Terahertz Time-domain Spectroscopy Measurements Research Articles

Wide-range resistivity characterization of semiconductors with terahertz time-domain spectroscopy

Resistivity is one of the most important characteristics in the semiconductor industry. The most common way to measure resistivity is the four-point probe method, which requires physical contact with the material under test. Terahertz time domain spectroscopy, a fast and non-destructive measurement method, is already well established in the characterization of dielectrics. In this work, we demonstrate the potential of two Drude model-based approaches to extract resistivity values from terahertz time-domain spectroscopy measurements of silicon in a wide range from about 10−3 Ωcm to 102 Ωcm. One method is an analytical approach and the other is an optimization approach. Four-point probe measurements are used as a reference. In addition, the spatial resistivity distribution is imaged by X-Y scanning of the samples to detect inhomogeneities in the doping distribution.

Terahertz Time-Domain Spectroscopic (THz-TDS) Insights into Protein Deformation

In this study, we utilized terahertz time-domain spectroscopy (THz-TDS) to study the radiation-induced protein deformation. The absorption coefficient spectra obtained from THz-TDS measurements in the frequency range (0.06–2 THz) was fitted using the Lorentzian model. The absorption coefficient fitting data was used to identify the α-helix and β-structure relative contributions in the protein secondary structure of the kidney tissue of rats irradiated with 10-cGy and 2-Gy X-ray separately or in combination. Our data show that 2-Gy X-irradiation leads to an increase in the β-structure contribution associated with a decrease in the α-helix contribution as indicated by the fitting parameters extracted from fitting the absorption coefficient α(ω) spectra with the Lorentzian function. The results point out that there is a strong correlation between the strength of the hydrogen bonds located between or inside the polypeptide chains of the extended β-sheet and α-helix, respectively, and the absolute value of the absorption coefficient α(ω), the refractive index, and the dielectric constant. The lowest refractive index and dielectric constant are recorded in the 2-Gy-irradiated group followed by the 10-cGy–2 Gy-irradiated group while the least effect was recorded in the 10-cGy-irradiated group. These data provide evidence of the adaptive effect of the 10-cGy X-irradiation delivered 24 h prior to the 2-Gy x-irradiation.

The absorption properties of ZrO2 nanoparticles in the THz and sub-THz frequency ranges.

As terahertz (THz) and sub-THz region electromagnetic waves are becoming vital for industrial applications such as 5G wireless communication, so too are THz and sub-THz wave absorbing materials. Herein, we report the optical properties of monoclinic zirconia (m-ZrO2) nanoparticles in these frequency regions, with different crystalline sizes. The crystalline sizes of the three samples, measured by transmission electron microscopy, are 93 ± 23 nm (denoted 1), 28 ± 14 nm (denoted 2) and 2.6 ± 0.7 nm (denoted 3). X-ray diffraction and Raman spectra show that 1 and 2 have high crystallinity whereas 3 shows peak broadening due to its small crystalline size. Terahertz time-domain spectroscopy (THz-TDS) measurements of pelletised samples show that the small crystalline size sample exhibits larger absorption, e.g., the absorbance value at 300 GHz is 0.18 mm-1 (1), 0.04 mm-1 (2) and 1.11 mm-1 (3), and the related dielectric loss value (ε'') is 0.04 (1), 0.01 (2) and 0.82 (3), respectively. This is considered to be due to the proportional increase in surface water molecules for the small particle size sample due to the relative increase in surface area and under-coordinated atoms, shown by IR spectra. These results show that small crystalline size m-ZrO2 nanoparticles have potential as THz and sub-THz wave absorbing materials, which are crucial for noise reduction in THz and sub-THz wave technologies.

Refractive index measurement of IP-S and IP-Dip photoresists at THz frequencies and validation via 3D photonic metamaterials made by direct laser writing

Direct laser writing (DLW) is widely used to fabricate complex metamaterials (MMs) and photonic devices for nanoscale applications across the electromagnetic frequency spectrum. While the optical properties of conventional photoresists used in DLW are well studied in the visible and infrared range, it is still unclear how they behave at lower frequencies. Here, we measure the refractive index and absorption of IP-S and IP-Dip photoresists within the THz range of the electromagnetic spectrum. Further, we utilize THz time-domain spectroscopy (THz-TDS) to experimentally measure the laser-processed three-dimensional (3D) MM structures. We conduct full-wave electromagnetic simulations using the measured refractive index values to validate our experiments. The THz-TDS measurements are in excellent agreement with the theoretical predictions verifying the validity of our refractive index measurements. This study aims to support and lead future investigations utilizing standard DLW photoresists for photonic applications in the THz range.

Thickness-Dependent Terahertz Permittivity of Epitaxially Grown PbTe Thin Films

The exceptional thermoelectric properties of PbTe are believed to be associated with the incipient ferroelectricity of this material, which is caused by strong electron–phonon coupling that connects phononic and electronic dynamics. Here, we have used terahertz time-domain spectroscopy measurements to generate complex permittivity spectra for a set of epitaxially grown PbTe thin films with thicknesses between 100 and 500 at temperatures from 10K to 300K. Using a Drude–Lorentz model, we retrieved the physical parameters of both the phononic and electronic contributions to the THz permittivity. We observed a strong decrease, or softening, of the transverse optical phonon mode frequency with decreasing temperature, determining a thickness-independent negative ferroelectric-transition critical temperature, while we found a thickness-dependent anharmonic phonon decay lifetime. The electronic contribution to the permittivity was larger in thinner films, and both the carrier density and mobility increased with decreasing temperature in all films. Finally, we detected a thickness-dependent longitudinal optical phonon mode frequency, indicating the presence of plasmon–phonon coupling.

Optical measurements of the silicon vacuum window with anti-reflective sub-wavelength structure for ASTE Band 10.

For millimeter and submillimeter-wave astronomy, it is highly desirable to have vacuum windows within the receiver cryostat that exhibit low reflection, low loss, and a wide bandpass. The use of antireflective (AR) sub-wavelength structures (SWSs) on substrates has expanded the possibilities for creating new vacuum windows. Recently, a novel method of fabricating AR SWS on a silicon-on-insulator wafer has been proposed, and a vacuum window with a two-layer AR SWS has been developed for use with the Atacama Submillimeter Telescope Experiment Band 10 receiver. To thoroughly assess the characteristics of the silicon window sample, we conducted transmittance measurements using terahertz time-domain spectroscopy, and noise and beam measurements using an Atacama Large Millimeter/submillimeter Array (ALMA) Band 10 receiver. We found that the silicon window sample exhibits characteristics comparable to the quartz window of the ALMA Band 10 receiver. The result strongly encourages applications of AR silicon windows in receivers with wider bandwidths.

THz computed tomography for non-destructive testing

This work describes a complete THz computed tomography imaging system. Starting from a physical imaging model based on geometrical optics, an image reconstruction algorithm is derived. This algorithm uses the raw time-domain measurement signals acquired from THz time-domain spectroscopy measurements of the sample in order to calculate the sample cross-section. In particular, the phase of the transmitted THz pulse is evaluated for image reconstruction. The results show a significant improvement compared to the reconstruction based solely on the absorption. If preliminary knowledge about the sample geometry is available, refraction effects occurring on the sample interfaces can be considered in order to obtain a more accurate measurement result. This is especially beneficial in industrial non-destructive testing, where a sample is typically tested for deviations from a predefined specification or geometrical shape. Typical accuracies around 150 µm are demonstrated using 3d printed benchmark samples.

Numerical Analysis of the Influence of Fabrication Process Uncertainty on Terahertz Metasurface Quality

The purpose of this paper was to investigate the influence of fabrication process uncertainty on terahertz metasurface quality. The focus was on the effect of metasurface fabrication inaccuracy on resonances. To the best of our knowledge, this is the first paper to study the effect of the metasurface fabrication process on its resonant frequency. The terahertz split ring resonator-based metasurface is under consideration. Using a numerical model, the influence of the uncertainty of various geometrical parameters obtained during the fabrication process (mainly layer deposition, photolithography, and etching processes) is analyzed according to the resonance of the designed metasurface. The influence of the following parameters causes a shift of resonant frequencies of the considered metasurface: etching deviation e, metallization thickness tAl and SiO2 layer thickness tSiO2. The quality of the metasurface affected by the variations of obtained geometrical parameters was determined by the deviation of resonant frequency Δfr. The developed numerical model was verified by THz-TDS (terahertz time-domain spectroscopy) measurements of the fabricated structure.

Observation of terahertz transition from Fano resonances to bound states in the continuum.

Bound states in the continuum (BIC) in metamaterials have recently attracted attention for their promising applications in photonics. Here, we investigate the transition from Fano resonances to BIC, at terahertz (THz) frequencies, of a one-dimensional photonic crystal slab made of rectangular dielectric rods. Simulations performed by an analytical exact solution of the Maxwell equations showed that symmetry-protected, high-quality factor (Q), BIC emerge at normal incidence. For non-normal incidence, BIC couple with the freely propagating waves and appear in the scattering field as a Fano resonance. Simulations were verified by realizing the photonic crystal slab by 3D-printing technique. THz time-domain spectroscopy measurements as a function of the incidence angle matched the simulation to good accuracy and confirmed the evolution of Fano resonances to high-Q resonances typical of BIC. These results point out the design of highly sensitive and low-cost THz devices for sensing for a wide range of applications.

Non-Linear Conductivity Response of Graphene on Thin-Film PET Characterized by Transmission and Reflection Air-Plasma THz-TDS.

We demonstrate that the conductivity of graphene on thin-film polymer substrates can be accurately determined by reflection-mode air-plasma-based THz time-domain spectroscopy (THz-TDS). The phase uncertainty issue associated with reflection measurements is discussed, and our implementation is validated by convincing agreement with graphene electrical properties extracted from more conventional transmission-mode measurements. Both the reflection and transmission THz-TDS measurements reveal strong non-linear and instantaneous conductivity depletion across an ultra-broad bandwidth (1-9 THz) under relatively high incident THz electrical field strengths (up to 1050 kV/cm).

Dual-band terahertz absorber based on square ring metamaterial structure.

In this paper, a dual-band terahertz absorber based on metamaterial structure is designed, fabricated, and measured. The metal periodic array is located on the upper surface of a silicon wafer with a metal ground plane, while the metamaterial structure is created utilizing a square metal ring with four T-shaped metal strips loaded inside of the ring. Two absorption peaks are realized at 0.715 and 1.013 THz with high Q-factors of 152.1 and 98.3, respectively, under normal TE and TM polarized incidence. A prototype of the proposed metamaterial absorber is fabricated by electron beam lithography (EBL) and electron beam evaporation (EBE) technology. Furthermore, a terahertz time-domain spectroscopy (TDS) measurement system is employed to test the absorber sample, with good measurement results obtained. This work provides a new option for the design of multi-band terahertz metamaterial absorbers.

Realization of Photonic Topological Insulators at Terahertz Frequencies Characterized by Time-Domain Spectroscopy

Topological systems are inherently robust to disorder and continuous perturbations, resulting in dissipation-free edge transport of electrons in quantum solids, or reflectionless guiding of photons and phonons in classical wave systems characterized by topological invariants. Realization of robust, lossless topological insulators in the technologically important terahertz (THz) frequency range has drawn immense attention. In this paper, we propose a Kagome lattice structure that supports topological edge states with valley-dependent transport. Optical topological insulators are subsequently fabricated, in which mirror symmetry is broken and degenerate states are lifted at $K({K}^{\ensuremath{'}})$ valleys in the band structure. Theoretical and numerical analyses show that four types of edge states can be obtained. The performance of the fabricated topological waveguides is characterized with THz time-domain spectroscopy (TDS). Nearly identical THz wave transmission in the 0.437--0.453-THz range is verified with a straight-line topological waveguide and Z-shaped waveguides with multiple sharp turning corners, which quantitatively illustrate the strong backscattering suppression effects from the nontrivial topology edge states of the structures. Particularly, the THz TDS measurements provide important extra time-domain information about the topological waveguiding mode, which is generally unavailable from previous topological insulator investigations solely replying on power spectrum measurements.

Accurate and early prediction of the wound healing outcome of burn injuries using the wavelet Shannon entropy of terahertz time-domain waveforms.

Severe burn injuries cause significant hypermetabolic alterations that are highly dynamic, hard to predict, and require acute and critical care. The clinical assessments of the severity of burn injuries are highly subjective and have consistently been reported to be inaccurate. Therefore, the utilization of other imaging modalities is crucial to reaching an objective and accurate burn assessment modality. We describe a non-invasive technique using terahertz time-domain spectroscopy (THz-TDS) and the wavelet packet Shannon entropy to automatically estimate the burn depth and predict the wound healing outcome of thermal burn injuries. We created 40 burn injuries of different severity grades in two porcine models using scald and contact methods of infliction. We used our THz portable handheld spectral reflection (PHASR) scanner to obtain the in vivo THz-TDS images. We used the energy to Shannon entropy ratio of the wavelet packet coefficients of the THz-TDS waveforms on day 0 to create supervised support vector machine (SVM) classification models. Histological assessments of the burn biopsies serve as the ground truth. We achieved an accuracy rate of 94.7% in predicting the wound healing outcome, as determined by histological measurement of the re-epithelialization rate on day 28 post-burn induction, using the THz-TDS measurements obtained on day 0. Furthermore, we report the accuracy rates of 89%, 87.1%, and 87.6% in automatic diagnosis of the superficial partial-thickness, deep partial-thickness, and full-thickness burns, respectively, using a multiclass SVM model. The THz PHASR scanner promises a robust, high-speed, and accurate diagnostic modality to improve the clinical triage of burns and their management.

Multifrequency Contrast Source Inversion-Based Permittivity Estimation for Terahertz Multilayer Analysis

In this study, the method of estimating permittivity using inverse scattering is presented for multilayered analysis in the terahertz (THz) frequency band. While many studies have been conducted to determine the relative permittivity estimation of multilayer media, most of the studies are based on the time-of-flight (TOF) analysis, which requires the careful consideration of multiple reflection factors and a sufficiently short pulse, i.e., a wider frequency bandwidth, to discriminate the number of TOF from each layer. Therefore, the contrast source inversion-based permittivity estimator exploiting multiple frequency cost function analysis has been introduced. The efficiency of our proposed approach is shown using THz time-domain spectroscopy measurements on two thin layer objects.

Broadband Dielectric Characterization of High-Permittivity Rogers Substrates via Terahertz Time-Domain Spectroscopy in Reflection Mode

We report the dielectric characterization of three commercially available, high-permittivity Rogers laminates in the sub-terahertz range, by means of terahertz time-domain spectroscopy measurements in reflection mode. A transmission-line model is developed to obtain the reflectance spectra as a function of the frequency-dispersive complex relative permittivity of the substrates. The latter is fitted through optimization to a single Lorentzian term, which is shown to accurately reproduce the measured reflectance spectra. The substrates RO3010 and RT/duroid 6010.2LM exhibit significant frequency dispersion of both their relative permittivity and loss tangent. Conversely, the thermoset microwave laminate TMM10i is characterized by both a lower frequency dispersion and overall dielectric losses, thus making it a promising candidate for the design of low-profile and broadband components for novel terahertz applications. Owing to the simple Lorentzian dispersion model used for the description of the relative permittivity, the presented results can serve as a reference, and they can be directly introduced in design and optimization workflows for novel devices in emerging terahertz applications.

Comprehensive study of 3D printing materials over the terahertz regime: absorption coefficient and refractive index characterizations

Generation of terahertz (THz) radiation has become increasingly accessible over time. The research and development of THz applications is ongoing, often requiring the use of THz compatible optical components. At the same time, rapid prototyping three-dimensional (3D) printing systems are now commercially accessible and are capable of printing resolutions on the order of the THz wavelengths. Thus, 3D printing systems can be leveraged for use in creating novel THz optical components in varied experiments and applications. The filament material used in 3D printing systems dictates the absorptive and refractive properties of the 3D printed THz optical component. The commercial release of filament materials is continuous, year after year, inducing a need for literature to stay current with characterizing these filament materials over the THz gap. We use terahertz time-domain spectroscopy (THz-TDS) to characterize the absorptive and refractive properties of 3D printing materials over the THz gap. We present a consolidative and comprehensive aggregation of THz-TDS measurements of twenty-three 3D printing materials. A comparison of THz-TDS measurements for thick and thin samples provides verification of measurement accuracy. The measured THz bandwidth of these samples is extended by up to 1.2 THz. Furthermore, to the authors’ best knowledge, the proposed work puts forward the first THz-TDS measurements of polyvinyl butyral, polyetherimide, and low temperature polycaprolactone filament materials. This work primarily focuses on fused deposition modeling (FDM) 3D printed materials, rather than stereolithography (SLA) 3D printed materials.

Fragmented graphene synthesized on a dielectric substrate for THz applications

Fragmented multi-layered graphene films were directly synthesized via chemical vapor deposition (CVD) on dielectric substrates with a pre-deposited copper catalyst. We demonstrate that the thickness of the sacrificial copper film, process temperature, and growth time essentially influence the integrity, quality, and disorder of the synthesized graphene. Atomic force microscopy and Kelvin probe force microscopy measurements revealed the presence of nano-agglomerates and charge puddles. The potential gradients measured over the sample surface confirmed that the deposited graphene film possessed a multilayered structure, which was modelled as an ensemble of randomly oriented conductive prolate ellipsoids. THz time domain spectroscopy measurements gave the ac conductivity of the graphene flakes and homogenized graphitic films as being around 1200 S cm−1 and 1000 S cm−1, respectively. Our approach offers a scalable fabrication of graphene structures composed of graphene flakes, which have effective conductivity sufficient for a wide variety of THz applications.

Characterization of the remediation of chromium ion contamination with bentonite by terahertz time-domain spectroscopy

Heavy metal pollution of agricultural and urban soils limits economic progress in the rapidly developing society. Terahertz technology is applied to detect heavy metal pollutants under existence of multiple pathways of their dissemination. In this study, terahertz time-domain spectroscopy (THz-TDS) is employed as an advanced probing technique in combination with traditional detecting methods to measure the adsorption ability of trivalent chromium ions on bentonite. The concentration of chromium ions and the weight of bentonite are known to influence on the adsorption capacity of the latter. It is tested here by both qualitative and quantitative measurements of two mentioned parameters. The adsorption process of chromium ions by bentonite is monitored using THz-TDS. The adsorptions signal from samples at 0.5 THz gradually increases with the increase of bentonite weight or chromium ion concentration. It would appear to indicate that terahertz could be used for quantitative detection of metal ions. Secondly, the ratios of results obtained by inductively coupled plasma mass spectrometry (ICP-MS) and the THz-TDS ones are stabilized at 0.105 ± 0.014 as the bentonite weight or chromium ion concentration increase. Such finding confirms that terahertz technology can be used for the quantitative detection of metal ions. Using the relationship between the ICP-MS test results and the THz-TDS ones, the amplitude value of bentonite is obtained to be 13.925 at the concentration of chromium ions of 0.05 mol/L, the mass of bentonite sample involved in adsorption of 1.5 g, and the detection frequency in THz-TDS measurements of 0.5 THz. The adsorption coefficient of bentonite is calculated to be 1.44%. Increase of the chromium ion concentration to 0.2 mol/L, and the mass of bentonite involved in adsorption to 3 g leads to the increase of the amplitude corresponding to adsorbed chromium ions to about 19.463, and the adsorption coefficient to about 2.1%. Obtained results demonstrate that terahertz technology is promising to meet the ever-increasing requirements in mineral analyses for rapid detection of chemical contaminants and measurement of the adsorption efficiencies of materials.

Polymer Pellet Fabrication for Accurate THz-TDS Measurements

We investigate fabrication of compacts using polytetrafluoroethylene (PTFE) and polyethylene (PE), and the effect of compaction conditions on their terahertz transmission properties. The conditions used to fabricate compressed powder samples for terahertz time-domain spectroscopy (THz-TDS) can impact the accuracy of the measurements and hence the interpretation of results. This study investigated the effect of compaction conditions on the accuracy of the THz-TDS analysis. Two polymers that are commonly used as matrix materials in terahertz spectroscopy studies were explored using a compaction simulator and a hydraulic press for sample preparation. THz-TDS was used to determine the refractive index and loss coefficient to compare the powder compacts (pellets) to the values of solid material. Sample porosity, axial relaxation and tensile strength were measured to assess the material’s suitability for terahertz spectroscopy. It was found that PTFE is the preferable material for creating THz-TDS samples due to its low porosity and high tensile strength. PE was found to show significant porosity at all compaction pressures, making it an unsuitable material for the accurate determination of optical parameters from THz-TDS spectroscopy measurements. The larger particle sizes of PE resulted in compacts that exhibited significantly lower tensile strength than those made from PTFE making handling and storage difficult.

Translation-Invariant Zero-Phase Wavelet Methods for Feature Extraction in Terahertz Time-Domain Spectroscopy.

Wavelet transform is an important tool in the computational signal processing of terahertz time-domain spectroscopy (THz-TDS) measurements. Despite its prevalence, the effects of using different forms of wavelet transforms in THz-TDS studies have not been investigated. In this paper, we explore the implications of using the maximal overlap discrete wavelet transform (MODWT) versus the well-known discrete wavelet transform (DWT). We demonstrate that the spectroscopic features extracted using DWT can vary over different overlapping frequency ranges. On the contrary, MODWT is translation-invariant and results in identical features, regardless of the spectral range used for its implementation.We also demonstrate that the details coefficients obtained by the multiresolution analysis (MRA) using MODWT are associated with zero-phase filters. In contrast, DWT details coefficients suffer from misalignments originated from the down- and upsampling operations in DWT pyramid algorithm. Such misalignments have adverse effects when it is critical to retain the exact location of the absorption lines. We study the differences of DWT and MODWT both analytically and experimentally, using reflection THz-TDS measurements of -lactose monohydrate. This manuscript can guide the researchers to select the right wavelet analysis tool for their specific application of the THz spectroscopy.