Thickness Of Thin Films Research Articles

Spectroscopic ellipsometry utilizing frequency division multiplexed lasers

Spectroscopic ellipsometry (SE), which measures the thickness of thin films in a non-contact way with an accuracy of angstroms, has been widely used for optical metrology. Several types of SE are available both commercially and in research, although they require specific implementations depending on the application. Here, we theoretically and experimentally demonstrate the Frequency Division Multiplexing Spectroscopic Ellipsometry (FDM-SE) technique. With respect to conventional rotating polarizing element ellipsometry, our variant uses discrete-wavelength intensity-modulated laser diodes. This modification enables the measurement of optical properties of materials at multiple wavelengths simultaneously. We further compare the performance of the FDM-SE to a commercial instrument by measuring the thickness of SiO2 films on a Si wafer, obtaining a difference between the measured thicknesses with both methods of less than 5 Å. The proposed FDM-SE technique therefore provides a more efficient alternative to conventional SE with a high accuracy for thickness measurements.

Chiral spin-liquid-like state in pyrochlore iridate thin films

The pyrochlore iridates have become ideal platforms to unravel fascinating correlated and topological phenomena that stem from the intricate interplay among strong spin-orbit coupling, electronic correlations, lattice with geometric frustration, and itinerancy of the 5d electrons. The all-in-all-out antiferromagnetic state, commonly considered as the magnetic ground state, can be dramatically altered in reduced dimensionality, leading to exotic or hidden quantum states inaccessible in bulk. Here, by means of magnetotransport, resonant elastic and inelastic x-ray scattering experiments, we discover an emergent quantum disordered state in (111) Y2Ir2O7 thin films (thickness ≤30 nm) persisting down to 5 K, characterized by dispersionless magnetic excitations. The anomalous Hall effect observed below an onset temperature near 125 K corroborates the presence of chiral short-range spin configurations expressed in non-zero scalar spin chirality, breaking the macroscopic time-reversal symmetry. The origin of this chiral state is ascribed to the restoration of magnetic frustration on the pyrochlore lattice in lower dimensionality, where the competing exchange interactions together with enhanced quantum fluctuations suppress any long-range order and trigger spin-liquid-like behavior with degenerate ground-state manifold.

A High-Sensitivity Fiber Optic Soil Moisture Sensor Based on D-Shaped Fiber and Tin Oxide Thin Film Coatings

We present a high-sensitivity fiber optic soil moisture sensor based on side-polished multimode fibers and lossy mode resonance (LMR). The multimode fibers (MMFs), after side-polishing to form a D-shaped structure, are coated with a single-layer SnO2 thin film by electron beam evaporation with ion-assisted deposition technology. The LMR effect can be obtained when the refractive index of the thin film is positive and greater than its extinction coefficient and the real part of the external medium permittivity. The D-shaped fiber optic soil moisture sensor was placed in soil, allowing moisture to penetrate into the thin film microstructure, and it observed the resonance wavelength shift in LMR spectra to measure the relative humidity change in soil. Meanwhile, an Arduino electronic soil moisture sensing module was used as the experimental control group, with soil relative humidity ranging from 10%RH to 90%RH. We found that the D-shaped fiber with a residual thickness of 93 μm and SnO2 thin film thickness of 450 nm had a maximum sensitivity of 2.29 nm/%RH, with relative humidity varying from 10%RH to 90%RH. The D-shaped fiber also demonstrates a fast response time and good reproducibility.

Gas-specific adsorption capability of titanium dioxide and MXene nanocomposite thin films prepared by ultrasonic spray printing using inks oxidized at room temperature

The development of two-dimensional (2D) layered MXene materials has opened new possibilities for gas adsorption applications due to their high specific surface area, tunable surface chemistry, and excellent selectivity towards specific gases. These materials exhibit tremendous potential in adsorption-based gas separation and detection, particularly due to their strong interactions with target gas molecules, making them highly effective in gas removal and detection applications. However, currently available methods for synthesizing these oxidized nanocomposite inks are limited by the typically high temperatures involved. The present work addresses this issue by developing titanium dioxide and MXene (TiO2/Ti3C2 MXene) nanocomposite inks, where TiO2 nanoparticles are formed between the layers of the Ti3C2 MXene via oxidation in solution state under extended exposure in an oxygen rich atmosphere at room temperature. As a proof of concept, gas adsorption studies are conducted by applying the TiO2/Ti3C2 MXene nanocomposite inks onto gold-coated silicon wafers via an ultrasonic spray printing method. The gas adsorption results demonstrate that the TiO2/Ti3C2 MXene nanocomposites possess excellent adsorption selectivity toward methane and butane among alkane gases, and can achieve maximum adsorption capacities of 8.62 and 18.8 cm3/g, respectively. The results of ultrasonic spray printing quality tests conducted for different numbers of printed layers using the proposed TiO2/Ti3C2 MXene nanocomposite ink demonstrate that the film thickness can be regulated by controlling the number of printed layers, and the average thin film thickness remains only 0.313 μm for 10 printed layers. Meanwhile, the average roughness of the films resides between 0.130 μm (3 layers) and 0.220 μm (8 layers), which is uniformly and less than the average roughness of 0.225 μm measured for the original gold-plated silicon wafer. Hence, by employing facile ink-based printing techniques, such as ultrasonic spray printing, thin films with controlled thickness can be fabricated, thereby laying the foundation for their practical applications in environmental monitoring and industrial gas separation.

A mathematical model for predicting the electro-mechanical behavior of biomimetic crack sensors: Effect of crack depth and gap

Various biomimetic microstructures, such as porous, cracks, wrinkles, micro-pyramids, and micro-domes, are applied to improve the sensing performance of mechanical sensors. Among them, the crack-based strain sensors are widely investigated due to high sensitivity and fast response time. To clearly describe the relationship between crack morphology and sensor sensitivity, a mathematical model is developed for investigating the performance of a poly(3,4-ethylenedioxythiophene)-silicon oxide/polydimethylsiloxane (SiOx/PDMS) based crack strain sensor. First, the displacement field of a crack tip is calculated based on the theory of fracture mechanics, and the mathematical relationship between the crack depth, crack gap, and strain is obtained. The predicted crack depth of the SiOx thin film's thicknesses in 7.91 μm (SiOx/PDMS-7.91) is 2.82 μm, with the error of 3.75% compared to the experimental result. Correspondingly, the deviation of SiOx/PDMS-7.91 is 5.74% between the predicted crack gap and the experimental data. Second, above the aforementioned crack tip characteristics, the mathematical model based on crack edges contacts probability (CECP) is used to construct the relationship between the crack tip characteristics, applied stress, and device sensitivity. The maximum predicted sensitivity can reach 3562.68 compared with the experimental data of 3800.44, and the deviation is about 6.26%. Moreover, the CECP model has good universality with the other reported crack-based strain sensors. It can be concluded that crack morphology affects the distribution and quantity of conductive paths. When the strain sensor is subjected to external forces, brittle thin films generate a certain number of bumped-like elements for microcracks. The wider and deeper crack will increase the relative resistance change and the decrease of conductive paths, resulting in a rapid increase in the sensitivity of the strain sensor.

Calibration-free thickness and temperature measurement of oil films using broadband near-infrared absorption spectroscopy

Abstract This paper assesses broadband absorption spectroscopy for calibration-free, single-ended thickness and temperature measurements of thin liquid films with a free interface using spectrally resolved intensity measurements. The spectroscopic properties of the liquid in question, here an oil lubricant, are characterized using a Fourier Transform Infrared (FTIR) spectrometer. This data forms the basis for a measurement model that is used to infer the thickness and temperature of films wetting metal surfaces based on broadband spectral transmission measurements. The technique is demonstrated by inferring the properties of static films of known properties as well as free films on a rotating metal disk.

The Effect of O2 Flow Rate on Nanostructured TiO2 Thin Films Prepared by Reactive DC Magnetron Sputtering with OAD Technique

In this project, we explored how different oxygen flow rates influenced the creation of TiO2 nanostructures in thin films using magnetron sputtering preparation with oblique angle deposition (OAD) technique. The experiment involved oxygen flow rates of 20, 40, 60, 80 and 100 sccm along with a constant argon flow at 20 sccm. Morphological analysis by FE-SEM was performed to determine film thickness and deposition rate. In a subsequent stage, thin films thickness was confirmed to be 100 nm. After coating, specimens were annealed at 300°C for 2 h using various O2 flow rates. FE-SEM revealed morphological changes, GIXRD to explore crystal structures, and UV-Vis spectrophotometry to measure light transmittance. The results showed an optimal oxygen flow rate at 60 sccm, with annealed specimens exhibiting anatase structure and promising light transmittance of 73-83%.

Surface plasmon resonance spectrometer in the double prism configuration: Fast characterization of the thickness and dielectric constant dispersion of thin films

Surface plasmon resonance (SPR)-based sensors are widely used to measure thin film thickness, material dielectric constants, biomolecular interactions, and more. However, conventional monochromatic setups limit the simultaneous determination of dielectric constant dispersion and film thickness. To address this, we developed a fully automated wavelength-resolved SPR using a double-prism Kretschmann configuration. Combining this setup with a computational approach based on Fresnel equations and the Nelder-Mead optimization method, we introduced a novel technique to simultaneously determine the dispersion (520–1000 nm) of the real and imaginary components of the dielectric constant of thin films directly from SPR curves. As far as we know, this is the first time an SPR spectrometer has accomplished such a remarkable achievement. As a proof of concept for biosensor applications, we determined the thickness and dielectric constant dispersion of gold and bovine serum albumin thin film. These thicknesses were validated through atomic force microscopy, and the dielectric constants aligned closely with literature values obtained by ellipsometry. The developed SPR system enables precise measurements of these parameters within a short time (10 minutes), paving the way for future applications in advanced sensors and biosensors.

Wafer-level metal thin film thickness scanning based on multiple probe wavelengths nanosecond transient thermoreflectance

The present metal film thickness (dMetal) measurement methods (e.g., profiler and electron microscope) are not able to simultaneously achieve non-invasion, wide measurement range, high-resolution, and wafer-level scanning. In this work, a dMetal measurement method based on multiple probe wavelengths transient thermoreflectance (MW-TTR) is developed. Through a systematic sensitivity discussion, the guidance for reliable dMetal measurement is illustrated theoretically. The realization of measuring different types of metals (Au, Al, Ni, Ti) is achieved with different wavelengths of probe lights. After the rigorous comparison with profiler and picosecond acoustic measurement, the accuracy of measuring nanosized film is verified (∼1% difference). The fitting uncertainties of dMetal are < 5 % for Au and Al metals. The high-throughput wafer-level scanning measurement, with a spatial resolution of ∼ 50 μm, is also realized by integrating automatic displacement control and deep learning fast predicting model into MW-TTR. Spatial mapping of dMetal is consistent with profiler measurement (∼5% deviation in 2000 μm length).

Determination of Optical and Structural Parameters of Thin Films with Differently Rough Boundaries

The optical characterization of non-absorbing, homogeneous, isotropic polymer-like thin films with correlated, differently rough boundaries is essential in optimizing their performance in various applications. A central aim of this study is to derive the general formulae necessary for the characterization of such films. The applicability of this theory is illustrated through the characterization of a polymer-like thin film deposited by plasma-enhanced chemical vapor deposition onto a silicon substrate with a randomly rough surface, focusing on the analysis of its rough boundaries over a wide range of spatial frequencies. The method is based on processing experimental data obtained using variable-angle spectroscopic ellipsometry and spectroscopic reflectometry. The transition layer is considered at the lower boundary of the polymer-like thin film. The spectral dependencies of the optical constants of the polymer-like thin film and the transition layer are determined using the Campi–Coriasso dispersion model. The reflectance data are processed using a combination of Rayleigh–Rice theory and scalar diffraction theory in the near-infrared and visible spectral ranges, while scalar diffraction theory is used for the processing of reflectance data within the ultraviolet range. Rayleigh–Rice theory alone is sufficient for the processing of the ellipsometric data across the entire spectral range. We accurately determine the thicknesses of the polymer-like thin film and the transition layer, as well as the roughness parameters of both boundaries, with the root mean square (rms) values cross-validated using atomic force microscopy. Notably, the rms values derived from optical measurements and atomic force microscopy show excellent agreement. These findings confirm the reliability of the optical method for the detailed characterization of thin films with differently rough boundaries, supporting the applicability of the proposed method in high-precision film analysis.

Tuning Thin Film Thickness and Porosity with Layer‐by‐Layer Submicronic Particles Assembly

AbstractPorous NiO films were prepared using Layer‐by‐Layer assembly of submicronic β‐Ni(OH)2 nanoplatelets and size‐controlled poly(methyl methacrylate) (PMMA) particles. β‐Ni(OH)2/PMMA thin films were elaborated using different PMMA particle sizes and concentrations. The elaborated films were then heated at a temperature of 325 °C in air for one hour to form porous NiO films by calcining β‐Ni(OH)2 nanoplatelets. PMMA polymeric particles were also calcined during this process, leading to film porosity. Thermal treatment experiments clearly showed a relationship between PMMA particle size and film properties i. e., porosity and thickness. NiO films exhibited huge pores, around 1 μm, and matter loss after calcination when PMMA particles with a diameter of 190±43 nm were employed. Partial collapsing of the films was also denoted. Experiments were then carried out by decreasing PMMA particle size (100±19 nm) leading to cohesive NiO films. Finally, the specific surface area (SSA) of the NiO films prepared with PMMA particles of 100 nm was determined by adsorption‐desorption of nitrogen gas using the BET (Brunauer–Emmet–Teller) method. This showed an increase in SSA with PMMA particle concentration.

Investigation of Hf/Ti bilayers for the development of transition-edge sensor microcalorimeters.

The superconducting properties of 85 nm thick hafnium thin films with a 5 nm thick titanium layer on top have been investigated for three different geometries, that is, a film covering the entire 7 × 7 mm2 chip surface, bridges with a width of 200 μm and length up to 1800 μm, and bridges in the form of squares with sides from 100 to 1000 μm. The bridges were formed by a photolithographic lift-off process and are intended to be used as the main sensing element of a microcalorimeter based on a transition-edge sensor (TES) in experiments to determine the magnetic moment of neutrinos. Based on the measurements of the critical current, the critical temperature, and the width of the superconducting transition, we estimate the energy resolution δE of the TES prototypes, showing that it is possible to fabricate microcalorimeters with δE less than 1 eV using these films.

Spectral in situ ellipsometer for thin layer measurements in thermonuclear fusion applications.

Ellipsometry is widely used to characterize the thickness and optical parameters of thin films deposited, for example, in industrial processes. It is based on the measurement of polarization change upon reflection of, for example, visible light at a material sample. Commercially available devices are designed for stationary applications and often rely on precise geometric adjustment of the optical setup to maximize the measurement precision. In this work, a simplified spectral ellipsometer is proposed and tested with the aim of flexible implementation in space-limited applications in thermonuclear fusion research: on the one hand, as a hand-held device for large thickness scans of coatings deposited on first-wall components inside the vacuum vessel of fusion experiments and, on the other hand, for in situ monitoring of plasma deposited coatings on diagnostic vacuum windows, reducing their transmission in the optical spectral range, which hampers spectroscopic diagnostics in long-pulse plasma experiments. The simplicity of the hardware setup is partially compensated by complex Bayesian inference of the coating parameters, which incorporates all uncertainties of the measurement and the model and provides a quantitative assessment of the final uncertainties of inferred coating parameters. The Bayesian inference based on synthetic observations is also used to optimize the diagnostic design, identifying the limiting parameters and quantifying their impact on final accuracy. For real-time analysis of layer thickness on first-wall components in fusion devices measured with the hand-held device, a neural network based analysis has been implemented, and promising test results are presented.

Silica conversion of polysilazanes by low-temperature plasma jet generated from Ar and water-vapor mixed gas

Perhydropolysilazane (PHPS), which contains no organic catalyst, chemically reacts with H2O in the atmosphere by heating it at 450 °C for more than 1 h to turn it into a SiO2 film. If silica conversion can be achieved at temperatures below 100 °C, which plastics can withstand, it may be applicable to a wide range of applications, such as flexible electronics. Here, we report a technique for forming SiO2 films with leakage current characteristics very close to those of thermally oxidized (THOX) films that works at a very low temperature of 52 °C with high speed. Using a 9-kV, 30-kHz power supply, a low-temperature plasma jet containing a gas mixture of Ar and water vapor irradiated an 8 nm thick PHPS thin film, inducing silica conversion at a maximum substrate temperature of 52 °C. The current density-electric field strength (J-E) characteristics of metal oxide semiconductor capacitors fabricated with this SiO2 film showed characteristics very close to those of THOX films. In addition, the mechanism of silica conversion of PHPS through low-temperature plasma jet irradiation using this gas mixture was clarified in real-time FT-IR measurements.

Effects of Thickness and Anisotropic Strain on Polarization Switching Properties of Sub-10nm Epitaxial Hf0.5Zr0.5O2 Thin Films

Abstract Doped HfO2-based ferroelectric (FE) films are emerging as leading contenders for next-generation FE non-volatile memories due to their excellent compatibility with complementary metal oxide semiconductor processes and robust ferroelectricity at nanoscale dimensions. Despite the considerable attention paid to the FE properties of HfO2-based films in recent years, enhancing their polarization switching speed remains a critical research challenge. We demonstrate the strong ferroelectricity of sub-10 nm Hf0.5Zr0.5O2 (HZO) thin films and show that the polarization switching speed of these thin films can be significantly affected by HZO thickness and anisotropically strained La0.67Sr0.33MO3-buffered layer. Our observations indicate that the HZO thin film thickness and anisotropically strained La0.67Sr0.33MO3 layer influence the nucleation of reverse domains by altering the phase composition of the HZO thin film, thereby reducing the polarization switching time. Although the increase in HZO thickness and anisotropic compressive strain hinder the formation of the FE phase, they can enable faster switching. Our findings suggest that FE HZO ultrathin films with polar orthorhombic structures have broad application prospects in microelectronic devices. These insights into novel methods for increasing polarization switching speed are poised to advance the development of high-performance FE devices.

Fabrication of thin film for triple-cation perovskite via hot-bar-coating method without post-annealing process

The triple-cation perovskite Cs0.05(MA0.17FA0.83)0.95Pb(I0.83Br0.17)3 was deposited using the hot-bar-coating method. The effects of the substrate temperature and coating bar sweep speed on the film quality were investigated. Coating the precursor solution at a substrate temperature of 150 °C, reduced fabrication time by eliminating the post-annealing process, which is essential to conventional film fabrication methods, i.e., the antisolvent method. We further investigated the dependence of thin film thickness and quality on the coating bar sweep speed, finding that the optimal film quality was achieved at a speed of 4 mm/s. Importantly, decomposition into PbI2 was not observed during film fabrication for the triple-cation perovskite. The results of solar cell property measurements, indicating that the fabricated devices maintained high performance for 500 h in ambient air, suggest that the hot-bar-coating method is a promising approach for producing perovskite solar cells with high atmospheric stability and potentially low cost.

Ni/n-Si Schottky junction: Self-biased infrared photodetection via hot carrier photoemission

Internal photoemission-based hot electron generation at metal-semiconductor junctions holds significant potential for silicon-based sub-bandgap NIR photodetectors. In this work, we designed a simple nickel-silicon Schottky junction using the pulsed laser deposition technique and performed both experimental and theoretical analyses. To reduce the complexity of fabrication and lower costs, we used a planar nickel thin film on top of n-type silicon. The thickness of the nickel thin film was optimized to improve absorption and hot electron generation near the Ni/Si interface. We measured and calculated reflectance using the transfer matrix approach to quantify the effect of thickness on EQE. We also calculated the thickness-dependent absorption profile to estimate hot electron production near the junction. The current-voltage characterization of Ni/n-Si Schottky photodetector was investigated under the dark conditions as well under 1200 nm and 1300 nm light illumination. Under self-bias conditions, a photodiode with a 12 nm Ni thickness exhibits responsivity of 0.124 mA/W and 0.069 mA/W under illumination from 1200 nm and 1300 nm LED light, respectively. Furthermore, we used a comprehensive theoretical model to quantify the planar Ni/Si hot carrier generation and emission efficiency. and experimentally validated the calculated EQEs with the fabricated device. We believe the proposed complementary metal-oxide-semiconductor-compatible and simply structured Ni/Si Schottky photodetector will have potential applications in the silicon-based optoelectronics market.

Enhancing Charge Trapping Performance of Hafnia Thin Films Using Sequential Plasma Atomic Layer Deposition.

We aimed to fabricate reliable memory devices using HfO2, which is gaining attention as a charge-trapping layer material for next-generation NAND flash memory. To this end, a new atomic layer deposition process using sequential remote plasma (RP) and direct plasma (DP) was designed to create charge-trapping memory devices. Subsequently, the operational characteristics of the devices were analyzed based on the thickness ratio of thin films deposited using the sequential RP and DP processes. As the thickness of the initially RP-deposited thin film increased, the memory window and retention also increased, while the interface defect density and leakage current decreased. When the thickness of the RP-deposited thin film was 7 nm, a maximum memory window of 10.1 V was achieved at an operating voltage of ±10 V, and the interface trap density (Dit) reached a minimum value of 1.0 × 1012 eV-1cm-2. Once the RP-deposited thin film reaches a certain thickness, the ion bombardment effect from DP on the substrate is expected to decrease, improving the Si/SiO2/HfO2 interface and thereby enhancing device endurance and reliability. This study confirmed that the proposed sequential RP and DP deposition processes could resolve issues related to unstable interface layers, improve device performance, and enhance process throughput.

Variations of the elemental composition distribution over the thickness of YBa2Cu3O7-δ thin films obtained by pulsed laser deposition from one target

Epitaxial YBa2Cu3O7‒δ (YBCO) films 150–200 and 300 nm thick, respectively, were deposited on SrTiO3 (100) substrates by pulsed laser deposition at different conditions: with and without using the velocity filtration technique. The films have T(R = 0) in the range of 77.4–87 R(T) depending on the conditions of deposition from one target with YBa2Cu3O6.8 composition. The films contain Zn, Sr, Pd, Ag and Ti impurity elements obtained from the target (a total of no more than 2 at. %). Data of the film resistance temperature dependences, X-ray phase analysis, analysis of X-ray fluorescence (XRF) spectra and study of the surface relief by SEM methods revealed the nonuniform distributions of impurity and matrix Y, Ba, Cu elements over the film depth. Impurity concentrations near the surface lead to the formation of faceted spiral pyramids on the surface, which probably evolve into large elongated particles according to the Ostwald mechanism. This knowledge is practically important for optimizing pulsed laser deposition technologies and creating 2D instruments and devices for studying physical phenomena.

Effect of thin film thickness of ferrofluid on inclined bioconvective flow

This research examines the effect of variable thin film thickness on the bioconvective ferrofluid flow through a rotating sloped surface when a magnetic field (dipole) is present. Similarity transformation is used to standardize the current model's governing equations. By using a finite element method, the normalized nonlinear differential equations are numerically solved. Variable thickness of ferrofluid thin film and bioconvective parameters (bioconvective Lewis number, bioconvective Peclet number, and micro-organism concentration difference) yield the following results: velocity profiles (radial, tangential, and axial), gravity flow (drainage velocity and induced velocity), temperature profile, concentration profile and microorganism profile. In addition, this investigation examines the density of moving microorganisms as well as local heat and mass transport. The temperature, concentration, radial, axial, drainage, induced, and motile microbe velocity are all improved with increasing film thickness. Variable thickness increases local heat transfer whereas increasing Brownian motion and thermophoresis parameters decreases it. This study could be helpful for self-sterilizing applications and biomedical engineering.