Makfir Sefa

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.

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].

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.

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.

Comparison of permeation of atmospheric gases through Viton O-ring gaskets for different initial conditions

Viton O-ring gaskets are frequently used in high vacuum for demountable flange and vacuum valve seals. Atmospheric gases, particularly water vapor from humid air, permeate through Viton gaskets and thus limit the lowest attainable pressure level in vacuum systems. In this work, a comparison of a vacuum degassed Viton O-ring gasket and a gasket fully saturated with atmospheric gases was performed. A reference measurement with an alternative soft metal gasket for Klein Flange type flanges was also made. The permeation rate of each individual gas from the atmosphere (water vapor, N2, O2, Ar, and CO2) through the Viton O-ring was measured using quadrupole mass spectrometry. The partial gas flow curves Q(t) were also modeled using finite difference modeling (FDM). Using FDM, one can determine the diffusion constant, permeability, and solubility of the gas in the material.

How to Build a Vacuum Spring-transport Package for Spinning Rotor Gauges.

The spinning rotor gauge (SRG) is a high-vacuum gauge often used as a secondary or transfer standard for vacuum pressures in the range of 1.0 x 10(-4) Pa to 1.0 Pa. In this application, the SRGs are frequently transported to laboratories for calibration. Events can occur during transportation that change the rotor surface conditions, thus changing the calibration factor. To assure calibration stability, a spring-transport mechanism is often used to immobilize the rotor and keep it under vacuum during transport. It is also important to transport the spring-transport mechanism using packaging designed to minimize the risk of damage during shipping. In this manuscript, a detailed description is given on how to build a robust spring-transport mechanism and shipping container. Together these form a spring-transport package. The spring-transport package design was tested using drop-tests and the performance was found to be excellent. The present spring-transport mechanism design keeps the rotor immobilized when experiencing shocks of several hundred g (g = 9.8 m/sec(2) and is the acceleration due to gravity), while the shipping container assures that the mechanism will not experience shocks greater than about 100 g during common shipping mishaps (as defined by industry standards).

Building a spring-transport package for spinning rotor gauges

Spinning rotor gauges (SRGs) are widely used as transfer standards in interlaboratory comparisons and as secondary standards by calibration laboratories. In both of these applications, it is necessary to ship the SRG for calibration, often internationally over long distances. A spring-transport mechanism is a device used to immobilize the SRG and keep it under vacuum during transport. To assure that the SRG will not be damaged during shipment, it is also important to have packaging that protects the SRG and spring-transport mechanism. This shop-note describes the design and mechanical testing of a robust spring-transport mechanism and shipping container built by National Institute of Standards and Technology.