Quantum-Enabled Nondestructive Optical Microscopy (QENOM)
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quantum enabled microscopy, two photon fluorescenc↗
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Equation of State Measurements of Materials Using Optical Microscopy and Interferometry
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Materials science↗
Correlated Materials Characterization via Multimodal Chemical and Functional Imaging
Multimodal chemical imaging simultaneously offers high-resolution chemical and physical information with nanoscale and, in select cases, atomic resolution. By coupling modalities that collect physical and chemical information, we can address scientific problems in biological systems, battery and fuel cell research, catalysis, pharmaceuticals, photovoltaics, medicine, and many others. The combined systems enable the local correlation of material properties with chemical makeup, making fundamental questions of how chemistry and structure drive functionality approachable. In this Review, we present recent progress and offer a perspective for chemical imaging used to characterize a variety of samples by a number of platforms. Specifically, we present cases of infrared and Raman spectroscopies combined with scanning probe microscopy; optical microscopy and mass spectrometry; nonlinear optical microscopy; and, finally, ion, electron, and probe microscopies with mass spectrometry. As a result, we also discuss the challenges associated with the use of data originated by the combinatorial hardware, analysis, and machine learning as well as processing tools necessary for the interpretation of multidimensional data acquired from multimodal studies.
36 MATERIALS SCIENCE↗
Thermally initiated disproportionation of manganese(II) bis(1-hydroxyethylidene)diphosphonate. Formation and properties of the lepidoid structure of manganese(II) (1-hydroxyethylidene)diphosphonate-2-hydroxyethaneaminium whiskers. Agronomical efficiency of the manganese(II) complex with (1-hydroxyethylidene)diphosphonic acid
The reaction of poorly soluble manganese(II) bis(1-hydroxyethylidene)diphosphonate tetrahydrate (Mn(H{sub 3}L){sub 2}•4H{sub 2}O) with 2-aminoethanol (H{sub 2}NCH{sub 2}CH{sub 2}OH) in an aqueous medium on heating to 70—80 оС causes the initial formation of soluble manganese(II) bis(1-hydroxyethylidene)diphosphonate tris(1-hydroxyethaneaminium) (Mn(H{sub 3}L)2• •3H{sub 2}NCH{sub 2}CH{sub 2}OH•4H{sub 2}O), which then disproportionates to slightly soluble manganese(II) (1-hydroxyethylidene)diphosphonate-2-hydroxyethaneaminium (MnH{sub 2}L•H{sub 2}NCH{sub 2}CH{sub 2}OH) and coordination polymer of 1-hydroxyethylidenediphosphonic acid with 2-aminoethanol containing no metal cations. In the course of the reaction, MnH{sub 2}L•H{sub 2}NCH{sub 2}CH{sub 2}OH precipitates as whiskers that are grouped into a leaf (lepidoid) structure. The latter was examined by IR spectroscopy, X-ray phase analysis, scanning electron microscopy, atomic force microscopy, optical microscopy, and thermal desorption of nitrogen. The starting and resulting manganese compounds refer to poorly soluble crystalline complexes. The presence of a 2-aminoethanol molecule in the final product leads to an increase in the solubility from 0.40 to 0.54 g in 100 mL of the solution. Poorly soluble MnH{sub 2}L•H{sub 2}NCH{sub 2}CH{sub 2}OH is easily converted to a soluble form by the treatment with 2-aminoethanol or 2-amino-2-(hydroxy- methyl)propane-1,3-diol (H{sub 2}NC(CH{sub 2}OH)3). The agronomical efficiency of a solution of the Mn(H{sub 3}L){sub 2}•3H{sub 2}NCH{sub 2}CH{sub 2}OH•4H{sub 2}O complex was studied on the cultures of white lupine Degas, spring wheat Ester, spring rape, and pea Stabil.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Isomorphism and solid solutions among Ag- and Au-selenides
Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag{sub 2−x}Au{sub x}Se with a step of x=0.25 (0≤x≤2) to 1050 °C and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag{sub 2}Se – Ag{sub 1.94}Au{sub 0.06}Se, fischesserite Ag{sub 3}AuSe{sub 2} - Ag{sub 3.2}Au{sub 0.8}Se{sub 2} and gold selenide AuSe - Au{sub 0.94}Ag{sub 0.06}Se. Solid solutions and AgAuSe phases were added to the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe. - Highlights: • Au-Ag selenides were synthesized. • Limited Ag-Au isomorphism in the selenides is affected by structural features. • Some new phases were introduced to the phase diagram Ag-Au-Se.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Plastic deformation and material transfer on steel gage blocks during low force mechanical probing
Contact probing of gaging surfaces is enabled throughout dimensional metrology. Probe tips such as ruby, sapphire, or diamond are commonly employed as styli for universal length measuring machines (ULMs) and coordinate measuring machines (CMMs) due to the hardness, durability, and wear resistance. Gaging surfaces of gage blocks are precision ground or lapped, with very low surface roughness to enable wringing. Damage or contamination of these surfaces can prevent wringing and lead to measurement error. Experimental investigations using a horizontal ULM and CMM have revealed that even at low force settings (≤0.16 N), probe materials such as ruby and sapphire can cause plastic deformation to hardened carbon chrome steel (such as AISI 52,100) gage block surfaces at the microscale, likely attributed to fretting-associated wear. Under some conditions, permanent transfer of material from the probe stylus to the gaging surface is possible. Results show irreversible changes and damage to gaging surfaces with repeated probe contact on a ULM and CMM. Optical microscopy, optical profilometry, and scanning electron microscopy (SEM) provide a semi-quantitative assessment of microscale plastic deformation and material transfer. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and Raman techniques validate chemical constituency of reference materials used (gage blocks and probes) and also identify makeup of deposits on gaging surfaces following probe contact.
42 ENGINEERING↗
Degradation of Spacesuit Fabrics in Low Earth Orbit
Six samples of pristine and dust-abraded outer layer spacesuit fabrics were included in the Materials International Space Station Experiment-7, in which they were exposed to the wake-side low Earth orbit environment on the International Space Station (ISS) for 18 months in order to determine whether abrasion by lunar dust increases radiation degradation. The fabric samples were characterized using optical microscopy, optical spectroscopy, field emission scanning electron microscopy, atomic force microscopy, and tensile testing before and after exposure on the ISS. Comparison of pre- and post-flight characterizations showed that the environment darkened and reddened all six fabrics, increasing their integrated solar absorptance by 7 to 38 percent. There was a decrease in the ultimate tensile strength and elongation to failure of lunar dust abraded Apollo spacesuit fibers by a factor of four and an increase in the elastic modulus by a factor of two.
Gaier, James R.↗
Structural and Mechanical Properties of Zr-Si-N Coatings Deposited by Arc Evaporation at Different Substrate Bias Voltages
ZrN and Zr-Si-N coatings were formed using vacuum-arc plasma fluxes deposition system at the substrate bias voltage (U{sub B}) ranged from − 50 to − 220 V on HS6-5-2 steel substrates. The structural, mechanical and tribological properties were characterized using x-ray diffraction, atomic force microscopy, scanning electron microscopy, optical microscopy, nanoindentation and ball-on-disk test. The surface roughness parameter Ra of ZrN coatings is lower than Zr-Si-N coatings. Both roughness Ra of Zr-Si-N coatings and the number of surface defects with mainly small dimensions to 1 µm decrease with increasing negative substrate bias voltage. The addition of silicon to ZrN significantly reduces the crystallite size, from about 18.3 nm for ZrN coating to 6.4 nm for Zr-Si-N coating both deposited at the same U{sub B} = − 100 V and 7.8 nm for U{sub B} = − 150 V. The hardness of Zr-Si-N coatings increases to about 30 GPa with the increase in negative substrate bias voltage (U{sub B} = − 220 V). Adhesion of the coatings tested is high, and critical load is above 80 N and reduces with U{sub B} increase. Coefficient of friction determined using AFM shows similar trend as surface roughness in microscale.
36 MATERIALS SCIENCE↗
Diffusion and impurity segregation in hydrogen-implanted silicon carbide
Diffusion and segregation behavior of hydrogen and oxygen in silicon carbide subjected to H implantation and subsequent annealing were studied with a number of analytical techniques including Secondary Ion Mass Spectrometry (SIMS), Rutherford backscattering spectrometry in channeling geometry, field emission scanning electron microscopy, optical microscopy, cross-sectional transmission electron microscopy, and atomic force microscopy. H{sup +} implantation was carried out with energies of 200 keV, 500 keV, or 1 MeV to doses of 1 × 10{sup 16}, 1 × 10{sup 17}, or 2 × 10{sup 17} ion/cm{sup 2}, and thermal treatment was conducted in flowing argon for 1 to 2 h at temperatures of 740, 780, 1000, or 1100 °C. The process of migration and eventual loss of hydrogen in a point defect regime is postulated to proceed to a large extent through ionized vacancies. This conclusion was derived from the observed substantial difference in H mobilities in n- vs. p-type SiC as the population of ionized vacancies is governed by the Fermi-Dirac statistics, i.e., the position of the Fermi level. For higher doses, a well defined buried planar zone forms in SiC at the maximum of deposited energy, comprising numerous microvoids and platelets that are trapping sites for hydrogen atoms. At a certain temperature, a more or less complete exfoliation of the implanted layer is observed. For a 1 MeV implant heated to 1100 °C in nominally pure argon, SIMS profiling reveals a considerable oxygen peak of 10{sup 16} O atoms/cm{sup 2} situated at a depth close to that of the peak of the implanted H{sup +}. Similarly, 1100 °C annealing of a 200 keV implant induces the formation of a thin oxide (4 nm), located at the interface between the implanted layer and the substrate as evidenced by both SIMS and HRTEM. The measurements were taken on the part of the sample that remained un-exfoliated. In view of a lack of convincing evidence that a hexagonal SiC might contain substantial amounts of oxygen, further investigation is under way to elucidate its presence in the irradiation-damaged films.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Exploring leakage in dielectric films via automated experiments in scanning probe microscopy
Here electronic conduction pathways in dielectric thin films are explored using automated experiments in scanning probe microscopy (SPM). In this study, we use large field of view scanning to identify the position of localized conductive spots and develop an SPM workflow to probe their dynamic behavior at higher spatial resolution as a function of time, voltage, and scanning process in an automated fashion. Using this approach, we observe the variable behaviors of the conductive spots in a 20-nm-thick ferroelectric Hf 0.54 Zr 0.48 O 2 film, where conductive spots disappear and reappear during continuous scanning. There are also fresh conductive spots that develop during scanning. The automated workflow is universal and can be integrated into a wide range of microscopy techniques, including SPM, electron microscopy, optical microscopy, and chemical imaging.
36 MATERIALS SCIENCE↗
The Effect of Adsorbed Volatile Organic Compounds on an Ultrathin Water Film Measurement
Using surface plasmon resonance imaging (SPRi), we have recently shown for the first time the existence of a monolayer water film between droplets during dropwise condensation. This study examines the effect of adsorbed volatile organic compounds (VOCs) on the ultrathin film measurement using SPRi. Further, the work presents the proper surface-treatment process that enables measurements of the ultrathin water layer during high-speed imaging of dropwise condensation at 3000 frame per second. In this study, two methods were applied for cleaning the surface (gold-coated glass)—(1) standard cleaning procedure (SCP) using acetone, isopropyl alcohol, and deionized water and (2) SCP followed by air plasma cleaning. This work discusses the effect of the cleaning procedures on surface roughness, contact angle, and surface chemistry using atomic force microscopy, optical microscopy, and an X-ray photoelectron spectroscope meter. The results showed that SCP before the SPRi is a proper surface-treatment method. The effect of adsorbed VOCs during dropwise condensation on a surface treated with SCP was measured to be 0.0025 (reflectivity unit), which was 70% smaller than the reflectance associated with a monolayer water film. The results of this work confirm a monolayer water film observation during the dropwise condensation, which has been reported before.
36 MATERIALS SCIENCE↗
Array of Graphene Variable Capacitors on 100 mm Silicon Wafers for Vibration-Based Applications
Highly flexible, electrically conductive freestanding graphene membranes hold great promise for vibration-based applications. This study focuses on their integration into mainstream semiconductor manufacturing methods. We designed a two-mask lithography process that creates an array of freestanding graphene-based variable capacitors on 100 mm silicon wafers. The first mask forms long trenches terminated by square wells featuring cone-shaped tips at their centers. The second mask fabricates metal traces from each tip to its contact pad along the trench and a second contact pad opposite the square well. A graphene membrane is then suspended over the square well to form a variable capacitor. The same capacitor structures were also built on 5 mm by 5 mm bare dies containing an integrated circuit underneath. We used atomic force microscopy, optical microscopy, and capacitance measurements in time to characterize the samples.
36 MATERIALS SCIENCE↗
Stress corrosion in titanium alloys and other metallic materials
Multiple physical and chemical techniques including mass spectroscopy, atomic absorption spectroscopy, gas chromatography, electron microscopy, optical microscopy, electronic spectroscopy for chemical analysis (ESCA), infrared spectroscopy, nuclear magnetic resonance (NMR), X-ray analysis, conductivity, and isotopic labeling were used in investigating the atomic interactions between organic environments and titanium and titanium oxide surfaces. Key anhydrous environments studied included alcohols, which contain hydrogen; carbon tetrachloride, which does not contain hydrogen; and mixtures of alcohols and halocarbons. Effects of dissolved salts in alcohols were also studied. This program emphasized experiments designed to delineate the conditions necessary rather than sufficient for initiation processes and for propagation processes in Ti SCC.
Harkins, C. G.↗
Chemical vapor deposition growth
A chemical vapor deposition (CVD) reactor system with a vertical deposition chamber was used for the growth of Si films on glass, glass-ceramic, and polycrystalline ceramic substrates. Silicon vapor was produced by pyrolysis of SiH4 in a H2 or He carrier gas. Preliminary deposition experiments with two of the available glasses were not encouraging. Moderately encouraging results, however, were obtained with fired polycrystalline alumina substrates, which were used for Si deposition at temperatures above 1,000 C. The surfaces of both the substrates and the films were characterized by X-ray diffraction, reflection electron diffraction, scanning electron microscopy optical microscopy, and surface profilometric techniques. Several experiments were conducted to establish baseline performance data for the reactor system, including temperature distributions on the sample pedestal, effects of carrier gas flow rate on temperature and film thickness, and Si film growth rate as a function of temperature.
Ruth, R. P.↗
The evaluation of the interfacial behavior of LaRC-TPI/Graphite Composites
Discussed are the results of several approaches recently considered for improving the interfacial adhesion of LaRC-TPI/graphite composites. Two approaches were investigated, namely altering the matrix and altering the fiber. As a result, three types of LaRC-TPI laminates were produced: amorphous/AS-4, amorphous/XAS, and semicrystalline/AS-4. The laminates were characterized using the transverse tensile test, scanning electron microscopy, optical microscopy, and thermal analysis.
Ogden, A. L.↗
Scanning Tunneling Optical Resonance Microscopy
Scanning tunneling optical resonance microscopy (STORM) is a method, now undergoing development, for measuring optoelectronic properties of materials and devices on the nanoscale by means of a combination of (1) traditional scanning tunneling microscopy (STM) with (2) tunable laser spectroscopy. In STORM, an STM tip probing a semiconductor is illuminated with modulated light at a wavelength in the visible-to-near-infrared range and the resulting photoenhancement of the tunneling current is measured as a function of the illuminating wavelength. The photoenhancement of tunneling current occurs when the laser photon energy is sufficient to excite charge carriers into the conduction band of the semiconductor. Figure 1 schematically depicts a proposed STORM apparatus. The light for illuminating the semiconductor specimen at the STM would be generated by a ring laser that would be tunable across the wavelength range of interest. The laser beam would be chopped by an achromatic liquid-crystal modulator. A polarization-maintaining optical fiber would couple the light to the tip/sample junction of a commercial STM. An STM can be operated in one of two modes: constant height or constant current. A STORM apparatus would be operated in the constant-current mode, in which the height of the tip relative to the specimen would be varied in order to keep the tunneling current constant. In this mode, a feedback control circuit adjusts the voltage applied to a piezoelectric actuator in the STM that adjusts the height of the STM tip to keep the tunneling current constant. The exponential relationship between the tunneling current and tip-to-sample distance makes it relatively easy to implement this mode of operation. The choice of method by which the photoenhanced portion of the tunneling current would be measured depends on choice of the frequency at which the input illumination would be modulated (chopped). If the frequency of modulation were low enough (typically < 10 Hz) that the feedback circuit could respond, then the voltage applied to the piezoelectric tip-height actuator could be measured by use of a lock-in amplifier locked to the modulation (chopping) signal. However, at a high modulation frequency (typically in the kilohertz range or higher), the feedback circuit would be unable to respond. In this case, the photoenhanced portion of the tunneling current could be measured directly. For this purpose, the tunneling current would be passed through a precise resistor and the voltage drop would be measured by use of the lock-in amplifier.
Bailey, Sheila↗
Quantum Enhanced Probes of Magnetic Circular Dichroism
Magneto-optical microscopies, including optical measurements of magnetic circular dichroism, are increasingly ubiquitous tools for probing spin-orbit coupling, charge-carrier g-factors, and chiral excitations in matter, but the minimum detectable signal in classical magnetic circular dichroism measurements is fundamentally limited by the shot-noise limit of the optical readout field. Here, a two-mode squeezed light source is used to improve the minimum detectable signal in magnetic circular dichroism measurements by 3 decibels compared with state-of-the-art classical measurements, even with relatively lossy samples like terbium gallium garnet. Furthermore, these results provide a framework for new quantum-enhanced magneto-optical microscopies that are particularly critical for environmentally sensitive materials and for low temperature measurements where increased optical power can introduce unacceptable thermal perturbations.
42 ENGINEERING↗
Synthesis, characterization and optical properties of hybrid PVA–ZnO nanocomposite: A composition dependent study
Graphical abstract: - Highlights: • ZnO nanoparticles were prepared by solution combustion method. • PVA–ZnO nanocomposites were synthesized by solution casting method. • Doped and undoped films were characterized using different techniques. • Red shift in optical band gap was observed in Nanocomposite films with respect to nano ZnO. • Photoluminescence intensity was found to be optimum for PVA–10 mol% ZnO nanocomposite film. - Abstract: Nanocomposites of poly vinyl alcohol (PVA) and ZnO have been synthesized using the solution casting technique for different concentrations of nano ZnO powder prepared by low temperature solution combustion method. The formation of polymer nanocomposite and changes in the structural and micro structural properties of the materials were investigated by X-ray diffraction, Energy dispersive X ray spectroscopy and optical microscopy techniques (FTIR and UV–Visible). The surface morphology of PVA–ZnO nanocomposite films were elucidated using Scanning Electron Microscopy. The optical absorption spectrum of nano ZnO shows blue shift in the optical band gap energy with respect to characteristic bulk ZnO at room temperature, whereas PVA–ZnO hybrid films show red shift with respect to nano ZnO. The photoluminescence studies show that the intensity of the blue emission (470 nm) varies with change in concentration of ZnO with an optimum intensity observed at 10 mol% of ZnO.
36 MATERIALS SCIENCE↗