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Title: Outgassing Studies of Foams for the W80 LEP (FY05)

Abstract

Removable epoxy foam (REF) is a novel material developed by researchers at Sandia National Laboratories to simplify the removal of encapsulants from electronic components [McElhanon, et al., Journal of Applied Polymer Science, 2002, 85, 1496-1502]. The material is based on a resin that includes a thermally reversible chemical bond. When the material is heated at relatively mild temperatures ({approx}50-90 C) in the presence of appropriate solvents, the reversible bonds are broken, and the material is easily rinsed away. In order to ease the removal of the encapsulant for surveillance purposes, it was proposed to use REF in the W80 LEP in place of the polyurethane TDI (toluene diisocyanate), which is being phased out at the Kansas City Plant due to toxicity concerns. Colleagues at Sandia noted that REF exhibited especially high outgassing of the liquid fluorinert, FC-72, which is used at a level of 5 wt% as the blowing agent in the foaming process. After obtaining a sample of the material from Sandia, headspace solid phase microextraction gas chromatography-mass spectrometry (SPME GC/MS) measurements were performed. These measurements revealed significant outgassing of fluorinert as well as other solvents and siloxanes [Memo, Vance, 3/3/05 & Vance, Foam PRT presentation UCRL-PRES-212462]. This reportmore » is intended to summarize foam outgassing studies performed at LLNL in support of the W80 LEP.« less

Authors:
; ;
Publication Date:
Research Org.:
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
889995
Report Number(s):
UCRL-TR-217477
TRN: US200620%%196
DOE Contract Number:
W-7405-ENG-48
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CHEMICAL BONDS; DEGASSING; KANSAS CITY PLANT; LAWRENCE LIVERMORE NATIONAL LABORATORY; POLYMERS; POLYURETHANES; REMOVAL; RESINS; SANDIA NATIONAL LABORATORIES; SILOXANES; SOLVENTS; SPECTROSCOPY; TOLUENE; TOXICITY

Citation Formats

Alviso, C, Harvey, C, and Vance, A. Outgassing Studies of Foams for the W80 LEP (FY05). United States: N. p., 2005. Web. doi:10.2172/889995.
Alviso, C, Harvey, C, & Vance, A. Outgassing Studies of Foams for the W80 LEP (FY05). United States. doi:10.2172/889995.
Alviso, C, Harvey, C, and Vance, A. Wed . "Outgassing Studies of Foams for the W80 LEP (FY05)". United States. doi:10.2172/889995. https://www.osti.gov/servlets/purl/889995.
@article{osti_889995,
title = {Outgassing Studies of Foams for the W80 LEP (FY05)},
author = {Alviso, C and Harvey, C and Vance, A},
abstractNote = {Removable epoxy foam (REF) is a novel material developed by researchers at Sandia National Laboratories to simplify the removal of encapsulants from electronic components [McElhanon, et al., Journal of Applied Polymer Science, 2002, 85, 1496-1502]. The material is based on a resin that includes a thermally reversible chemical bond. When the material is heated at relatively mild temperatures ({approx}50-90 C) in the presence of appropriate solvents, the reversible bonds are broken, and the material is easily rinsed away. In order to ease the removal of the encapsulant for surveillance purposes, it was proposed to use REF in the W80 LEP in place of the polyurethane TDI (toluene diisocyanate), which is being phased out at the Kansas City Plant due to toxicity concerns. Colleagues at Sandia noted that REF exhibited especially high outgassing of the liquid fluorinert, FC-72, which is used at a level of 5 wt% as the blowing agent in the foaming process. After obtaining a sample of the material from Sandia, headspace solid phase microextraction gas chromatography-mass spectrometry (SPME GC/MS) measurements were performed. These measurements revealed significant outgassing of fluorinert as well as other solvents and siloxanes [Memo, Vance, 3/3/05 & Vance, Foam PRT presentation UCRL-PRES-212462]. This report is intended to summarize foam outgassing studies performed at LLNL in support of the W80 LEP.},
doi = {10.2172/889995},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Wed Nov 23 00:00:00 EST 2005},
month = {Wed Nov 23 00:00:00 EST 2005}
}

Technical Report:

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  • Compatibility and outgassing studies of non-nuclear materials were carried out in support of the W80 Life Extension Program. These studies included small-scale laboratory experiments as well as participation in Sandia's Materials Aging and Compatibility test (MAC-1). Analysis of the outgassing signature of removable epoxy foam (REF) revealed unusually high levels of volatile organic compounds in the material. REF was replaced with the polyurethane PMDI. Laboratory compatibility tests of high priority materials were performed and revealed incompatibilities between Viton A (LX-07 binder) and syntactic polysulfide as well as Viton A and REF. With the removal of REF from the system, themore » incompatibility with Viton A is not an issue. In the case of the viton/polysulfide, both of these materials have a history of reliability in the stockpile, and the observed results, while scientifically interesting, appear to be a laboratory anomaly. Participation in the MAC-1 test led to a detailed study of Viton A degradation. At elevated temperatures up to 70 C, the Viton A samples darkened and exhibited increased crosslinking. Laboratory experiments were pursued to correlate the observed changes to exposure to specific compounds that were present in the MAC-1 canister atmospheres. Exposure to siloxanes resulted in changes similar to those seen in the MAC-1 samples. Knowledge gained from the MAC-1 test will be applied to the upcoming MAC-2 test planned for FY06. Finally, the suitability of isotopically labeled nitrogen fill gas ({sup 15}N{sub 2}) was addressed. This gas will behave as standard nitrogen with no compatibility concerns expected.« less
  • Established techniques must be extended down to the ps and sub-ps time domain to directly probe product states of materials under extreme conditions. We used short pulse ({le} 1 ps) x-ray radiation to track changes in the physical properties in tandem with measurements of the atomic and electronic structure of materials undergoing fast laser excitation and shock-related phenomena. The sources included those already available at LLNL, including the picosecond X-ray laser as well as the ALS Femtosecond Phenomena beamline and the SSRL based sub-picosecond photon source (SPPS). These allow the temporal resolution to be improved by 2 orders of magnitudemore » over the current state-of-the-art, which is {approx} 100 ps. Thus, we observed the manifestations of dynamical processes with unprecedented time resolution. Time-resolved x-ray photoemission spectroscopy and x-ray scattering were used to study phase changes in materials with sub-picosecond time resolution. These experiments coupled to multiscale modeling allow us to explore the physics of materials in high laser fields and extreme non-equilibrium states of matter. The ability to characterize the physical and electronic structure of materials under extreme conditions together with state-of-the-art models and computational facilities will catapult LLNL's core competencies into the scientific world arena as well as support its missions of national security and stockpile stewardship.« less
  • New corrosion-resistant, iron-based amorphous metals have been identified from published data or developed through combinatorial synthesis, and tested to determine their relative corrosion resistance. Many of these materials can be applied as coatings with advanced thermal spray technology. Two compositions have corrosion resistance superior to wrought nickel-based Alloy C-22 (UNS No. N06022) in some very aggressive environments, including concentrated calcium-chloride brines at elevated temperature. Two Fe-based amorphous metal formulations have been found that appear to have corrosion resistance comparable to, or better than that of Ni-based Alloy C-22, based on breakdown potential and corrosion rate. Both Cr and Mo providemore » corrosion resistance, B enables glass formation, and Y lowers critical cooling rate (CCR). SAM1651 has yttrium added, and has a nominal critical cooling rate of only 80 Kelvin per second, while SAM2X7 (similar to SAM2X5) has no yttrium, and a relatively high critical cooling rate of 610 Kelvin per second. Both amorphous metal formulations have strengths and weaknesses. SAM1651 (yttrium added) has a low critical cooling rate (CCR), which enables it to be rendered as a completely amorphous thermal spray coating. Unfortunately, it is relatively difficult to atomize, with powders being irregular in shape. This causes the powder to be difficult to pneumatically convey during thermal spray deposition. Gas atomized SAM1651 powder has required cryogenic milling to eliminate irregularities that make flow difficult. SAM2X5 (no yttrium) has a high critical cooling rate, which has caused problems associated with devitrification. SAM2X5 can be gas atomized to produce spherical powders of SAM2X5, which enable more facile thermal spray deposition. The reference material, nickel-based Alloy C-22, is an outstanding corrosion-resistant engineering material. Even so, crevice corrosion has been observed with C-22 in hot sodium chloride environments without buffer or inhibitor. Comparable metallic alloys such as SAM2X5 and SAM1651 may also experience crevice corrosion under sufficiently harsh conditions. Accelerated crevice corrosion tests are now being conducted to intentionally induce crevice corrosion, and to determine those environmental conditions where such localized attack occurs. Such materials are extremely hard, and provide enhanced resistance to abrasion and gouges (stress risers) from backfill operations, and possibly even tunnel boring. The hardness of Type 316L Stainless Steel is approximately 150 VHN, that of Alloy C-22 is approximately 250 VHN, and that of HVOF SAM2X5 ranges from 1100-1300 VHN. These new materials provide a viable coating option for repository engineers. SAM2X5 and SAM1651 coatings can be applied with thermal spray processes without any significant loss of corrosion resistance. Both Alloy C-22 and Type 316L stainless lose their resistance to corrosion during thermal spraying. Containers for the transportation, storage and disposal of spent nuclear fuel (SNF) and high-level radioactive waste (HLW) with corrosion resistant coatings are envisioned. For example, an enhanced multi-purpose container (MPC) could be made with such coatings, leveraging existing experience in the fabrication of such containers. These coating materials could be used to protect the final closure weld on SNF/HLW disposal containers, eliminate need for stress mitigation. Integral drip shield could be produced by directly spraying it onto the disposal container, thereby eliminating the need for an expensive titanium drip shield. In specific areas where crevice corrosion is anticipated, such as the contact point between the disposal container and pallet, HVOF coatings could be used to buildup thickness, thereby selectively adding corrosion life where it is needed. Both SAM2X5 & SAM1651 have high boron content which enable them to absorb neutrons and therefore be used for criticality control in baskets. Alloy C-22 and 316L have no neutron absorber, and cannot be used for such functions. Borated stainless steel and G« less
  • A study was performed that examined the microstructure and mechanical properties of 63Sn-37Pb (wt.%, Sn-Pb) solder joints made to thick film layers on low-temperature co-fired (LTCC) substrates. The thick film layers were combinations of the Dupont{trademark} 4596 (Au-Pt-Pd) conductor and Dupont{trademark} 5742 (Au) conductor, the latter having been deposited between the 4596 layer and LTCC substrate. Single (1x) and triple (3x) thicknesses of the 4596 layer were evaluated. Three footprint sizes were evaluated of the 5742 thick film. The solder joints exhibited excellent solderability of both the copper (Cu) lead and thick film surface. In all test sample configurations, themore » 5742 thick film prevented side wall cracking of the vias. The pull strengths were in the range of 3.4-4.0 lbs, which were only slightly lower than historical values for alumina (Al{sub 2}O{sub 3}) substrates. General (qualitative) observations: (a) The pull strength was maximized when the total number of thick film layers was between two and three. Fewer that two layers did not develop as strong of a bond at the thick film/LTCC interface; more than three layers and of increased footprint area, developed higher residual stresses at the thick film/LTCC interface and in the underlying LTCC material that weakened the joint. (b) Minimizing the area of the weaker 4596/LTCC interface (e.g., larger 5742 area) improved pull strength. Specific observations: (a) In the presence of vias and the need for the 3x 4596 thick film, the preferred 4596:5742 ratio was 1.0:0.5. (b) For those LTCC components that require the 3x 4596 layer, but do not have vias, it is preferred to refrain from using the 5742 layer. (c) In the absence of vias, the highest strength was realized with a 1x thick 5742 layer, a 1x thick 4596 layer, and a footprint ratio of 1.0:1.0.« less
  • This report documents the study that was performed from October 1993 through June 1994 to determine the effects of humidity on the W80 MC3268/3269 Trajectory-Sensing Signal Generators (TSSGs) during the test bed build and laboratory test processes. Mason and Hanger, Silas Mason Co., performs the disassembly and inspections along with the test bed build processes at the Pantex Plant in Amarillo, Texas. The laboratory testing of the TSSGs is performed at Sandia`s Weapons Evaluation Test Laboratory (WETL), located at the Pantex Plant. This report summarizes the historical sequence of events, the engineering analyses and decisions, and the future plans formore » controlling the ingress of moisture into the TSSGS during laboratory testing.« less