David D. Allred received Alumni Professorship Award

High-temperature microfluidic devices (such as gas chromatography microcolumns) have traditionally been fabricated using photolithography, etching, and wafer bonding which allow for precise microscale features but lack the ability to form complex 3D designs. Metal additive manufacturing could enable higher complexity microfluidic designs if reliable methods for fabrication are developed, but forming small negative features is challenging-especially in powder-based processes. In this paper, the formation of sealed metal microchannels was demonstrated using stainless-steel binder jetting with bronze infiltration. To create small negative features, bronze infiltrant must fill the porous part produced by binder jetting without filling the negative features. This was achieved through sacrificial powder infiltration (SPI), wherein sacrificial powder reservoirs (pore size similar to 60 mu m) are used to control infiltrant pressure. With this pressure control, the infiltrant selectively filled the small pores between particles in the printed part (pore size similar to 3 mu m) while leaving printed microchannels (700 mu m and 930 mu m) empty. To develop the SPI method, a pore filling study was performed in this stainless-steel/bronze system with 370 mu m, 650 mu m, and 930 mu m microchannel segments. This study enabled SPI process design on these length scales by determining variations in pore filling across a sample and preferential filling between different sized pores.

A miniaturized short-wavelength infrared spectrometer for use with diffuse light was created by combining a thin form factor carbon nanotube composite collimator, a linear variable filter, and an InGaAs photodiode array. The resulting spectrometer measures 3 mm × 4 mm × 14 mm and shows a significant improvement in resolution over a spectrometer without the collimator when used with diffuse light. Its small size and high throughput make it ideal for applications such as wearable optical sensing, where light from highly scattering tissue is measured. Plethysmographic measurements on the wrist were demonstrated, showing rapid data collection with diffuse light.

Understanding processing-structure-property (PSP) linkages of solid-phase microextraction (SPME) coating materials is crucial for the rational design and advancement of these new materials. As SPME is a diffusion-based extraction technique, analyzing the morphology of its coating materials is important for optimizing its performance. In this study, we assess the morphological evolution of micro/mesoporous amorphous silicon (a-Si) thin films sputtered at an oblique angle onto silicon, which serve as models for support materials in SPME devices. The contrast of scanning transmission electron microscopy (STEM) images is enhanced via ZnO infiltration by atomic layer deposition (ALD). Various metrics, including physical descriptors and two-point statistics methods, are employed to follow the films' evolution. Analysis of the two-point correlation function reveals a simple ellipse/spherical local pore geometry in contrast to the long-range irregular arrangement of pores identified by a range of traditional and novel metrics. Additionally, analyzing the internal structure of the pores through homology metrics aligns well with the theoretical understanding of morphological evolution in oblique sputtered films. These analyses show that the “average ratio of principal moment of inertia”, “Betti numbers”, and “two-point statistics” based metrics can capture valuable information during film growth.

The morphological analysis approach proposed in this study can be applied to analyze any nanoporous medium as a first step towards developing structure-property relationships that tie back to a given preparation method. Ultimately, a more extensive experimental and/or simulation-based study should confirm the correlations between these metrics and actual diffusion properties as the basis for process-structure-properties relations for improved design and optimization of this film.

Estimating the elastic modulus and strength of heterogeneous films requires local measurement techniques. For local mechanical film testing, microcantilevers were cut into suspended many-layer graphene using a focused ion beam. An optical transmittance technique was used to map thickness near the cantilevers, and multipoint force–deflection mapping with an atomic force microscope was used to record the compliance of the cantilevers. These data were used to estimate the elastic modulus of the film by fitting the compliance at multiple locations along the cantilever to a fixed-free Euler–Bernoulli beam model. This method resulted in a lower uncertainty than is possible from analyzing only a single force–deflection. The breaking strength of the film was also found by deflecting cantilevers until fracture. The average modulus and strength of the many-layer graphene films are 300 and 12 GPa, respectively. The multipoint force–deflection method is well suited to analyze films that are heterogeneous in thickness or wrinkled.

In the last two decades, advances in the dark field detectors and microscopes of scanning transmission electron microscopy (STEM) have inspired a resurgence of interest in quantitative STEM analysis. One promising avenue is the use of STEM as a nanothermometric probe. In this application, thermal diffuse scattering, captured by a CCD camera or an annular dark field detector, acts as an indirect measurement of the specimen temperature. One challenge with taking such a measurement is achieving adequate sensitivity to quantify a change in scattered electron signal on the order of 1% or less of the full electron beam. Another difficulty is decoupling the thermal effect on electron scattering from scattering changes due to differing specimen thicknesses and materials. To address these issues, we have developed a method using STEM, combined with electron energy loss spectroscopy (EELS), to produce a material-specific calibration curve. On silicon, across the range 89 K to 294 K, we measured a monotonically increasing HAADF signal ranging from 4.0% to 4.4% of the direct beam intensity at a thickness-to-mean-free-path ratio of 0.5. This yielded a calibration curve of temperature versus full-beam-normalized, thickness-normalized HAADF signal. The method enables thermal measurements on a specimen of varying local thickness at a spatial resolution of a few nanometers. We demonstrated the potential of the technique for testing electron scattering models by applying single-electron scattering theory to the data collected to extract a measurement of the mean atomic vibration amplitude in silicon at 294 K. The measured value, 0.00738 +/- 0.00002 nm, agrees well with reported measurement using X-rays.

Hollow cathode plasmas are common extreme ultraviolet (EUV) lamps used for material characterization. However, the relatively high pressure of the plasma can affect downstream instruments, as well as absorb the EUV. EUV windows are difficult to fabricate due to EUV’s strong interaction with all materials. We present a carbon nanotube (CNT) microfabricated window composed of multiple high aspect-ratio columns in parallel. The open areas allow wide bandpass transmission, while the walls restrict gas flow. We model the CNT window transmission as a weight function on the light from of a Mcpherson 629-like hollow cathode helium plasma in visible wavelengths. We model the CNT window differential pumping as a series of columns between two chambers of different pressures.