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Keller, Jennie

Publications and source records attributed to Keller, Jennie.

SAVY-4000 O-Ring and Filter Lifetime Extension Report

The 3-year accelerated aging study of the SAVY-4000 O-ring detailed in our previous Lifetime Extension Report showed very little evidence of significant degradation to samples subjected to aggressive elevated temperature and radiation conditions. Whole container thermal aging studies followed by helium leakage testing and compression set measurements were used to establish a failure criterion estimate for O-ring compression set of ≥ 65 %, which led to an O-ring lifetime estimate of greater than 65 years at 80°C. Herein, we describe a statistical model of the 3-year accelerated aging study and present additional results gathered in FY17 that further support the lifetime extension of the O-ring to 40 years at 80°C. Because we are choosing an extremely conservative lifetime value (40 years) compared to the aging study results (>65 years), the O-ring lifetime could be extended further, especially if supported by surveillance results collected over the years to come.

36 MATERIALS SCIENCE↗

Comparative Assessment of Copper-Coated Kapton: Analysis of Microclad from Several Manufacturing Lots

Microclad is a composite material consisting of a thin copper coating applied on a single side over a Kapton substrate. Kapton is the commercial designator for polyimide supplied by DuPont. Microclad is a key material in detonator manufacture and function. Detonators which utilize Microclad function when a large current applied through a thin bridge etched into the copper produces a plasma, accelerating a Kapton flyer into an explosive (PETN) pellet. The geometry and properties of the Microclad are a critical element of this process.

36 MATERIALS SCIENCE↗

Lifetime Extension Report: Progress on the SAVY-4000 Lifetime Extension Program

The 3-year accelerated aging study of the SAVY-4000 O-ring shows very little evidence of significant degradation to samples subjected to aggressive elevated temperature and radiation conditions. Whole container thermal aging studies followed by helium leakage testing and compression set measurements were used to establish an estimate for a failure criterion for O-ring compression set of ≥65 %. The whole container aging studies further show that the air flow and efficiency functions of the filter do not degrade significantly after thermal aging. However, the degradation of the water-resistant function leads to water penetration failure after four months at 210°C, but does not cause failure after 10 months at 120°C (130°C is the maximum operating temperature for the PTFE membrane). The thermal aging data for O-ring compression set do not meet the assumptions of standard time-temperature superposition analysis for accelerated aging studies. Instead, the data suggest that multiple degradation mechanisms are operative, with a reversible mechanism operative at low aging temperatures and an irreversible mechanism dominating at high aging temperatures. To distinguish between these mechanisms, we have measured compression set after allowing the sample to physically relax, thereby minimizing the effect of the reversible mechanism. The resulting data were analyzed using two distinct mathematical methods to obtain a lifetime estimate based on chemical degradation alone. Both methods support a lifetime estimate of greater than 150 years at 80°C. Although the role of the reversible mechanism is not fully understood, it is clear that the contribution to the total compression set is small in comparison to that due to the chemical degradation mechanism. To better understand the chemical degradation mechanism, thermally aged O-ring samples have been characterized by Fourier Transform Infrared (FTIR), Electron Paramagnetic Resonance (EPR), Gel Permeation Chromatography (GPC), and Differential Scanning Calorimetry (DSC). These experiments detect no significant O-ring degradation below 80°C. Furthermore, durometer measurements indicate that there is no significant change in O-ring hardness at all aging conditions examined. Therefore, our current conservative lifetime estimate for the O-ring and the filter is 10 years at 80°C. In FY17, we will continue to probe the chemical degradation mechanism using oxygen consumption measurements under accelerated aging conditions to reveal temperatures at which oxidation occurs, along with any differences in oxidation rate at the low vs. high aging temperatures. We will also refine the failure criteria and finalize the radiation/thermal synergistic studies to determine a final design lifetime.

42 ENGINEERING↗

Sylgard® Mixing Study

Sylgard® 184 and Sylgard® 186 silicone elastomers form Dow Corning® are used as potting agents across the Nuclear Weapons Complex. A standardized mixing procedure is required for filled versions of these products. The present study is a follow-up to a mixing study performed by MST-7 which established the best mixing procedure to use when adding filler to either 184 or 186 base resins. The most effective and consistent method of mixing resin and curing agent for three modified silicone elastomer recipes is outlined in this report. For each recipe, sample size, mixing type, and mixing time was varied over 10 separate runs. The results show that the THINKY™ Mixer gives reliable mixing over varying batch sizes and mixing times. Hand Mixing can give improved mixing, as indicated by reduced initial viscosity; however, this method is not consistent.

36 MATERIALS SCIENCE↗

Plackett-Burman Analysis of Glass Microballoon Filled Syntactic Foams

Syntactic foams are an important category of composite materials that have abundant applications in a wide variety of fields. The current study utilized a Plackett-Burman (PB) experimental design to investigate the main effects of six variables on properties of syntactic foams formulated from a silicone elastomer and glass microballoons(MB). Findings from this investigation are meant to identify the most significant variables with respect to foam properties. Eight foam samples were created and tested using thermal, physical and mechanical techniques. The data from these tests was then evaluated using a Plackett-Burman response coefficient calculation (RCC). This calculation was applied to determine the statistical significance of the selected variables by comparison with a dummy variable. The data suggests that thermal properties, such as glass transition temperature and coefficient of thermal expansion, do not rely on any of the studied variables. Physical and mechanical measurements however were found to depend heavily on the matrix composition and the vacuum pressure used during mixing. Some variables were found to have little to no effect on any of the studied properties. Ultimately, this data could be used to formulate a comprehensive catalogue of syntactic foams based on their compositions. This type of database would allow customers in industry to identify which syntactic foam would best fit their application according to one or two properties.

36 MATERIALS SCIENCE↗

Literature Review: Silicone Applications in Health Care

Early in the 20 th century, the term ‘silicone’ was coined by Professor Frederic Stanley Kipping, a British chemist and one of the founding fathers of silicon chemistry. The word was given to describe new compounds containing a Si-O linkage (siloxane bond) and basic chemical formula R 2 -Si-O. In industry, silicone usually refers to linear polydimethylsiloxane (PDMS), the most basic silicone polymer containing only methyl groups as substituents in the polymeric structure. However, the term silicone can also be used to describe complex polymer structures that feature a wide range of functional groups, branching or crosslinking. “The properties of basic PDMS materials can be changed by replacing some methyl groups with other organic groups or atoms.” Substitution of this type is useful when specific physical and chemical properties are required of the material, such as adhesion or compatibility with a certain substrate.

36 MATERIALS SCIENCE↗

Literature Review: An Overview of Epoxy Resin Syntactic Foams with Glass Microballoons

Syntactic foams are an important category of composite materials that have abundant applications in a wide variety of fields. The bulk phase of syntactic foams is a three-part epoxy resin formulation that consists of a base resin, a curative (curing agent) and a modifier (diluent and/or accelerator) [12]. These thermoset materials [12] are used frequently for their thermal stability [9], low moisture absorption and high compressive strength [10]. The characteristic feature of a syntactic foam is a network of beads that forms pores within the epoxy matrix [3]. In this review, hollow glass beads (known as glass microballoons) are considered, however, solid beads or microballoons made from materials such as ceramic, polymer or metal can also be used [3M, Peter]. The network of hollow beads forms a closed-cell foam; the term closed-cell comes from the fact that the microspheres used in the resin matrix are completely closed and filled with gas (termed hollow). In contrast, the microspheres used in open-cell foams are either not completely closed or broken so that matrix material can fill the spheres [11]. Although closed foams have been found to possess higher densities than open cell foams, their rigid structures give them superior mechanical properties [12]. Past research has extensively studied the effects that changing the volume fraction of microballoons to epoxy will have on the resulting syntactic foam [3,4,9]. In addition, published literature also explores how the microballoon wall thickness affects the final product [4,9,10]. Findings detail that indeed both the mechanical and some thermal properties of syntactic foams can be tailored to a specific application by varying either the volume fraction or the wall thickness of the microballoons used [10]. The major trends in syntactic foam research show that microballoon volume fraction has an inversely proportionate relationship to dynamic properties, while microballoon wall thickness is proportional to those same properties [3,4,9,10]. The glass transition temperature has a proportional relationship to the volume fraction of microballoons used, however, there is limited research that supports correlations between other thermal variables and microballoons specifications. In fact, very little experimental data exists to relate thermal conductivity and volume fraction or wall thickness of microballoons [5]. This review proposes that thermal conductivity should be a topic of interest for future researchers because of how frequently syntactic foams are used in insulating applications. This paper will explore three aspects pertaining to epoxy resin syntactic foams with glass microballoons: the immense range of applications that syntactic foams are used for, the materials and fabrication techniques most commonly used, and lastly the results from characterization of syntactic foams with varying microballoon volume fractions and wall thicknesses. In addition to varying microballoon parameters, it is also possible to change the base, accelerator and curing agent used in the epoxy formulation. For simplicity, this paper will focus on a very common combination of materials produced by the Dow Chemical Company®.

36 MATERIALS SCIENCE↗