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Microlens arrays (MLAs) which are increasingly popular micro-optical elements in compact integrated optical systems were fabricated by femtosecond direct laser write (fs-DLW) technique in the low-shrinkage SZ2080TM photoresist. High fidelity definition of 3D surfaces on IR transparent CaF2 substrates allowed to achieve ∼ 50% transmittance at chemical fingerprinting spectral region 2-5 μm wavelengths since MLAs were only ∼ 10 μm high corresponding to the numerical aperture of 0.3 (the lens height is comparable with the IR wavelength). To combine diffractive and refractive capabilities in miniaturised optical setup, a graphene oxide (GO) grating acting as a linear polariser was also fabricated by fs-DLW by ablation of a 1 μm-thick GO thin film. Such an ultra-thin GO polariser can be integrated with the fabricated MLA to add dispersion control at the focal plane. Pairs of MLAs and GO polarisers were characterised throughout visible-IR spectral window and numerical modeling was used to simulate their performance. Good match between experimental results of MLA focusing and simulations was achieved.

Polarisation analysis in the mid-infrared fingerprint region was carried out on thin (∼1 μm) Si and SiO2 films evaporated via glancing angle deposition (GLAD) method at 70∘ to the normal. Synchrotron-based infrared microspectroscopic measurements were carried out on the Infrared Microspectroscopy (IRM) beamline at Australian Synchrotron. Specific absorption bands, particularly Si-O-Si stretching vibration, was found to follow the angular dependence of ∼cos2θ, consistent with the absorption anisotropy. This unexpected anisotropy stems from the enhanced absorption in nano-crevices, which have orientation following the cos2θ angular dependence as revealed by Fourier transforming the image of the surface of 3D columnar films and numerical modeling of light field enhancement by sub-wavelength nano-crevices.

Capabilities of the Attenuated Total Reflection (ATR) at THz wavelengths for increased sub-surface depth characterisation of (bio-)materials is presented. The penetration depth of a THz evanescent wave in biological samples is dependent on the wavelength and temperature and can reach 0.1-0.5 mm depth due to strong refractive index change ∼0.4 of the ice-water transition; this is quite significant and important when studying biological samples. Technical challenges are discussed when using ATR for uneven, heterogeneous, high refractive index samples with possibility of frustrated total internal reflection (a breakdown of the ATR reflection-mode into transmission-mode). Local field enhancements at the interface are discussed with numerical/analytical examples. Maxwell’s scaling was used to model behaviour of absorber-scatterer inside materials at the interface with ATR prism for realistic complex refractive indices of bio-materials. Modality of ATR with polarisation analysis is proposed and its principle illustrated, opening an invitation for its experimental validation. The sensitivity of the polarised ATR mode to the refractive index between the sample and ATR prism is revealed. Design principles of polarisation active optical elements and spectral filters are outlined. The results and concepts are based on experiments carried out at the THz beamline of the Australian Synchrotron.

Anisotropy of absorbance (dichroism) and birefringence limits spatial resolution, sensitivity during quantitative detection of trace analytes, as well as spectral imaging in the near-IR and mid-IR spectral ranges. Here we show hyperspectral imaging capable of determining retardance and absorbance due to small changes in the real and imaginary parts of the refractive index ∼Δn and ∼Δκ at each single point of a measurement at diffraction limited resolution. This single-beam technique allows the retrieval of the phase and amplitude information by virtue of a twice different angular dependence of Δn and Δκ on the sample orientation angle. It has potential applications in analytical science, multi-dimensional optical memory devices, and forensic/defense/sensor fields.

Capabilities of the attenuated total reflection (ATR) at THz wavelengths for increased sub-surface depth characterisation of (bio-)materials are presented. The penetration depth of a THz evanescent wave in biological samples is dependent on the wavelength and temperature and can reach 0.1–0.5 mm depth, due to the strong refractive index change ∼0.4 of the ice-water transition; this is quite significant and important when studying biological samples. Technical challenges are discussed when using ATR for uneven, heterogeneous, high refractive index samples with the possibility of frustrated total internal reflection (a breakdown of the ATR reflection mode into transmission mode). Local field enhancements at the interface are discussed with numerical/analytical examples. Maxwell’s scaling is used to model the behaviour of absorber–scatterer inside the materials at the interface with the ATR prism for realistic complex refractive indices of bio-materials. The modality of ATR with a polarisation analysis is proposed, and its principle is illustrated, opening an invitation for its experimental validation. The sensitivity of the polarised ATR mode to the refractive index between the sample and ATR prism is numerically modelled and experimentally verified for background (air) spectra. The design principles of polarisation active optical elements and spectral filters are outlined. The results and proposed concepts are based on experimental conditions at the THz beamline of the Australian Synchrotron.

Birefringence of 3 &times, 10 - 3 is demonstrated inside cross-sectional regions of 100 &mu, m, inscribed by axially stretched Bessel-beam-like fs-laser pulses along the c-axis inside sapphire. A high birefringence and retardance of &lambda, / 4 at mid-visible spectral range (green) can be achieved using stretched beams with axial extension of 30&ndash, 40 &mu, m. Chosen conditions of laser-writing ensure that there are no formations of self-organized nano-gratings. This method can be adopted for creation of polarization optical elements and fabrication of spatially varying birefringent patterns for optical vortex generation.

A focal plane array (FPA) detector was used for hyperspectral imaging in the infrared (IR) spectral region using thermal and synchrotron light sources. FPA Fourier-transform IR (FTIR) imaging microspectroscopy will be able to monitor real time changes at specific absorption bands when combined with high brightness synchrotron source. In this study, several types of samples with unique structural motifs were selected and used for assessing the capability of the FPA-FTIR imaging technique. It was shown that the time required for polariscopy at IR wavelengths can be substantially reduced by the FPA-FTIR imaging approach. By using natural and laser fabricated polymers with sub-wavelength features, alignment of absorbing molecular dipoles was revealed as well as higher order patterns (laser fabricated structures). Micro-spectroscopy of absorber orientation reveals alignment patterns even when they are not spatially resolved.

Polarised light imaging microscopy, with the addition of a liquid crystal (LC) phase retarder, was used to determine the birefringence of silk fibres with high (∼1 μm) spatial resolution. The measurement was carried out with the silk fibres (the optical slow axis) and the slow axis of the LC-retarder set at parallel angles. The direct fit of the transmission data allowed for high fidelity determination of the birefringence Δn ≈ 1.63 × 10−2 (with ∼2% uncertainty) of the brown silk fibre, (Antheraea pernyi) averaged over the wavelength range λ = (425–625) nm. By measuring retardance at four separate wavelengths, it was possible to determine the true value of the birefringence of a thicker sample when an optical path may include a large number of wavelengths. The numerical procedures and required hardware are described for the do-it-yourself assembly of the imaging polariscope at a fractional budget compared to commercial units.

Inter-related mechanical, thermal, and optical macroscopic properties of biomaterials are defined at the nanoscale by their constituent structures and patterns, which underpin complex functions of an entire bio-object. Here, the temperature diffusivity of a cicada (Cyclochila australasiae) wing with nanotextured surfaces was measured using two complementary techniques: a direct contact method and IR imaging. The 4-6-μm-thick wing section was shown to have a thermal diffusivity of α⊥ = (0.71 ± 0.15) × 10(-7) m(2)/s, as measured by the contact temperature wave method along the thickness of the wing; it corresponds to the inherent thermal property of the cuticle. The in-plane thermal diffusivity value of the wing was determined by IR imaging and was considerably larger at α∥ = (3.6 ± 0.2) × 10(-7) m(2)/s as a result of heat transport via air. Optical properties of wings covered with nanospikes were numerically simulated using an accurate 3D model of the wing pattern and showed that light is concentrated between spikes where intensity is enhanced by up to 3- to 4-fold. The closely packed pattern of nanospikes reduces the reflectivity of the wing throughout the visible light spectrum and over a wide range of incident angles, hence acting as an antireflection coating.

Molecular alignment underpins optical, mechanical, and thermal properties of materials, however, its direct measurement from volumes with micrometer dimensions is not accessible, especially, for structurally complex bio-materials. How the molecular alignment is linked to extraordinary properties of silk and its amorphous-crystalline composition has to be accessed by a direct measurement from a single silk fiber. Here, we show orientation mapping of the internal silk fiber structure via polarisation-dependent IR absorbance at high spatial resolution of 4.2 μm and 1.9 μm in a hyper-spectral IR imaging by attenuated total reflection using synchrotron radiation in the spectral fingerprint region around 6 μm wavelength. Free-standing longitudinal micro-slices of silk fibers, thinner than the fiber cross section, were prepared by microtome for the four polarization method to directly measure the orientational sensitivity of absorbance in the molecular fingerprint spectral window of the amide bands of β-sheet polypeptides of silk. Microtomed lateral slices of silk fibers, which may avoid possible artefacts that affect spectroscopic measurements with fibers of an elliptical cross sections were used in the study. Amorphisation of silk by ultra-short laser single-pulse exposure is demonstrated.

Grid polarisers 3D-printed out of commercial acrilic resin were tested for the polariser function and showed spectral regions where the dichroic ratio and implying importance of molecular and/or stress induced anisotropy. Metal-coated 3D-printed THz optical elements can find a range of applications in intensity and polarization control of IR-THz beams. The used 3D printing method allows for fabrication of an arbitrary high aspect ratio grid polarisers. Polarization analysis of synchrotron THz radiation was carried out with a standard stretched polyethylene polariser and revealed that the linearly polarized (horizontal) component contributes up to 22% ± 5% to the circular polarized synchrotron emission extracted by a gold-coated mirror with a horizontal slit inserted near the bending magnet edge. Comparison with theoretical predictions shows a qualitative match with dominance of the edge radiation.

International audience; The purpose of this article is to present a new calibration procedure for spectroscopic measurements using an infrared focal plane array (IRFPA) spectrometer on highly opaque middle-wave infrared (MWIR) media. The procedure is based on the properties of the IRFPA camera and especially the integration time (IT), which is the main parameter that can be adjusted to control the sensitivity of the measurements. The goal of the paper is to experimentally validate this dependence with the direct reference intensity light coming out of the IR monochromator in order to predict the spectrum shape and intensity level in a range out of the camera saturation. This method allows determining spectrum used as background for transmittance calculation. It has been applied in the case of measurement of water transmittance, which is a highly opaque medium and whose measurement requires high ITs. The main result is the ability to take an IR spectroscopic imaging measurement through 300 µm of water and the determination of its transmittance with sufficient sensitivity due to the proposed calibration procedure. This procedure allows the possibility of transitory studies in heterogeneous aqueous media.

Nano-textured Au surfaces were prepared on pre-stretched 2D polystyrene (PS) sheets sputtered with different thicknesses of Au. The Au-coated PS was subjected to thermal annealing above the glass transition temperature at ∼150 °C, thus undergoing surface area rescaling via a volume phase transition. The yellow color of the Au changed from the typical mirror-like appearance to a diffusive dark yellow, progressing to dark brown at the smallest feature size, hence, electromagnetic energy was coupled into the substrate. While the surface area footprint is the same after shrinking the PS, the roughness can be modified from the nano- to the micro-scale for different initial thicknesses of sputtered Au. The nanometer-sized features of surface wrinkles on the Au films make them suitable for surface-enhanced Raman scattering (SERS) sensors that can reach ∼104 counts per s per mW. The thermal diffusivity of the contracted surfaces was determined by a non-contact temperature wave method and was larger than that of PS (α ≃ 1.1 × 10−7 m2 s−1) with a linear scaling on the Au thickness: each 10 nm addition of Au increased the diffusivity by 4%. This allows improved heat dissipation from the laser irradiated spot during SERS measurements.

Three dimensional (3D) fast (< 0.5 hour) printing of micro-optical elements down to sub-wavelength resolution over 100 micrometers footprint areas using femtosecond (fs-)laser oscillator is presented. Using sub-1 nJ pulse energies, optical vortex generators made of polymerised grating segments with an azimuthally changing orientation have been fabricated in SZ2080 resist; width of polymerised rods was ~150 nm and period 0.6-1 micrometers. Detailed phase retardance analysis was carried out manually with Berek compensator (under a white light illumination) and using an equivalent principle by an automated Abrio implementation at 546 nm. Direct experimental measurements of retardance was required since the period of the grating was comparable (or larger) than the wavelength of visible light. By gold sputtering, transmission-type optical vortex generators were turned into reflective ones with augmented retardance, n.h defined by the form birefringence, n, and the height h = 2d where d is the thickness of the polymerised structure. Retardance reached 315 nm as measured with Berek compensator at visible wavelengths. Birefringent phase delays of 180 degrees (or half-wavelength) required for high purity vortex generators can be made based on the proposed approach. Optical vortex generators for telecom wavelengths with sub-wavelength patterns of azimuthally oriented gratings are amenable by direct laser polymerisation., Pacific Rim Laser Damage 2017: Optical Materials for High Power Lasers (PLD17); Shanghai, China 21 - 24 May 2017. Invited talk

Molecular alignment underpins optical, mechanical, and thermal properties of materials, however, its direct measurement from volumes with micrometer dimensions is not accessible, especially, for structurally complex bio-materials. How the molecular alignment is linked to extraordinary properties of silk and its amorphous-crystalline composition has to be accessed by a direct measurement from a single silk fiber. Here, we show orientation mapping of the internal silk fiber structure via polarisation-dependent IR absorbance at high spatial resolution of 4.2 μm and 1.9 μm in a hyper-spectral IR imaging by attenuated total reflection using synchrotron radiation in the spectral fingerprint region around 6 μm wavelength. Free-standing longitudinal micro-slices of silk fibers, thinner than the fiber cross section, were prepared by microtome for the four polarization method to directly measure the orientational sensitivity of absorbance in the molecular fingerprint spectral window of the amide bands of β-sheet polypeptides of silk. Microtomed lateral slices of silk fibers, which may avoid possible artefacts that affect spectroscopic measurements with fibers of an elliptical cross sections were used in the study. Amorphisation of silk by ultra-short laser single-pulse exposure is demonstrated., An Author Correction to this article was published on 24 January 2018.

This work aims to achieve contactless absolute-temperature measurements of infrared-semi-transparent solids using an infrared thermal and spectroscopic imaging technique. The multispectral thermo-transmittance coefficient fields in the 3–5 μm wavelength range for Sapphire, KBr, and Silicon are determined to be 6 × 10−4 K−1, 4 × 10−4 K−1, and −3 × 10−3 K−1, respectively. The most interesting result is the high temperature-dependent transmittance coefficient in the middle wave infrared region. With these coefficients, the absolute temperature fields in a range from room temperature to 140 °C are shown.

Polariscopy is demonstrated using hyperspectral imaging with a focal plane array (FPA) detector in the infrared (IR) spectral region under illumination by thermal and synchrotron light sources. FPA Fourier-transform IR (FTIR) imaging microspectroscopy is useful for monitoring real time changes at specific absorption bands when combined with a high brightness synchrotron source. In this study, several types of samples with unique structural motifs were selected and used for assessing the capability of polariscopy under this FPA-FTIR imaging technique. It was shown that the time required for polariscopy at IR wavelengths can be substantially reduced by the FPA-FTIR imaging approach. By using natural and laser fabricated polymers with sub-wavelength features, alignment of absorbing molecular dipoles and higher order patterns (laser fabricated structures) were revealed. Spectral polariscopy at the absorption peaks can reveal the orientation of sub-wavelength patterns (even when they are not spatially resolved) or the orientation of the absorbing dipoles.

To study the kinetics of phase transitions and to obtain artificial materials with improved physical properties, a set of thin-film high-sensitivity sensors for ultra-fast scanning nanocalorimetry has been constructed. To investigate the dynamics of the temperature distribution in thin-film calorimetric sensors, high-resolution high-speed infrared thermography has been applied as a tool of non-contact thermal imaging in combination with ultra-fast scanning calorimetry. The dynamic heat-transfer problem, causing the temperature distribution in a thin-film sensor at ultrafast scanning of temperature, has been solved analytically. Analytical solutions for square and circular geometry have been obtained and compared with the temperature profiles obtained by infrared thermographic measurements. A theoretical background for ultra-fast-cooling experiments has been formulated. The origin of the restrictions imposed on the maximum attainable controlled cooling rate has been investigated. It is shown that thin-film sensors can be applied for controlled ultra-fast cooling, as well as heating, at 108 K/s and even 109 K/s.To study the kinetics of phase transitions and to obtain artificial materials with improved physical properties, a set of thin-film high-sensitivity sensors for ultra-fast scanning nanocalorimetry has been constructed. To investigate the dynamics of the temperature distribution in thin-film calorimetric sensors, high-resolution high-speed infrared thermography has been applied as a tool of non-contact thermal imaging in combination with ultra-fast scanning calorimetry. The dynamic heat-transfer problem, causing the temperature distribution in a thin-film sensor at ultrafast scanning of temperature, has been solved analytically. Analytical solutions for square and circular geometry have been obtained and compared with the temperature profiles obtained by infrared thermographic measurements. A theoretical background for ultra-fast-cooling experiments has been formulated. The origin of the restrictions imposed on the maximum attainable controlled cooling rate has been investigated. It is shown that thin-film...

In this paper, simultaneous microscopic measurements of thermal and spectroscopic fields of a paraffin wax n-alkane phase change material are reported. Measurements collected using an original set-up are presented and discussed with emphasis on the ability to perform simultaneous characterization of the system when the proposed imaging process is used. Finally, this work reveals that the infrared wavelength contains two sets of important information. Furthermore, this versatile and flexible technique is well adapted to characterize many systems in which the mass and heat transfers effects are coupled.

We have developed an instrument for the measurement of microscale infrared (IR) spectroscopic thermal images in a dynamic mode. The high speed image processing based on the two-image technique enables a simultaneous spectroscopic and thermal imaging that detects a dynamic change of IR absorption spectrum by a transmission mode, and the emission of IR radiation from the sample surface. With this dynamic mode scan at 200 Hz, the spectra at any temperatures are free from the base line variation that comes from the temperature dependent surface emission signal, which can be subtracted from the total signal. In addition, the precise calibration between temperature – emissivity in phase transitions has become possible. The phase transitions, from liquid to hexagonal – monoclinic crystal systems, of normal tetracosane (n-C24H50), is presented as an example of the dynamic mode spectroscopic thermal imaging in microscale of normal alkane.

We have been developing the instruments for microscale IR thermography with original optics’ designs and a signal superimposed system, which has been applied to (1) pseudo acceleration of temporal resolution of periodic thermal events, (2) pixel by pixel emissivity-temperature conversion, (3) micro-scale flying spot method. A novel portable instrument design for microscale IR thermography improves the differential temperature and temporal resolution of images that can be obtained even with uncooled detectors.

Pyramidal silicon nanospikes, termed black-Si (b-Si), with controlled height of 0.2 to 1 μm, were fabricated by plasma etching over 3-in wafers and were shown to act as variable density filters in a wide range of the IR spectrum 2.5 to 20 μm, with transmission and its spectral gradient dependent on the height of the spikes. Such variable density IR filters can be utilized for imaging and monitoring applications. Narrow IR notch filters were realized with gold mesh arrays on Si wafers prospective for applications in surface-enhanced IR absorption sensing and “cold materials” for heat radiation into atmospheric IR transmission window. Both types of filters for IR: spectrally variable and notch are made by simple fabrication methods.