Terahertz Transmission Measurements Research Articles

3D Printed Fabry–Pérot Filters for Terahertz Spectral Range

3D printing is evolving into a standard tool for prototyping various optical components suitable for application in the terahertz range of the electromagnetic spectrum. This work takes the next step in this evolution by demonstrating the fabrication and subsequent evaluation of Fabry–Pérot interferometers (FPIs). Large optical area (centimetre scale) Fabry–Pérot transmission filters have been 3D printed with polylactic acid (PLA) using a commonly used low-cost 3D printer. The advantages of the proposed approach include low cost, rapid prototyping and repeatability. Terahertz transmission measurements for two demonstrated filter designs realised to target optimisation of either signal transmission or spectral filter performance have been performed using terahertz time-domain spectroscopy (THz-TDS) and demonstrate good agreement with the simulated response in the operating spectral band of 0.30–0.75 THz (wavelengths from 1000 down to 400 μm). The critical spectral characteristics assessed were the filter peak transmission magnitude, central wavelength and full width at half-maximum (FWHM) of the transmission peak, as well as the free spectral range (FSR). The signal transmission levels were observed to reach beyond 90% for the first series of filters that targeted optimisation of this aspect; however, this was accompanied by diminished out-of-band rejection and broader transmission peaks in comparison to the second series of filters which targeted the overall performance. For the latter filter series, the resolution in terms of FWHM values of the transmission peaks was reduced to 40–50 GHz, with the out-of-band rejection approaching a ratio of 10:1. This level of spectral performance, along with the achieved signal peak transmission characteristics of 65–75%, provides adequate performance for many applications harnessing the terahertz spectral range.

On the terahertz response of metal-gratings on anisotropic dielectric substrates and its prospective application for anisotropic refractive index characterization

This paper discusses the terahertz electromagnetic response of metallic gratings on anisotropic dielectric substrates. The metallic gratings consist of parallel gold stripes. Utilizing numerical simulations, we observe that it is possible to excite a series of resonant modes in these structures. These modes are affected differently by the different indices on the anisotropic substrate. An analytical model is discussed to show that modes associated with transmission peaks are due to the excitation of (a) Fabry–Pérot modes with polarization along the grating and/or (b) waveguide modes with polarization perpendicular to the grating. It is observed that the resonance associated with the TM1,1 mode is a narrow linewidth resonance which, in some particular circumstances, becomes nearly independent of substrate thickness. Therefore, from the spectral position of this resonance, it is possible to extract the out-of-plane component of the substrate refractive index with very small uncertainty. Based on this observation, we demonstrate the refractive index characterization of several lossless semiconductor substrates through frequency-domain polarized terahertz transmission measurements in the frequency range of 0.2–0.6 THz at normal incidence. The reliability of the technique is demonstrated on well-known materials, such as high-resistivity silicon and sapphire substrates. This technique is also applied for the characterization of a Fe-doped β-Ga2O3 single-crystal substrate.

Effect of oils on the transmission properties of a terahertz photonic crystal.

The transmission properties of a photonic crystal immersed in several different oils have been characterized using terahertz time domain spectroscopy in the spectral range of 0.3-1.5 THz. As in previous works, oil samples can be distinguished using terahertz transmission measurements. When the same oils are introduced into a photonic crystal, we find that the effective refractive index of the photonic crystal is sensitive to the properties of the oils and shows differences not seen in bulk measurements. These effects are described in detail and have potential applications in both the sensing of very small volumes of oils and in the fine control of the refractive indices of photonic crystals.

Bilayer MoS2 on silicon for higher terahertz amplitude modulation

The terahertz (THz) amplitude modulation has been experimentally demonstrated by employing bilayer molybdenum disulfide (MoS2) on high-resistivity silicon (Si). The Raman spectroscopy and x-ray photoelectron spectra confirm the formation of bilayer MoS2 film. The THz transmission measurements are carried out using a continuous wave (CW) frequency-domain THz system. This reveals the higher modulation depth covering wide THz spectra of 0.1–1 THz at low optical pumping power. The modulation depth up to 72.3% at 0.1 THz and 62.8% at 0.9 THz under low power optical excitation is achieved. After annealing, the strong built-in electric field is induced at the MoS2–Si interface due to p-type doping in MoS2. This improves modulation depth to 86.4% and 79.7%, respectively. The finite-difference time-domain (FDTD) based numerical simulations match well with the experimental results. The higher modulation depth at low optical power, broadband response, low insertion losses, and simplicity in the design are the key attributes of this THz modulator.

Terahertz anisotropic response of additively manufactured one-dimensional photonic crystals.

A polymer-based, one-dimensional photonic crystal exhibiting anisotropic responses was demonstrated in the terahertz frequency range. The photonic crystal was composed of alternating compact and low-density polymethacrylate layers. The low-density layers consisted of sub-wavelength sized columns, which were slanted 45° with respect to the substrate surface normal to achieve form-birefringence. Normal incidence polarized terahertz transmission measurements were carried out for characterization of the fabricated photonic crystals in the range from 82 to 125 GHz. The experimental data revealed a 2 GHz shift in the center frequency of the photonic bandgap as a function of in-plane orientation, well demonstrating the anisotropic behavior of the fabricated crystal. The transmission data were analyzed using stratified optical layer model calculations. A good agreement was found between the relevant model parameters and the corresponding design parameters.

Ultrafast multi-cycle terahertz measurements of the electrical conductivity in strongly excited solids

Key insights in materials at extreme temperatures and pressures can be gained by accurate measurements that determine the electrical conductivity. Free-electron laser pulses can ionize and excite matter out of equilibrium on femtosecond time scales, modifying the electronic and ionic structures and enhancing electronic scattering properties. The transient evolution of the conductivity manifests the energy coupling from high temperature electrons to low temperature ions. Here we combine accelerator-based, high-brightness multi-cycle terahertz radiation with a single-shot electro-optic sampling technique to probe the evolution of DC electrical conductivity using terahertz transmission measurements on sub-picosecond time scales with a multi-undulator free electron laser. Our results allow the direct determination of the electron-electron and electron-ion scattering frequencies that are the major contributors of the electrical resistivity.

Non-destructive quantification of fragmentation within tablets after compression from scattering analysis of terahertz transmission measurements.

Material deformation behaviour has a critical impact on tablet formation. Fragmentation is one of the key mechanisms affecting the strength of a final compact, however, quantitative methods for estimating fragmentation are often complex, destructive and time-consuming. The purpose of this study was to investigate the applicability of terahertz time-domain spectroscopy (THz-TDS) to quantify fragmentation upon tableting. Up to five size fractions of microcrystalline cellulose (MCC), dibasic calcium phosphate (DCP), and lactose monohydrate (lactose) in the range of <125µm up to the range of 355-500µm were compressed into tablets and analysed with THz-TDS. The effective refractive index and absorbance spectra of whole tablets were measured in transmission, and the optical properties were clearly affected by fragmentation upon compression. The scattering observed from the absorbance spectra was fitted into a power law equation (y=AνB). It was observed that up to pressures of 50MPa the values of parameter A that were extracted from the power law fit decreased exponentially with increasing compression pressure. For higher compression pressures the value of A remained constant. This observation was more pronounced for DCP, followed by lactose and then MCC and the effect was more pronounced for larger compared to smaller initial particles. The non-destructive measurements correlated with previously obtained results based on particle size distribution measurements of the particles before compression and those obtained from destructive analysis of tablets. The terahertz method can resolve similar differences in fragmentation behaviour upon compression compared to the particle size analysis but requires no sample preparation.

Mitigating the effects of granular scattering using cepstrum analysis in terahertz time-domain spectral imaging.

Terahertz (THz) imaging is a widely used technique in the study and detection of many chemicals and biomolecules in polycrystalline form because the spectral absorption signatures of these target materials often lie in the THz frequencies. When the size of dielectric grain boundaries are comparable to the THz wavelengths, spectral features can be obscured due to electromagnetic scattering. In this study, we first investigate this granular scattering effect in identification of chemicals with THz spectral absorption features. We then will propose a signal processing technique in the so-called “quefrency” domain to improve the ability to resolve these spectral features in the diffuse scattered THz images. We created a pellet with α-lactose monohydrate and riboflavin, two biologically significant materials with well-known vibrational spectral resonances, and buried the pellet in a highly scattering medium. THz transmission measurements were taken at all angles covering the half focal plane. We show that, while spectral features of lactose and riboflavin cannot be distinguished in the scattered image, application of cepstrum filtering can mitigate these scattering effects. By employing our quefrency-domain signal processing technique, we were able to unambiguously detect the dielectric resonance of lactose in the diffused scattering geometries. Finally we will discuss the limitation of the new proposed technique in spectral identification of chemicals.

Non-destructive Determination of Disintegration Time and Dissolution in Immediate Release Tablets by Terahertz Transmission Measurements

ABSTRACTPurposeThe aim of this study was to establish the suitability of terahertz (THz) transmission measurements to accurately measure and predict the critical quality attributes of disintegration time and the amount of active pharmaceutical ingredient (API) dissolved after 15, 20 and 25 min for commercial tablets processed at production scale.MethodsSamples of 18 batches of biconvex tablets from a production-scale design of experiments study into exploring the design space of a commercial tablet manufacturing process were used. The tablet production involved the process steps of high-shear wet granulation, fluid-bed drying and subsequent compaction. The 18 batches were produced using a 4 factor split plot design to study the effects of process changes on the disintegration time. Non-destructive and contactless terahertz transmission measurements of the whole tablets without prior sample preparation were performed to measure the effective refractive index and absorption coefficient of 6 tablets per batch.ResultsThe disintegration time (R2 = 0.86) and API dissolved after 15 min (R2 = 0.96) linearly correlates with the effective refractive index, neff, measured at terahertz frequencies. In contrast, no such correlation could be established from conventional hardness measurements. The magnitude of neff represents the optical density of the sample and thus it reflects both changes in tablet porosity as well as granule density. For the absorption coefficient, αeff, we observed a better correlation with dissolution after 20 min (R2 = 0.96) and a weaker correlation with disintegration (R2 = 0.83) compared to neff.ConclusionThe measurements of neff and αeff provide promising predictors for the disintegration and dissolution time of tablets. The high penetration power of terahertz radiation makes it possible to sample a significant volume proportion of a tablet without any prior sample preparation. Together with the short measurement time (seconds), the potential to measure content uniformity and the fact that the method requires no chemometric models this technology shows clear promise to be established as a process analyser to non-destructively predict critical quality attributes of tablets.

Transmission of reactive pulsed laser deposited VO2 films in the THz domain

This work reports on the characteristics of the insulator-to-metal transition (IMT) of reactive pulsed laser deposited vanadium dioxide (VO2) films in the terahertz (THz) frequency range, namely the transition temperature TIMT, the amplitude contrast of the THz transmission over the IMT ΔA, the transition sharpness ΔT and the hysteresis width ΔH. XRD analysis shows the sole formation of VO2 monoclinic structure with an enhancement of (011) preferential orientation when varying the O2 pressure (PO2) during the deposition process from 2 to 25mTorr. THz transmission measurements as a function of temperature reveal that VO2 films obtained at low PO2 exhibit low TIMT, large ΔA, and narrow ΔH. Increasing PO2 results in VO2 films with higher TIMT, smaller ΔA, broader ΔH and asymmetric hysteresis loop. The good control of the VO2 IMT features in the THz domain could be further exploited for the development of advanced smart devices, such as ultrafast switches, modulators, memories and sensors.

Field Intensity Detection of Individual Terahertz Pulses at 80 MHz Repetition Rate

We present a new approach to detect the intensity of individual terahertz pulses at repetition rates as high as 80 MHz. Our setup comprises a femtosecond fiber laser, an InGaAs-based terahertz emitter, a zero-bias Schottky detector, and a high-speed data acquisition unit. The detected pulses consist of two lobes with half-widths of 1–2 ns, which is much shorter than the inverse repetition rate of the laser. The system lends itself for high-speed terahertz transmission measurements, e.g., to study wetting dynamics in real time.

Ultrafast terahertz Faraday rotation in graphene

Terahertz (THz) Faraday rotation measurements were performed to investigate carrier dynamics in p-type Chemical vapor deposition (CVD) graphene. We used static and time-resolved polarization-sensitive THz transmission measurements in a magnetic field to probe free carriers in GaAs, InP, and Graphene. Static measurements probe the equilibrium carrier density and momentum scattering rate. Time-resolved (optical pump/THz probe) measurements probe the change in these quantities following photoexcitation. In a typical CVD graphene sample, we found that 0.5 ps following photoexcitation with 1 × 1013 photons/cm2 pulses at 800 nm the effective hole scattering time decreased from 37 fs to 34.5 fs, while the carrier concentration increased from 2.0 × 1012 cm−2 to 2.04 × 1012 cm−2, leading to a transient decrease in the conductivity of the film.

Tuning the properties of VO2 thin films through growth temperature for infrared and terahertz modulation applications

Results are reported on tuning the electrical and optical properties of sputter-deposited vanadium dioxide (VO2) thin films through control of substrate growth temperature (Ts). As Ts increases from 550 to 700 °C, the morphology changes from granular to smooth film and finally to rough film. X-ray diffraction shows the presence of VO2 along with additional weak features related to the presence of non-stoichiometric phases. Electrical measurements show the phase transition to change from abrupt to gradual as both the below- and above-transition resistivities vary with Ts. The transition and hysteresis dependences observed in electrical resistivity are similarly observed in infrared transmission. Terahertz transmission measurements show that high conductivity above the phase transition is more important in achieving high modulation depth than obtaining high resistivity below the transition. We attribute changes in the electrical and optical properties to the formation of V and O vacancies, which result in diverse valence states from the ideal V4+ of VO2. Low Ts produces material with V5+ states resulting in higher resistivity in both the insulating and metallic phases. Alternatively, high Ts introduces material with V3+ states leading to lower resistivity in the insulating phase but slightly higher resistivity in the metallic phase.

Ultrafast sub-threshold photo-induced response in crystalline and amorphous GeSbTe thin films

Pump-probe optical reflectivity and terahertz transmission measurements have been used to investigate time resolved sub-threshold photo-induced effects in crystalline and amorphous GeSbTe films at MHz repetition rates. The reflectivity in both phases exhibits long-lived modulations consistent with the sign of the changes that occur upon switching but of smaller magnitude. These can be understood by the generation of acoustic strains with the crystalline phase response dominated by thermal effects and the amorphous phase response associated with electronically induced changes. Evidence for a photo-induced distortion is observed in the amorphous phase which develops homogeneously within the excited region on few-picosecond time scales.

Structural, electrical, and terahertz transmission properties of VO2 thin films grown on c-, r-, and m-plane sapphire substrates

The structure, metal-insulator transition (MIT), and related Terahertz (THz) transmission characteristics of VO2 thin films obtained by sputtering deposition on c-, r-, and m-plane sapphire substrates were investigated by different techniques. On c-sapphire, monoclinic VO2 films were characterized to be epitaxial films with triple domain structure caused by β-angle mismatch. Monoclinic VO2 β angle of 122.2° and the two angles of V4+–V4+ chain deviating from the am axis of 4.4° and 4.3° are determined. On r-sapphire, tetragonal VO2 was determined to be epitaxially deposited with VO2 (011)T perpendicular to the growth direction, while the structural phase transformation into lower symmetric monoclinic phase results in (2¯11) and (200) orientations forming a twinned structure. VO2 on m-sapphire has several growth orientations, related with the uneven substrate surface and possible inter-diffusion between film and substrate. Measurements of the electrical properties show that the sample on r-sapphire has MIT property superior to the other two samples, with a resistivity change as large as 9 × 104 times and a transition window as narrow as 3.9 K, and it has the highest resistivity with the lowest free carrier density in the insulating phase. THz transmission measurements on VO2 films grown on r-plane sapphire substrates revealed intensity modulation depth as large as 98% over a broadband THz region, suggesting that VO2 films are ideal material candidates for THz modulation applications.

Application of Terahertz Radiation to Soil Measurements: Initial Results

Developing soil sensors with the possibility of continuous online measurement is a major challenge in soil science. Terahertz (THz) electromagnetic radiation may provide the opportunity for the measurement of organic material density, water content and other soil parameters at different soil depths. Penetration depth and information content is important for a functional soil sensor. Therefore, we present initial research on the analysis of absorption coefficients of four different soil samples by means of THz transmission measurements. An optimized soil sample holder to determine absorption coefficients was used. This setup improves data acquisition because interface reflections can be neglected. Frequencies of 340 GHz to 360 GHz and 1.627 THz to 2.523 THz provided information about an existing frequency dependency. The results demonstrate the potential of this THz approach for both soil analysis and imaging of buried objects. Therefore, the THz approach allows different soil samples to be distinguished according to their different absorption properties so that relations among soil parameters may be established in future.

Terahertz and far-infrared response of Ba x Sr1− x TiO3 films

Here, we report on the experimental study of terahertz (THz) and far-infrared dielectric response of polycrystalline Ba x Sr1− x TiO3 (x = 0.5, 0.7, and 0.8) films of 0.3−1 µm thicknesses deposited on a sapphire. THz and far-infrared transmission measurements were performed in 100–420 K temperature range covering the vicinity of T C of their bulk prototypes. We identified all polar optical phonons observed in bulk samples below 400 cm−1 of the same composition including soft and central modes and found some additional features, which we assigned to the depolarizing field effect coming from the structural inhomogeneity and unreleased strain.

On-chip near-field terahertz detection based on a two-dimensional electron gas

We report on a high-resolution terahertz (THz) imaging beyond the diffraction limit by using a two-dimensional electron gas (2DEG) in a GaAs/AlGaAs heterostructure. In this imaging device, all components: an aperture, a probe, and a detector are integrated on one GaAs/AlGaAs chip. Calculations based on a finite element method show that the presence of the probe changes the distribution profile of the evanescent field just behind the aperture, enhancing the coupling of the evanescent field to the 2DEG THz detector. THz transmission measurements demonstrate that the present device works as a near-field THz imaging detector. A near-field image of THz cyclotron emission in another 2DEG sample is also presented.

Extended Fano model of Extraordinary Electromagnetic Transmission through subwavelength hole arrays in the terahertz domain

We developed an extended Fano model describing the Extraordinary Electromagnetic Transmission (EET) through arrays of subwavelength apertures, based on terahertz transmission measurements of arrays of various hole size and shapes. Considering a frequency-dependent coupling between resonant and non-resonant pathways, this model gives access to a simple analytical description of EET, provides good agreement with experimental data, and offers new parameters describing the influence of the hole size and shape on the transmitted signal.

RESONANT TERAHERTZ SPECTROSCOPY OF BACTERIAL THIOREDOXIN IN WATER: SIMULATION AND EXPERIMENT

The experimental and computational study of bacterial thioredoxin, an E. coli protein, at THz frequencies is presented. The absorption spectrum of the entire protein in water was studied numerically in the terahertz range (0.1 – 2 THz). In our work, the initial X-ray molecular structure of thioredoxin was optimized using the molecular dynamical (MD) simulations at room temperature and atmospheric pressure. The effect of a liquid content of a bacterial cell was taken into account explicitly via the simulation of water molecules using the TIP3P water model. Using atomic trajectories from the room-temperature MD simulations, thioredoxin's THz vibrational spectrum and the absorption coefficient were calculated in a quasi harmonic approximation. For our terahertz transmission measurements, we used solutions of thioredoxin in distilled water obtained from Sigma. The experimental and simulated signatures are correlated and dominant peaks are close in frequencies. The results of this study demonstrate that terahertz spectroscopy is a promising tool in generating spectral data for cellular components of bio agents such as bacterial cells and spores.