In-situ study of the crystallization of amorphous CuInSe2 thin films and the effect of InCl3 treatment
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Materials Science↗
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Gallium phosphide optical metasurfaces for visible light applications
There are few materials that are broadly used for fabricating optical metasurfaces for visible light applications. Gallium phosphide (GaP) is a material that, due to its optical properties, has the potential to become a primary choice but due to the difficulties in fabrication, GaP thin films deposited on transparent substrates have never been exploited. In this article we report the design, fabrication, and characterization of three different amorphous GaP metasurfaces obtained through sputtering. Although the material properties can be further optimized, our results show the potential of this material for visible applications making it a viable alternative in the material selection for optical metasurfaces.
36 MATERIALS SCIENCE↗
Amorphous 2D Materials – A Novel Platform for Remote Epitaxy and Nanopatterned Epitaxy of III-V Semiconductors with Low Decomposition Temperatures
III-V semiconductor materials such as indium phosphide (InP) offer outstanding photonic properties that outperforms silicon, but the cost of these wafers is extremely expensive. Although reusing original wafers can effectively minimize the cost, current techniques for wafer recycling of these substrates add significant costs in fabrication, nullifying the cost savings by reusing the wafers. Besides, unlike other III-V materials such as gallium arsenide (GaAs), commonly used epitaxial lift-off method for wafer recycling is not well studied for materials like InP due to lack of lattice-matched sacrificial layers, which makes reusing these wafers more difficult. Remote epitaxy and nanopatterned epitaxy are newly discovered methods that enable single-crystal growth of III-V semiconductor thin films and easy exfoliation of these grown films, thus promising for a new cost-effective pathway of reusing wafers. However, previous methods of transferring two-dimensional (2D) materials, which use polymethyl methacrylate (PMMA) or metal stressor layers to transfer 2D materials grown on foreign substrates like copper (Cu) or silicon carbide (SiC), introduce defects and damages on the 2D layer and/or substrates during the transfer process. Remote epitaxial and nanopatterned epitaxial films grown on the damaged 2D layer/substrate suffer from lower crystal quality and imperfect exfoliation, which undermines wafer reusability and device performance. Here we report the MBE growth of amorphous boron nitride (a-BN) on InP wafers at low temperature that enabled improved quality of remote epitaxial and nanopatterned epitaxial films and their perfect exfoliation. We show fully covered a-BN on InP substrates despite their low decomposition temperatures. The surface of a-BN coated InP substrate remains smooth with a RMS roughness of around 3Â. We also demonstrate 100% coverage of single-crystal InP thin films grown on a-BN, with the film's quality significantly improved compared to the case of transferred 2D materials. In addition, the growth and exfoliation were successfully repeated multiple times, proving the feasibility for InP wafer recycling. Through this low temperature MBE growth approach with remote epitaxy and nanopatterned epitaxy, we successfully demonstrate large-scale flexible thin film exfoliation and recycling of InP substrates, which will lead to new opportunities in InP thin film-based photonics and novel heterostructures with significantly reduced cost.
Lu, Kuangye↗
Amorphous 2D Materials – A Novel Platform for Remote Epitaxy and Nanopatterned Epitaxy of III-V Semiconductors with Low Decomposition Temperatures
III-V semiconductor materials such as indium phosphide (InP) offer outstanding photonic properties that outperforms silicon, but the cost of these wafers is extremely expensive. Although reusing original wafers can effectively minimize the cost, current techniques for wafer recycling of these substrates add significant costs in fabrication, nullifying the cost savings by reusing the wafers. Besides, unlike other III-V materials such as gallium arsenide (GaAs), commonly used epitaxial lift-off method for wafer recycling is not well studied for materials like InP due to lack of lattice-matched sacrificial layers, which makes reusing these wafers more difficult. Remote epitaxy and nanopatterned epitaxy are newly discovered methods that enable single-crystal growth of III-V semiconductor thin films and easy exfoliation of these grown films, thus promising for a new cost-effective pathway of reusing wafers. However, previous methods of transferring two-dimensional (2D) materials, which use polymethyl methacrylate (PMMA) or metal stressor layers to transfer 2D materials grown on foreign substrates like copper (Cu) or silicon carbide (SiC), introduce defects and damages on the 2D layer and/or substrates during the transfer process. Remote epitaxial and nanopatterned epitaxial films grown on the damaged 2D layer/substrate suffer from lower crystal quality and imperfect exfoliation, which undermines wafer reusability and device performance. Here we report the MBE growth of amorphous boron nitride (a-BN) on InP wafers at low temperature that enabled improved quality of remote epitaxial and nanopatterned epitaxial films and their perfect exfoliation. We show fully covered a-BN on InP substrates despite their low decomposition temperatures. The surface of a-BN coated InP substrate remains smooth with a RMS roughness of around 3Å. We also demonstrate 100% coverage of single-crystal InP thin films grown on a-BN, with the film's quality significantly improved compared to the case of transferred 2D materials. In addition, the growth and exfoliation were successfully repeated multiple times, proving the feasibility for InP wafer recycling. Through this low temperature MBE growth approach with remote epitaxy and nanopatterned epitaxy, we successfully demonstrate large-scale flexible thin film exfoliation and recycling of InP substrates, which will lead to new opportunities in InP thin film-based photonics and novel heterostructures with significantly reduced cost.
Lu, Kuangye↗
The PCM is Dead! Long Live O-PCM!
The ability to reconfigure the optical behavior of a device enables free-space applications ranging from imaging to sensing and signal control. Such optical devices can be compacted via meta-surfaces, patterned structures with feature sizes below the incident wavelength. Leveraging geometry in addition to material properties and CMOS fabrication techniques has allowed meta-surfaces for lenses, holograms, beam steerers and more. To incorporate multiple optical functions into one device, various methods of device control have been implemented, such as stretching of flexible substrates, tuning the refractive index of the comprising meta-atoms via the electro-optic or the thermo-optic effects, phase transition materials such as VO2 and more. Chalcogenide glasses used as optical phase change materials, such as Ge¬2Sb2Te5 (GST), have gained increased traction in the optics community for potential use in the near infrared (NIR) and mid infrared (MIR) bands, including the telecom bands. Various chalcogenides such as Sb2Se3, Sb2S3, Ge2Sb¬2Se5 and Ge2Sb2Se4Te (GSST) have been investigated due to their broad NIR or MIR transparency window and large changes in refractive index. In their amorphous phase, these materials usually display a lower refractive index and low absorption when compared to their crystalline state which display a higher refractive index and typically larger extinction coefficients. The amorphous-crystalline reversible switching can be done via fast melt-quenching thermal processes triggered by laser or electrical impulses, relying on a substrate as a heat sink. The potential of PCMs in photonic devices can be limited by intrinsic material limitations as well as by device fabrication issues. To explore the cyclability of GSST, a PCM with large refractive index contrast and on-chip electrothermal switching on a silicon-on-insulator platform has been done to analyze potential failure mechanisms from both a material and device perspective. A brief outline of the instrumentation and phase change contrast analysis is provided. Dewetting of the PCM, delamination of and damage in the PECVD SiNx protective layer, elemental migration in the PCM and optical contrast decay have been observed in cycled GSST devices. Guidelines for device performance improvement are proposed, and an improved design with larger endurance is shown in progress.
reconfigurable photonics↗
Investigation of phase-change coatings for variable thermal control of spacecraft
An investigation was conducted to determine the feasibility of producing a spacecraft coating system that could vary the ratio of its solar absorptance to thermal emittance to adjust automatically for changes in the thermal balance of a spacecraft. This study resulted in a new concept called the phase-change effect which uses the change that occurs in the optical properties of many materials during the phase transition from a crystalline solid to an amorphous material. A series of two-component model coatings was developed which, when placed on a highly reflecting substrate, exhibited a sharp decrease in solar absorptance within a narrow temperature range. A variable thermal control coating can have a significant amount of temperature regulation with the phase-change effect. Data are presented on several crystallite-polymer formulations, their physical and optical properties, and associated phase-change temperatures. Aspects pertaining to their use in a space environment and an example of the degree of thermal regulation attainable with these coatings is also given.
Kelliher, W. C.↗
Irradiation-induced amorphization of UO 2 films prepared by spraying-assisted combustion synthesis
Spraying-assisted combustion synthesis with uranyl nitrate – acetylacetone – 2-methoxyethanol solutions was used to prepare UO 2 films on an aluminum alloy substrate. The tuning of the spraying parameters and annealing temperatures allowed the preparation of UO 2 films with thicknesses varying from 10–300 nm and 5–10 nm UO 2 grain size. High-resolution electron microscopy and X-ray photoelectron spectroscopy showed that increasing the annealing temperature promotes Mg diffusion from the substrate into the films. The incorporation of Mg reduced the overall crystallinity of the films. The irradiation with Ar 2+ ions (1.7 MeV energy and a fluence of 2 × 10 16 ions/cm 2 ) did not degrade the quality of the films. However, the Mg content significantly influenced the irradiation-induced restructuring of the UO 2 films. Irradiated films with low or no Mg content exhibit high crystallinity, and the UO 2 /Al interfacial layer becomes highly porous. Films with higher Mg content are mostly amorphized after irradiation. The origin of irradiation-induced amorphization was related to the formation of Mg y U 1-y O 2±x solid solutions. Chemically complex, pore-free, and amorphous Mg-Al-O film/substrate interfacial layers enable continuous Mg diffusion during irradiation. As a result, the gradual increase in Mg amounts triggers irradiation-induced precipitation of a crystalline MgO-rich phase within the amorphous films.
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
Proton diffusion and hydrogen/deuterium exchange in amorphous solid water at temperatures from 114 to 134 K
The reaction coefficient for hydrogen/deuterium (H/D) exchange and the diffusion of hydrated excess protons within amorphous solid water (ASW) are characterized as a function of temperature. For these experiments, water films are deposited on a Pt(111) substrate at 108 K, and reactions with pre-adsorbed hydrogen atoms produce hydrated protons. Upon heating, protons diffuse within the water, and H/D exchange occurs when they encounter D2O probe molecules deposited in the films. The time-dependent concentration of D2O is monitored with infrared spectroscopy, and it indicates the protons diffusion from the substrate and establish an equilibrium distribution prior to significant H/D exchange for temperatures 114 K ≤T≤ 134 K. By controlling the distance between the D2O molecules and the substrate, we probe the distribution of protons within the film. It decays as x−2 for the examined range of x (12–52 nm) due to the electric field that develops between the diffusing protons and their image charges in the metal substrate. This agrees with the theoretical distance scaling for the equilibrated proton concentration in a dielectric near a metal boundary. From the proton concentration and the measured D2O decay rate, a lower bound for the proton diffusion coefficient ranging from 10−20 m2/s at 114 K to 10−18 m2/s at 134 K is estimated. The diffusion coefficient has an activation energy of 0.40 eV, which is comparable to energies reported for molecular translations and rotations of H2O, suggesting they may play a critical role in the proton diffusion mechanism within ASW.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Elastic Properties of Films of Water and Noble Gases Condensed at Low Temperatures
We have shown that there are extensive similarities between the quench-condensed noble gas films and those of amorphous water ice. In particular, both can be quite soft upon deposition and can stiffen considerably when annealed. Furthermore, this stiffening follows a logarithmic time dependence for all substances. The temperature dependence of these behaviors scales with the triple point. The results shown here show a strong thickness dependence, which has implications for any study of mechanical properties of films on substrates. The temperature dependence of the stiffening and the stiffening rate have now been characterized for the noble gases, and these observations provide a roadmap for new experiments on amorphous water ice.
Pohl, Robert O.↗
Morphology of Vapor-Deposited Acetonitrile Films
Crystalline acetonitrile has two polymorphs, a high temperature (HT) phase that is stable between 217 K and its melting point at 229 K, and a low temperature (LT) phase that is stable below 217 K. Solid acetonitrile films can be prepared by vapor deposition in an ultra-high vacuum chamber. To prevent sublimation of the film temperatures are often kept below 150 K. While the LT phase is thermodynamically favored at these low temperatures, such preparation usually results in the formation of the metastable HT polymorph. In this work we use reflection adsorption infrared spectroscopy (RAIRS) and temperature programmed desorption (TPD) experiments to investigate the effects of the deposition temperature and underlying substrate on the morphology of acetonitrile films prepared with molecular beam deposition. We obtained the elusive LT phase when dosing at 120 K on a graphene substrate and on a crystalline decane layer. Dosing acetonitrile on other surfaces produced the HT phase, as did annealing of amorphous films. We used TPD experiments to determine the Gibbs energy difference between the HT and LT phases. Our ΔG values agree with extrapolation of equilibrium calorimetry data. Furthermore, we also observed that acetonitrile films were amorphous when dosed at temperatures ≤ 60 K, and porous for temperatures ≤ 50 K.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Morphological growth of sputtered MoS2 films
Sputtered MoS2 films from 300 A to 20,000 A thick were deposited on metal and glass surfaces. The substrate effects such as surface temperature, finish, pretreatment and chemistry as they affect the film formation characteristics were investigated by optical, electron transmission, electron diffraction, and scanning electron microscopy. Substrate temperature and surface chemistry were found to be the prime variables as to the formation of a crystalline or amorphous film. The friction characteristics are strictly influenced by the type of film formed. Surface chemistry and surface pretreatment account for compound formation and corresponding grain growth, which directly affect the adhesion characteristics, resulting in poor adherence. The type of surface finish (topography) as related to scratches, impurities, inhomogeneities, etc., are favorable nucleation sites for the growth of isolated and complex nodules within the film, and various complex surface overgrowths on the film. These nodular growth features have progressively more undesirable effects on the film behavior as the film thickness increases.
Spalvins, T.↗
Morphological growth of sputtered MoS2 films
Sputtered MoS2 films from 300 A to 20,000 A thick were deposited on metal and glass surfaces. The substrate effects such as surface temperature, finish, pretreatment, and chemistry as they affect the film formation characteristics were investigated by optical, electron transmission, electron diffraction, and scanning electron microscopy. Substrate temperature and surface chemistry were found to be the prime variables as to the formation of a crystalline or amorphous film. The friction characteristics are strictly influenced by the type of film formed. Surface chemistry and surface pretreatment account for compound formation and corresponding grain growth, which directly affect the adhesion characteristics, resulting in poor adherence. Scratches, impurities, inhomogeneities, etc., are favorable nucleation sites for the growth of isolated and complex nodules within the film.
Spalvins, T.↗
Wafer-Scale Synthesis of 2D Materials by an Amorphous Phase-Mediated Crystallization Approach
The interest in the wafer-scale growth of two-dimensional (2D) materials, including transition metal dichalcogenides (TMDCs), has been rising for transitioning from lab-scale devices to commercial-scale systems. Among various synthesis techniques, physical vapor deposition, such as pulsed laser deposition (PLD), has shown promise for the wafer-scale growth of 2D materials. However, due to the high volatility of chalcogen atoms (e.g., S and Se), films deposited by PLD usually suffer from a lack of stoichiometry and chalcogen deficiency. To mitigate this issue, excess chalcogen is necessary during the deposition, which results in problems like uniformity or not being repeatable. This study demonstrates a condensed-phase or amorphous phase-mediated crystallization (APMC) approach for the wafer-scale synthesis of 2D materials. This method uses a room-temperature PLD process for the deposition and formation of amorphous precursors with controlled thicknesses, followed by a post-deposition crystallization process to convert the amorphous materials to crystalline structures. This approach maintains the stoichiometry of the deposited materials throughout the deposition and crystallization process and enables the large-scale synthesis of crystalline 2D materials (e.g., MoS 2 and WSe 2 ) on Si/SiO 2 substrates, which is critical for future wafer-scale electronics. We show that the thickness of the layers can be digitally controlled by the number of laser pulses during the PLD phase. Optical spectroscopy is used to monitor the crystallization dynamics of amorphous layers as a function of annealing temperature. The crystalline quality, domain sizes, and the number of layers were explored using nanoscale and atomistic characterization (e.g., AFM, STEM, and EDS) along with electrical characterization to explore process–structure–performance relationships. Finally, this growth technique is a promising method that could potentially be adopted in conventional semiconductor industries for wafer-scale manufacturing of next-generation electronic and optoelectronic devices.
2D electronics↗
Estimating viscosity of individual substrate-deposited particles from measurements of their height-to-width ratios
Airborne particles alter the radiative forcing of climate and have further consequences on air visibility, atmospheric chemistry, and human health. Recent studies reported the existence of highly viscous semisolid and even solid amorphous organic aerosol (OA) particles. Particle viscosity has an impact on the heterogeneous chemistry, gas-particle partitioning, and ice nucleation properties. Consequently, variations in particle viscosity must be considered when predicting the atmospheric impact of OA. Here, in this work, we use scanning electron microscopy (SEM) and scanning transmission X-ray microscopy (STXM) to estimate the viscosity of individual particles deposited on substrates based on their characteristic height-to-width ratios, which are affected by changes in morphology upon deposition. The height-to-width ratios obtained from SEM and STXM exhibit a strong correlation, demonstrating that both imaging approaches can be applied separately for viscosity assessment of the substrate-deposited particles. While these metrics are largely qualitative, this method enables rapid assessment of particle viscosity ranges, distinguishing between semisolid (>10 10 Pa·s), viscous (10 4– 10 8 Pa·s), and liquid (10°–10 1 Pa·s) particles within ensembles of ambient particles collected for microscopy studies.
54 ENVIRONMENTAL SCIENCES↗
Improving stability of ALD ZrN thin film coatings over U-Mo dispersion fuel
Atomic layer deposition (ALD) of ZrN is a candidate technology for coating U-Mo dispersion fuel as a diffusion barrier coating. During the early development stages of the coating the ZrN deposition showed to be mechanically unstable and ultimately resulted in spalling. Based on experimental outcomes it was found that instabillity can be eliminated through the introduction of a thin amorphous (a) Al 2 O 3 interlayer coating deposited in between the ~1-μm thick ZrN and the U-Mo. substrate. To elucidate these findings simulations were performed with density functional theory (DFT) to measure work of adhesions at different interfaces while finite element modeling (FEM) was performed to measure the residual stress distribution. DFT indicated that the ZrN coating deposited over (a)-Al 2 O 3 is ~2.5 times stronger when compared to direct deposition over U or UO 2 substrate. While calculations from FEM recognized; (1) large stress concentrations can originate from the irregularly distributed native surface oxides (UO 2 ) over U-Mo and (2) stress concentrations can be reduced if those surface UO 2 can be modified to a uniform layer (achieved after application of a 8 nm (a)-Al 2 O 3 interlayer). These results provided explanations and confirmed the role played by interlayer in eliminating the original mechanical instability of the ZrN.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Metallic glass as a temperature sensor during ion plating
The temperature of the interface and/or a superficial layer of a substrate during ion plating was investigated using a metallic glass of the composition Fe67Co18B14Si1 as the substrate and as the temperature sensor. Transmission electron microscopy and diffraction studies determined the microstructure of the ion-plated gold film and the substrate. Results indicate that crystallization occurs not only in the film, but also in the substrate. The grain size of crystals formed during ion plating was 6 to 60 nm in the gold film and 8 to 100 nm in the substrate at a depth of 10 to 15 micrometers from the ion-plated interface. The temperature rise of the substrate during ion plating was approximately 500 C. Discontinuous changes in metallurgical microstructure, and physical, chemical, and mechanical properties during the amorphous to crystalline transition in metallic glasses make metallic glasses extremely useful materials for temperature sensor applications in coating processes.
Miyoshi, K.↗
Metallic glass as a temperature sensor during ion plating
The temperature of the interface and/or a superficial layer of a substrate during ion plating was investigated using a metallic glass of the composition Fe67Co18B14Si1 as the substrate and as the temperature sensor. Transmission electron microscopy and diffraction studies determined the microstructure of the ion-plated gold film and the substrate. Results indicate that crystallization occurs not only in the film, but also in the substrate. The grain size of crystals formed during ion plating was 6 to 60 nm in the gold film and 8 to 100 nm in the substrate at a depth of 10 to 15 micrometers from the ion-plated interface. The temperature rise of the substrate during ion plating was approximately 500 C. Discontinuous changes in metallurgical microstructure, and physical, chemical, and mechanical properties during the amorphous to crystalline transition in metallic glasses make metallic glasses extremely useful materials for temperature sensor applications in coating processes.
Miyoshi, K.↗
Plasma sprayed mullite coatings on silicon-base ceramics
A silicon-base ceramic substrate is provided with a mullite chemical barrier/thermal barrier coating uniformly bonded to a surface. The coating is substantially free of amorphous mullite.
Lee, Kang N.↗