deposited by magnetron sputtering on vitreous carbon (Sigradur). Particular interest was devoted to the influence of interface defects on the interfacial thermal conductance (or resistance) of the CuC systems. The PTR data were analyzed in the frame of a heat diffusion equation for one- and three-dimensional heat transport. By comparing PTR signals from as-prepared and from heat-treated samples, the lateral inhomogeneities of the interfacial thermal conductance could be quantified. The measured phase differences were analyzed in the scope of a model where a small part of the surface area has a different interfacial thermal conductance than the major part of the surface.

Simultaneous measurement of thermal diffusivity and optical absorption coefficient using photothermal radiometry. I. Homogeneous solids

Modulated photothermal radiometry (PTR) has been widely used to measure the thermal diffusivity of bulk materials. The method is based on illuminating the sample with a plane light beam and measuring the infrared emission with an infrared detector. The amplitude and phase of the PTR voltage is recorded as a function of the modulation frequency and then fitted to the theoretical model. In this work, we test the ability of modulated PTR to retrieve simultaneously the thermal diffusivity and the optical absorption coefficient of homogeneous slabs. In order to eliminate the instrumental factor, self-normalization is used, i.e., the ratio of the PTR signal recorded at the rear and front surfaces. The influence of the multiple reflections of the light beam, the heat losses, and the transparency to infrared wavelengths are analyzed. Measurements performed on a wide variety of homogeneous materials, covering the whole range from transparent to opaque, confirm the validity of the method. In Part II of this work, the method is extended to multilayered materials.

Quantitative remineralization evolution kinetics of artificially demineralized human enamel using photothermal radiometry and modulated luminescence

Human molars were subjected to demineralization in acid gel followed by incubation in remineralization solutions without or with fluoride (1 or 1000 ppm). Photothermal radiometry (PTR) and modulated luminescence (LUM) frequency scans were performed prior to and during de/remineralization treatments. Transverse Micro-Radiography (TMR) analysis followed at treatment conclusion to determine mineral loss and lesion depth. The remineralization process illustrated a complex interplay between surface and subsurface mineral deposition, confining the thermal-wave centroid toward the dominating layer. Experimental amplitudes and phases were fitted to a coupled diffuse-photon-density-wave and thermal-wave theoretical model used to quantitatively evaluate evolving changes in thermal and optical properties of de/remineralized enamel lesions. Additional information obtained from the LUM data corroborated the remineralization kinetics affecting the PTR signals. The results pointed to enhanced effectiveness of subsurface lesion remineralization in the presence of fluoride.

Combined FPPE–PTR Calorimetry Involving TWRC Technique. Theory and Mathematical Simulations

Photopyroelectric calorimetry in the front detection configuration (FPPE) was combined with photothermal radiometry (PTR), in order to investigate dynamic thermal parameters of different layers of a detection cell. The layout of the detection cell consists of three layers: directly irradiated pyroelectric sensor, liquid layer, and solid backing material; and the scanning parameter is the thickness of the liquid layer (thermal-wave resonator cavity method). The theory developed for the two techniques indicates that both FPPE and PTR signals can lead, in the thermally thin regime for the sensor and liquid layer, to the direct measurement of the thermal diffusivity or effusivity of the sensor and/or liquid layer, or the thermal effusivity of the backing material. The two methods offer complementary results and/or reciprocally support each other.

Dental diagnostic clinical instrument ("Canary") development using photothermal radiometry and modulated luminescence

Since 1999, our group at the CADIFT, University of Toronto, has developed the application of Frequency Domain Photothermal Radiometry (PTR) and Luminescence (LUM) to dental caries detection. Various cases including artificial caries detection have been studied and some of the inherent advantages of the adaptation of this technique to dental diagnostics in conjunction with modulated luminescence as a dual-probe technique have been reported. Based on these studies, a portable, compact diagnostic instrument for dental clinic use has been designed, assembled and tested. A semiconductor laser, optical fibers, a thermoelectric cooled mid-IR detector, and a USB connected data acquisition card were used. Software lock-in amplifier techniques were developed to compute amplitude and phase of PTR and LUM signals. In order to achieve fast measurement and acceptable signal-to-noise ratio (SNR) for clinical application, swept sine waveforms were used. As a result sampling and stabilization time for each measurement point was reduced to a few seconds. A sophisticated software interface was designed to simultaneously record intra-oral camera images with PTR and LUM responses. Preliminary results using this instrument during clinical trials in a dental clinic showed this instrument could detect early caries both from PTR and LUM signals.

New methodology for thermal parameter measurements in solids using photothermal radiometry

The photothermal radiometry (PTR) signal is analyzed in order to simultaneously obtain the thermal diffusivity and effusivity of solid materials. Analytical procedures that allow the determination of the thermal parameters via a frequency scan of the amplitude or the phase of the PTR signal are presented. The measurement procedures do not involve a multiparameter-fit optimization algorithm. The methods have been used for the measurement of thermophysical properties of vitreous carbon and lead-itanate-zirconate ceramic samples.

Rapid, non-destructive and non-contact inspection of solid foods by means of photothermal radiometry; thermal effusivity and initial heating coefficient

CO 2-laser photothermal radiometry (PTR) was demonstrated to be suitable for the non-destructive and non-contact characterization (both optical and thermal) of solid phase agricultural commodities (fresh vegetables, fruits) and confectionery products (candy). Proper interpretation of PTR signals enable one to calculate two parameters, i.e. the well known thermal effusivity e ( e= λρc p , where λ and ρc p are the thermal conductivity and the volume specific heat, respectively) and a newly introduced physical quantity termed ‘initial heating coefficient’ chi ( χ= β/( ρc p ), β is the absorption coefficient). Obtained values for e are in a good agreement with data reported in the literature. PTR enables one to rapidly determine e via a single measurement. As opposed to this, the knowledge of two out of three thermophysical parameters (thermal diffusivity, thermal conductivity and volume specific heat) is a condition sine qua non for determining effusivity in the conventional manner.

Spectroscopic photothermal radiometry as a deep subsurface depth profilometric technique in semiconductors

The theoretical and experimental aspects of spectroscopic photothermal radiometry (PTR) of semiconductors are presented and the potential of the technique for depth profilometry is established. A three-dimensional model of the PTR signal from a semiconductor excited by light of arbitrary optical penetration depth is presented. Numerical simulations of the PTR response to the electronic transport parameters and the optical penetration depth of the excitation source are presented. Intensity-modulated frequency scans and two-dimensional surface scans at fixed frequencies have been performed at several different absorption depths on a Si wafer with various degrees of mechanical damage introduced to either the front or the back surface. The electronic transport parameters obtained from fitting the frequency scans to the theoretical model and analysis of the experimental curves show that while the surface recombination velocities extracted from the fits do not vary significantly with excitation wavelength, the carrier recombination lifetime and the overall sensitivity of the photothermal radiometric signal to spatially localized damage is strongly influenced by the proximity of the injected excess carrier density centroid to the defect location. This correlation between the sensitivity of the PTR signal to a localized defect and the proximity of the injected carriers to the defect demonstrates the potential for spectroscopic PTR as a depth profilometric technique for semiconductors.

Quantitative dental measurements by use of simultaneous frequency-domain laser infrared photothermal radiometry and luminescence.

Modulated (frequency-domain) infrared photothermal radiometry (PTR) is used as a dynamic quantitative dental inspection tool complementary to modulated luminescence (LM) to quantify sound enamel or dentin. A dynamic high-spatial-resolution experimental imaging setup, which can provide simultaneous measurements of laser-induced modulated PTR and LM signals from defects in teeth, has been developed. Following optical absorption of laser photons, the experimental setup can monitor simultaneously and independently the nonradiative (optical-to-thermal) energy conversion by infrared PTR and the radiative deexcitation by LM emission. The relaxation lifetimes (tau1, tau2) and optical absorption, scattering, and spectrally averaged infrared emission coefficients (mu(alpha), mu(s), mu(IR)) of enamel are then determined with realistic three-dimensional LM and photothermal models for turbid media followed by multiparameter fits to the data. A quantitative band of values for healthy enamel with respect to these parameters can be generated so as to provide an explicit criterion for the assessment of healthy enamel and, in a future extension, to facilitate the diagnosis of the onset of demineralization in carious enamel.

Deconvolution of surface and direct metastable- state blackbody emission in Ti:sapphire laser materials using boxcar time-domain photothermal radiometry

Single-gate boxcar-integrator time-domain photothermal radiometry (PTR) is proposed as a noncontact remote technique with a high signal-to-noise ratio that can evaluate the optical quality of the surface in a solid-state laser-gain medium such as Ti:sapphire. It was found that immediately after the boxcar-averaged laser-pulse cutoff, the PTR signal is dominated by the laser metastable-level transition lifetime. A PTR theoretical model was formulated to account for this effect and to deconvolute its contribution to the signal from surface absorption of the laser radiation. With the theoretical model, the surface contribution to experimental boxcar PTR signals was deconvoluted and the surface quality was quantified in terms of the surface nonradiative energy generation rate, as the percentage of the input optical power that is converted to heat.