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Title: Electroless Plated Nanodiamond Coating for Stainless Steel Passivation

Tritium gas sample bottles and manifold components require passivation surface treatments to minimize the interaction of the hydrogen isotopes with surface contamination on the stainless steel containment materials. This document summarizes the effort to evaluate electroless plated nanodiamond coatings as a passivation layer for stainless steel. In this work, we developed an electroless nanodiamond (ND)-copper (Cu) coating process to deposit ND on stainless steel parts with the diamond loadings of 0%, 25% and 50% v/v in a Cu matrix. The coated Conflat Flanged Vessel Assemblies (CFVAs) were evaluated on surface morphology, composition, ND distribution, residual hydrogen release, and surface reactivity with deuterium. For as-received Cu and ND-Cu coated CFVAs, hydrogen off-gassing is rapid, and the off-gas rates of H2 was one to two orders of magnitude higher than that for both untreated and electropolished stainless steel CFVAs, and hydrogen and deuterium reacted to form HD as well. These results indicated that residual H2 was entrapped in the Cu and ND-Cu coated CFVAs during the coating process, and moisture was adsorbed on the surface, and ND and/or Cu might facilitate catalytic isotope exchange reaction for HD formation. However, hydrocarbons (i.e., CH3) did not form, and did not appear to be anmore » issue for the Cu and ND-Cu coated CFVAs. After vacuum heating, residual H2 and adsorbed H2O in the Cu and ND-Cu coated CFVAs were dramatically reduced. The H2 off-gassing rate after the vacuum treatment of Cu and 50% ND-Cu coated CFVAs was on the level of 10-14 l mbar/s cm2, while H2O off-gas rate was on the level of 10-15 l mbar/s cm2, consistent with the untreated or electropolished stainless steel CFVA, but the HD formation remained. The Restek EP bottle was used as a reference for this work. The Restek Electro-Polished (EP) bottle and their SilTek coated bottles tested under a different research project exhibited very little hydrogen off-gassing and unmeasurable HD formation. ND and Cu were initially chosen to develop improved passivation technology, because Cu has a lower permeability of hydrogen, and diamond is more inert than other materials under a hydrogen atmosphere. However, our tests demonstrated that even after an 8-18 day vacuum extraction heat treatment, the electroless plated Cu and ND-Cu coated stainless steel CFVAs exhibited H2 off-gassing rates that were just comparable to those for the untreated or electropolished stainless steel CFVA, and the HD formation was still observed. Thus, the Restek Electro-Polished (EP) bottle outperformed the electroless plated Cu and ND-Cu coated stainless steel CFVAs, and the electroless plated nanodiamond coating is not promising as a surface passivation technology. However, the ND-Cu coating may be beneficial to another application in which catalyzing the H2-D2 exchange reaction is desired.« less
Authors:
 [1] ;  [1] ;  [1] ;  [1]
  1. Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)
Publication Date:
OSTI Identifier:
1332672
Report Number(s):
SRNL--STI-2016-00420
TRN: US1700735
DOE Contract Number:
AC09-08SR22470
Resource Type:
Technical Report
Research Org:
Savannah River Site (SRS), Aiken, SC (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 42 ENGINEERING; 08 HYDROGEN; STAINLESS STEELS; TRITIUM; HYDROGEN; PASSIVATION; ELECTROPOLISHING; ISOTOPIC EXCHANGE; SURFACE TREATMENTS; CONTAINERS; CHEMICAL REACTIONS; NANOMATERIALS; DIAMONDS; COPPER; HYDROGEN DEUTERIDE; COMPARATIVE EVALUATIONS; PLATING; DEUTERIUM; FLANGES; DEGASSING