Julia Scherschligt

Toward 3D printed hydrogen storage materials made with ABS-MOF composites

The push to advance efficient, renewable, and clean energy sources has brought with it an effort to generate materials that are capable of storing hydrogen. Metal-organic framework materials (MOFs) have been the focus of many such studies as they are categorized for their large internal surface areas. We have addressed one of the major shortcomings of MOFs (their processibility) by creating and 3D printing a composite of acrylonitrile butadiene styrene (ABS) and MOF-5, a prototypical MOF, which is often used to benchmark H2 uptake capacity of other MOFs. The ABS-MOF-5 composites can be printed at MOF-5 compositions of 10% and below. Other physical and mechanical properties of the polymer (glass transition temperature, stress and strain at the breaking point, and Youngs modulus) either remain unchanged or show some degree of hardening due to the interaction between the polymer and the MOF. We do observe some MOF-5 degradation through the blending process, likely due to the ambient humidity through the purification and solvent casting steps. Even with this degradation, the MOF still retains some of its ability to uptake H2, seen in the ability of the composite to uptake more H2 than the pure polymer. The experiments and results described here represent a significant first step toward 3D printing MOF-5-based materials for H2 storage.

Development of a new UHV/XHV pressure standard (cold atom vacuum standard)

The National Institute of Standards and Technology has recently begun a program to develop a primary pressure standard that is based on ultra-cold atoms, covering a pressure range of 1 × 10-6 Pa to 1 × 10-10 Pa and possibly lower. These pressures correspond to the entire ultra-high vacuum (UHV) range and extend into the extreme-high vacuum (XHV). This cold-atom vacuum standard (CAVS) is both a primary standard and absolute sensor of vacuum. The CAVS is based on the loss of cold, sensor atoms (such as the alkali-metal lithium) from a magnetic trap due to collisions with the background gas (primarily H2) in the vacuum. The pressure is determined from a thermally-averaged collision cross section, which is a fundamental atomic property, and the measured loss rate. The CAVS is primary because it will use collision cross sections determined from ab initio calculations for the Li + H2 system. Primary traceability is transferred to other systems of interest using sensitivity coefficients.

Investigations of medium-temperature heat treatments to achieve low outgassing rates in stainless steel ultrahigh vacuum chambers

The authors investigated the outgassing rates and fluxes of vacuum chambers constructed from common 304L stainless steel vacuum components and subjected to heat treatments. Our goal was to obtain H2 outgassing flux on the order of 10-11 Pa l s-1cm-2 or better from standard stainless steel vacuum components readily available from a variety of manufacturers. The authors found that a medium-temperature bake in the range of 400 to 450°C, performed with the interior of the chamber under vacuum, was sufficient to produce the desired outgassing flux. The authors also found that identical vacuum components baked in air at the same temperature for the same amount of time did not produce the same low outgassing flux. In that case, the H2 outgassing flux was lower than that of a stainless-steel chamber with no heat treatment, but was still approximately 1 order of magnitude higher than that of the medium-temperature vacuum-bake. Additionally, the authors took the chamber that was subjected to the medium-temperature vacuum heat treatment and performed a 24-h air bake at 430°C. This additional heat treatment lowered the outgassing rate by nearly a factor of two, which strongly suggests that the air-bake created an oxide layer which reduced the hydrogen recombination rate on the surface. [http://dx.doi.org/10.1116/1.4983211].

Pressure Balance Cross-Calibration Method Using a Pressure Transducer as Transfer Standard

Abstract: Piston gauges or pressure balances are widely used to realize the SI unit of pressure, the pascal, and to calibrate pressure sensing devices. However, their calibration is time consuming and requires a lot of technical expertise. In this article, we propose an alternate method of performing a piston gauge cross calibration that incorporates a pressure transducer as an immediate in-situ transfer standard. For a sufficiently linear transducer, the requirement to exactly balance the weights on the two pressure gauges under consideration is greatly relaxed. Our results indicate that this method can be employed without a significant increase in measurement uncertainty. Indeed, in the test case explored here, our results agreed with the traditional method within standard uncertainty, which was less than 6 parts per million.

Note: A 3D-printed alkali metal dispenser

We demonstrate and characterize a source of Li atoms made from direct metal laser sintered titanium. The sources outgassing rate is measured to be 5(2) × 10-7 Pa L s-1 at a temperature T = 330 °C, which optimizes the number of atoms loaded into a magneto-optical trap. The source loads ≈1077Li atoms in the trap in ≈1 s. The loaded source weighs 700 mg and is suitable for a number of deployable sensors based on cold atoms.

Vacuum furnace for degassing stainless-steel vacuum components

Ultra-high vacuum systems must often be constructed of materials with ultra-low outgassing rates to achieve pressure of 10-6 Pa and below. Any component placed into the ultra-high vacuum system must also be constructed of materials with ultra-low outgassing rates. Baking stainless steel vacuum components to a temperature range of 400 °C to 450 °C while under vacuum is an effective method to reduce the outgassing rate of vacuum components for use in ultra-high vacuum systems. The design, construction, and operation of a vacuum furnace capable of baking vacuum components to a temperature of 450° C while maintaining a pressure of 10-3 Pa or lower is described. The furnace has been used for extended bakes at 450 °C while maintaining pressures below 10-5 Pa. As an example, we obtained an outgassing rate of 1.2 × 10-9 Pa L s-1 for a gate valve baked for 20 days at a temperature of 420 °C.

Review Article: Quantum-based vacuum metrology at the National Institute of Standards and Technology

The measurement science in realizing and disseminating the unit for pressure in the International System of Units, the pascal (Pa), has been the subject of much interest at the National Institute of Standards and Technology (NIST). Modern optical-based techniques for pascal metrology have been investigated, including multiphoton ionization and cavity ringdown spectroscopy. Work is ongoing to recast the pascal in terms of quantum properties and fundamental constants and in doing so make vacuum metrology consistent with the global trend toward quantum-based metrology. NIST has ongoing projects that interrogate the index of refraction of a gas using an optical cavity for low vacuum, and count background particles in high vacuum to extreme high vacuum using trapped laser-cooled atoms.The measurement science in realizing and disseminating the unit for pressure in the International System of Units, the pascal (Pa), has been the subject of much interest at the National Institute of Standards and Technology (NIST). Modern optical-based techniques for pascal metrology have been investigated, including multiphoton ionization and cavity ringdown spectroscopy. Work is ongoing to recast the pascal in terms of quantum properties and fundamental constants and in doing so make vacuum metrology consistent with the global trend toward quantum-based metrology. NIST has ongoing projects that interrogate the index of refraction of a gas using an optical cavity for low vacuum, and count background particles in high vacuum to extreme high vacuum using trapped laser-cooled atoms.

Gas uptake of 3D printed acrylonitrile butadiene styrene using a vacuum apparatus designed for absorption and desorption studies

We describe a vacuum apparatus for determining the outgassing rate into vacuum, the diffusion coefficient, and the amount of gas absorbed for various materials. The diffusion coefficient is determined from a model applied to time-dependent desorption data taken using a throughput method. We used this method to determine the diffusion coefficient, D, for H2O in 3-D printed acrylonitrile butadiene styrene (ABS). We found DH2O = 8.3 × 10-8 cm2/s ± 1.3 × 10-8 cm2/s (k = 1; 67% confidence interval) at 23.2 °C. This result was compared to the diffusion coefficient determined another by a gravimetric method, in which the sample weight was monitored as it absorbed gas from the atmosphere. The two methods agreed to within 3%, which is well within the uncertainty of the measurement. We also found that at least 80% of the atmospheric gas (air) absorbed by the ABS is water. The total amount of all atmospheric gas absorbed by ABS was about 0.35% by weight when exposed to ambient air in the laboratory, which was at a pressure of 101 kPa with a relative humidity of 57% at 22.2 °C.

Automated Piston Gauge Calibration System

Abstract Piston gauges or pressure balances are important primary standards for the realization of the SI unit of pressure, the pascal. Because of their long-term stability, they are also used as secondary or working standards in the dissemination of the pressure scale. The National Institute of Standards and Technology (NIST) operates and maintains a calibration service for these devices, and has recently undertaken a modernization effort. Following a preliminary investigation into the feasibility of using transducers as instantaneous in-situ transfer standards, we now present the results of a near fully automated calibration system. This effort includes the design, building, and validation of an automated gas-handling manifold, and the development of a new software suite. The new system demonstrates an expanded uncertainty on the order of 1 in 105, comparable to the traditional system, but offers a five-fold decrease in calibration turnaround time.

Quantum-based vacuum metrology at NIST

The measurement science in realizing and disseminating the unit for pressure in the International System of Units (SI), the pascal (Pa), has been the subject of much interest at the National Institute of Standards and Technology (NIST). Modern optical-based techniques for pascal metrology have been investigated, including multi-photon ionization and cavity ringdown spectroscopy. Work is ongoing to recast the pascal in terms of quantum properties and fundamental constants and in so doing, make vacuum metrology consistent with the global trend toward quantum-based metrology. NIST has ongoing projects that interrogate the index of refraction of a gas using an optical cavity for low vacuum, and count background particles in high vacuum to extreme high vacuum using trapped laser-cooled atoms.