1. 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

2. 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

3. 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

4. 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

5. 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

6. 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 12-15 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

7. 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

8. 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 B571-91  Bend Test for Ductility performed as per ASTM B489- 85  Low Temperature Annealing Treatments Performed  191°C anneal shows little increase in hardness  250 ° C anneal (4 hr) increases hardness to ~800 VHN

9. 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 B571-97  No peeling and/or flaking of the coating from the substrate under low magnification (4x) - 30% elongation (bending)

10. 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

11. 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)

12. 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

13. 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 6.20.50719Nano Co~10%P 7.10.45733Nano Co~6%P 5.30.441013Nano Co~4%P (HT) 6.40.48745Nano Co~4%P 5.50.53728Nano Co~2%P 10.70.35500Nano Cobalt Nanocrystalline Samples 11.870.701208Hard Chrome 13.10.75250Tool Steel 18.20.73150Mild Steel Standard Samples Wear Volume Loss (mm 3 /N/m) x 10 -6 Coefficient of Friction Hardness (VHN) Material

14. 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

15. 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”

16. 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

17. 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

18. 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

19. 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

20. 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

21. 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

22. 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