Anthony W. van Buuren

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

In Situ Real-Time Radiographic Study of Thin Film Formation Inside Rotating Hollow Spheres

Hollow spheres with uniform coatings on the inner surface have applications in optical devices, time- or site-controlled drug release, heat storage devices, and target fabrication for inertial confinement fusion experiments. The fabrication of uniform coatings, which is often critical for the application performance, requires precise understanding and control over the coating process and its parameters. Here, we report on in situ real-time radiography experiments that provide critical spatiotemporal information about the distribution of fluids inside hollow spheres during uniaxial rotation. Image analysis and computer fluid dynamics simulations were used to explore the effect of liquid viscosity and rotational velocity on the film uniformity. The data were then used to demonstrate the fabrication of uniform sol-gel chemistry derived porous polymer films inside 2 mm inner diameter diamond shells.

Atomic layer deposition-derived ultra-low-density composite bulk materials with deterministic density and composition.

A universal approach for on-demand development of monolithic metal oxide composite bulk materials with air-like densities (<5 mg/cm(3)) is reported. The materials are fabricated by atomic layer deposition of titania (TiO2) or zinc oxide (ZnO) using the nanoscale architecture of 1 mg/cm(3) SiO2 aerogels formed by self-organization as a blueprint. This approach provides deterministic control over density and composition without affecting the nanoscale architecture of the composite material that is otherwise very difficult to achieve. We found that these materials provide laser-to-X-ray conversion efficiencies of up to 5.3%, which is the highest conversion efficiency yet obtained from any foam-based target, thus opening the door to a new generation of highly efficient laser-induced nanosecond scale multi-keV X-ray sources.

Grain boundary dominated electrical conductivity in ultrananocrystalline diamond

N-type electrically conductive ultrananocrystalline diamond (UNCD) films were deposited using the hot filament chemical vapor deposition technique with a gas mixture of H2, CH4 and NH3. Depending on the deposition temperature and ammonia feed gas concentration, which serves as a nitrogen source, room temperature electrical conductivities in the order of 10−2 to 5 × 101 S/cm and activation energies in the meV range were achieved. In order to understand the origin of the enhanced electrical conductivity and clarify the role of ammonia addition to the process gas, a set of UNCD films was grown by systematically varying the ammonia gas phase concentration. These samples were analyzed with respect to their morphology and electrical properties as well as their carbon and nitrogen bonding environments. Temperature dependent electrical conductivity measurements (300–1200 K) show that the electrical conductivity of the samples increases with temperature. The near edge x-ray absorption fine structure measurements reveal that the electrical conductivity of the UNCD films does not correlate directly with ammonia addition, but depends on the total amount of sp2 bonded carbon in the deposited films.N-type electrically conductive ultrananocrystalline diamond (UNCD) films were deposited using the hot filament chemical vapor deposition technique with a gas mixture of H2, CH4 and NH3. Depending on the deposition temperature and ammonia feed gas concentration, which serves as a nitrogen source, room temperature electrical conductivities in the order of 10−2 to 5 × 101 S/cm and activation energies in the meV range were achieved. In order to understand the origin of the enhanced electrical conductivity and clarify the role of ammonia addition to the process gas, a set of UNCD films was grown by systematically varying the ammonia gas phase concentration. These samples were analyzed with respect to their morphology and electrical properties as well as their carbon and nitrogen bonding environments. Temperature dependent electrical conductivity measurements (300–1200 K) show that the electrical conductivity of the samples increases with temperature. The near edge x-ray absorption fine structure measurements r...

Single-bunch imaging of detonation fronts using scattered synchrotron radiation

A centimeter-scale field of view for transmission X-ray radiography from a sub-millimeter-focused synchrotron X-ray beam is achieved by placing a strongly scattering material upstream of the sample. Combining the scattered beam with a detector system synchronized and gated to acquire images from single X-ray pulses provides the capability for time-resolved observations of transient phenomena in samples larger than the native X-ray beam. Furthermore, switching between this scatter-beam imaging (SBI) and scattering modes is trivial compared to switching between unfocused white beam imaging and scattering using a focused pink beam. As a result, SBI additionally provides a straightforward method to precisely align samples relative to the focused X-ray beam for subsequent small-angle X-ray scattering measurements. This paper describes the use of glassy carbon for SBI to observe phenomena during detonation of small-scale high explosive charges and compares the technique to conventional white beam imaging. SBI i...

Carbon Nanotube Porins in Amphiphilic Block Copolymers as Fully Synthetic Mimics of Biological Membranes

Biological membranes provide a fascinating example of a separation system that is multifunctional, tunable, precise, and efficient. Biomimetic membranes, which mimic the architecture of cellular membranes, have the potential to deliver significant improvements in specificity and permeability. Here, a fully synthetic biomimetic membrane is reported that incorporates ultra-efficient 1.5 nm diameter carbon nanotube porin (CNTPs) channels in a block-copolymer matrix. It is demonstrated that CNTPs maintain high proton and water permeability in these membranes. CNTPs can also mimic the behavior of biological gap junctions by forming bridges between vesicular compartments that allow transport of small molecules.