EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 1 Electroformed Nanocrystalline Coatings An Advanced Alternative to Hard-Chrome Electroplating PP-1152 Dr. Maureen J. Psaila-Dombrowski, McDermott Technology, Inc. Douglas E. Lee, Babcock & Wilcox Canada Dr. Jonathan L. McCrea, Integran Technologies Dr. Uwe Erb, University of Toronto HCAT Meeting, Toronto, Ontario September 26, 2002

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 2 Contents  Technical Objective  SERDP Program Overview  Background  Results Since Orlando Meeting  Summary

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 3 Technical Objective  Develop an environmentally benign advanced nanocrystalline Co-based coating technology that:  Is compatible with conventional electroplating infrastructure  Will produce coatings that meet or exceed the overall performance of hard chrome (hardness, wear, fatigue, corrosion, and thermal stability)  Has costs similar to or less than life-cycle cost of existing hard chrome electroplating processes  Will be applied to non-line-of-sight surfaces

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 4 Program Overview Three Phases  Phase ITechnology Viability Assessment  Completed  Phase IICoating Optimization  Completed  Phase IIIExtension to Complex ID Shapes  In Progress

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 5 Program Plan

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 6 Background  Synthesized Co-P, Co-Mo and Co-Fe nano alloys  Synthesized and Optimized Co-Fe,Co-Fe-P, Co-Fe-Zn and Co-Fe-Zn-P nano alloys  Optimized Co-P alloy  Cobalt chloride/ortho-phosphoric/phosphorous acid bath  Plating efficiency >90%  Grain size nm  As-deposited hardness 700 VHN  Deposition rate 2-8 mills/hr  Precipitation hardenable  Good salt spray results  High Taber wear results (CS 17)  Good pin-on-disk results

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 7 Process Cost Initial Study Update

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 8 Results  Process scale-up completed (2L to 50L)  Activation procedure developed for high carbon steel substrates  Adhesion tests performed as per ASTM B  Bend Test for Ductility performed as per ASTM B  Low Temperature Annealing Treatments Performed  191°C anneal shows little increase in hardness  250 ° C anneal (4 hr) increases hardness to ~800 VHN

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 9 Adhesion Test  ASTM B  No peeling and/or flaking of the coating from the substrate under low magnification (4x) - 30% elongation (bending)

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 10 Ductility

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 11 Abrasive Wear (Taber)

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 12 Sliding Wear  Experimental Set-up (Ball-on-Disk)  CSEM Tribometer  Static member - 6mm alumina (Al 2 O 3 ) Ball (1800VHN)  10 N Load  1000 meter total sliding distance  20 mm wear track diameter  10cm/s sliding velocity  Profile measured using stylus profilometer

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 13 Sliding Wear Nano Co~10%P Nano Co~6%P Nano Co~4%P (HT) Nano Co~4%P Nano Co~2%P Nano Cobalt Nanocrystalline Samples Hard Chrome Tool Steel Mild Steel Standard Samples Wear Volume Loss (mm 3 /N/m) x Coefficient of Friction Hardness (VHN) Material

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 14 Sliding Wear

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 15 Fatigue Testing  4340 HCAT specimens acquired from Metcut  Plated by Integran and ground by Metcut  Testing underway at MTI.25”

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 16 Fatigue Test Matrix

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 17 H 2 Embrittlement  ASTM F-519 Type 1a Specimens acquired from Smith & Williston  Plated by Integran  Testing underway at MTI

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 18 Initial H 2 Embrittlement Test Matrix

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 19 Electrochemical Testing  Establish electrochemical behaviour CoEHC plate Ni 200Nano Co-2-3wt%P (4340) Nano CoNano Co-4-5wt%P (4340)  Linear polarization resistance scan (LPR)  Potentiodynamic scan (PDS) per ASTM G61  3.56 wt% NaCl, room temperature  Determine corrosion rate and potential for pitting  Testing in process at MTI

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 20 NLS Application  Mockups designed and fabricated  Blind and through cylinders  Pins  External lugs  Anode design study in progress  Consumable Co electrode  Fixed graphite electrode Optical Micrograph - 13 mil Nano Co 2-3wt%P coating on 1” ID

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 21 Process Data Summary

EPA DOE DoD Strategic Environmental Research and Development Program Improving Mission Readiness Through Environmental Research SERDP Program 1152 DACA72-00-C-003 (9/26/02) 22 Property Data Summary