Timothy J. Roosendaal

An in situ tensile test apparatus for polymers in high pressure hydrogen

Degradation of material properties by high-pressure hydrogen is an important factor in determining the safety and reliability of materials used in high-pressure hydrogen storage and delivery. Hydrogen damage mechanisms have a time dependence that is linked to hydrogen outgassing after exposure to the hydrogen atmosphere that makes ex situ measurements of mechanical properties problematic. Designing in situ measurement instruments for high-pressure hydrogen is challenging due to known hydrogen incompatibility with many metals and standard high-power motor materials such as Nd. Here we detail the design and operation of a solenoid based in situ tensile tester under high-pressure hydrogen environments up to 42 MPa (6000 psi). Modulus data from high-density polyethylene samples tested under high-pressure hydrogen at 35 MPa (5000 psi) are also reported as compared to baseline measurements taken in air.

An in situ tribometer for measuring friction and wear of polymers in a high pressure hydrogen environment

High pressure hydrogen effects on the friction and wear of polymers are of importance to myriad applications. Of special concern are those used in the infrastructure for hydrogen vehicle refueling stations, including compressor sliding seals, valves, and actuators. While much is known about potentially damaging embrittlement effects of hydrogen on metals, relatively little is known about the effects of high pressure hydrogen on polymers. However, based on the limited results that are published in the literature, polymers also apparently exhibit compatibility issues with hydrogen. An additional study is needed to elucidate these effects to avoid incompatibilities either through design or material selection. As part of this effort, we present here in situ high pressure hydrogen studies of the friction and wear on example polymers. To this end, we have built and demonstrated a custom-built pin-on-flat linear reciprocating tribometer and demonstrated its use with in situ studies of friction and wear behavior of nitrile butadiene rubber polymer samples in 28 MPa hydrogen. Tribology results indicate that friction and wear is increased in high pressure hydrogen as compared both with values measured in high pressure argon and ambient air conditions.

Mechanical and electrical properties of low temperature phase MnBi

Low temperature phase (LTP) manganese bismuth (MnBi) is a promising rare-earth-free permanent magnet material due to its high intrinsic coercivity and large positive temperature coefficient. While scientists are making progress on fabricating bulk MnBi magnets, engineers have begun considering MnBi magnets for motor applications. Physical properties other than magnetic ones could significantly affect motor design. Here, we report results of our investigation on the mechanical and electrical properties of bulk LTP MnBi and their temperature dependence. A MnBi ingot was prepared using an arc melting technique and subsequently underwent grinding, sieving, heat treatment, and cryomilling. The resultant powders with a particle size of ∼5 μm were magnetically aligned, cold pressed, and sintered at a predefined temperature. Micro-hardness testing was performed on a part of original ingot and we found that the hardness of MnBi was 109 ± 15 HV. The sintered magnets were subjected to compressive testing at differen...

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

High pressure hydrogen gas is known to adversely affect metallic components of compressors, valves, hoses, and actuators. However, relatively little is known about the effects of high pressure hydrogen on the polymer sealing and barrier materials also found within these components. More study is required in order to determine the compatibility of common polymer materials found in the components of the hydrogen fuel delivery infrastructure with high pressure hydrogen. As a result, it is important to consider the changes in physical properties such as friction and wear in situ while the polymer is exposed to high pressure hydrogen. In this protocol, we present a method for testing the friction and wear properties of ethylene propylene diene monomer (EPDM) elastomer samples in a 28 MPa high pressure hydrogen environment using a custom-built in situ pin-on-flat linear reciprocating tribometer. Representative results from this testing are presented which indicate that the coefficient of friction between the EPDM sample coupon and steel counter surface is increased in high pressure hydrogen as compared to the coefficient of friction similarly measured in ambient air.

Fabrication of large area flexible nanoplasmonic templates with flow coating

We describe the development of a custom-built two-axis flow coater for the deposition of polymeric nanosphere monolayers that could be used in the fabrication of large area nanoplasmonic films. The technique described here has the capability of depositing large areas (up to 7 in. × 10 in.) of self-assembled monolayers of polymeric nanospheres onto polyethylene terephthalate (PET) films. Here, three sets of films consisting of different diameters (ranging from 100 to 300 nm) of polymeric nanospheres were used to demonstrate the capabilities of this instrument. To improve the surface wettability of the PET substrates during wet-deposition, we enhanced the wettability by using a forced air blown-arc plasma treatment system. Both the local microstructure, as confirmed by scanning electron microscopy, describing monolayer and multilayer coverage, and the overall macroscopic uniformity of the resultant nanostructured film were optimized by controlling the relative stage to blade speed and nanosphere concentration. We also show using a smaller nanoparticle template that such monolayers can be used to form nanoplasmonic films. As this flow-coating approach is a scalable technique, large area films such as the ones described here have a variety of crucial emerging applications in areas such as energy, catalysis, and chemical sensing.

Nanocrystalline SiC and Ti3SiC2 Alloys for Reactor Materials: Thermal and Mechanical Properties

SiC-polymers (pure polycarbosilane and polycarbosilane filled with SiC-particles) are being combined with Si and TiC powders to create a new class of polymer-derived ceramics for consideration as advanced nuclear materials in a variety of applications. Compared to pure SiC these materials have increased fracture toughness with only slightly reduced thermal conductivity. Future work with carbon nanotube (CNT) mats will be introduced with the potential to increase the thermal conductivity and the fracture toughness. At present, this report documents the fabrication of a new class of monolithic polymer derived ceramics, SiC + SiC/Ti3SiC2 dual phase materials. The fracture toughness of the dual phase material was measured to be significantly greater than Hexoloy SiC using indentation fracture toughness testing. However, thermal conductivity of the dual phase material was reduced compared to Hexoloy SiC, but was still appreciable, with conductivities in the range of 40 to 60 W/(m K). This report includes synthesis details, optical and scanning electron microscopy images, compositional data, fracture toughness, and thermal conductivity data.

Monitoring thermal fatigue damage in nuclear power plant materials using acoustic emission

Proactive aging management of nuclear power plant passive components requires technologies to enable monitoring and accurate quantification of material condition at early stages of degradation (i.e., pre-macrocrack). Acoustic emission (AE) is well-suited to continuous monitoring of component degradation and is proposed as a method to monitor degradation during accelerated thermal fatigue tests. A key consideration is the ability to separate degradation responses from external sources such as water spray induced during thermal fatigue testing. Water spray provides a significant background of acoustic signals, which can overwhelm AE signals caused by degradation. Analysis of AE signal frequency and energy is proposed in this work as a means for separating degradation signals from background sources. Encouraging results were obtained by applying both frequency and energy filters to preliminary data. The analysis of signals filtered using frequency and energy provides signatures exhibiting several characteristics that are consistent with degradation accumulation in materials. Future work is planned to enable verification of the efficacy of AE for thermal fatigue crack initiation detection. While the emphasis has been placed on the use of AE for crack initiation detection during accelerated aging tests, this work also has implications with respect to the use of AE as a primary tool for early degradation monitoring in nuclear power plant materials. The development of NDE tools for characterization of aging in materials can also benefit from the use of a technology such as AE which can continuously monitor and detect crack initiation during accelerated aging tests.