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Plasma Surface Engineering
     Santiago Corujeira Gallo


  Universidade de Caxias do Sul
         September 2009
Birmingham - UK




Founded in middle age (7th century)
Population ca 2,500,000
Traditional industrial centre
Cultural diversity

                                      powered by google maps
University of Birmingham
          Founded in 1900


          Research oriented
           Ranked 12th in UK (RAE)


          Multicultural
           over 4000 Intl students
           from 150 countries


          Colleges
           Arts and Law
           Engineering and Physical Sciences
           Life and Environmental Sciences
           Medical and Dental Sciences
           Social Sciences
Surface Engineering Group (2007)
                       Composition of the group:
                         1 Professor
                         1 Senior Lecturer / Reader
                         2 Research fellows
                         1 Visiting research fellow
                         7 PhD students
                         2 MSc students
                         2 Undergraduate students


                       Topics of research:
                        - Plasma diffusion treatments
                        - Thermal oxidation
                        - PVD coatings
                        - Nanoindentation
Active screen plasma surface engineering
of austenitic stainless steel for enhanced
   tribological and corrosion properties

• Austenitic stainless steel

• Plasma surface engineering

• Tribological and corrosion properties

• Active screen
Austenitic stainless steel
• Typical composition: 18% Cr – 8% Ni
• AISI 316: 17% Cr – 12% Ni – 2% Mo


                            Typical properties:
                            • Excellent corrosion resistance
                            • Non-magnetic
                            • No ductile-to-brittle transition
                            • Poor mechanical properties
                            • Low wear resistance
Surface engineering treatments

              Benefits of surface engineering
                • Improved performance
                • Use cheaper materials
                • Increase design flexibility


               Diffusion treatments:
                • No sharp interface - gradient
                • Slow (temperature – time)
Plasma surface engineering
C or N containing gas

                                 Conventional gas nitriding ~ 550oC
   Treated substrate
                                 Conventional gas carburising ~ 950oC


                                                                C or N containing gas
                                                                      at low pressure

                                                           - -
                        Cr23C6
                                                            +

                Cr1-2N                            -
                                                Treated substrate - cathode (-)
GDOES composition depth profiles
XRD - phase identification


                             S-phase
                                or
                             expanded
                             austenite
Micrographs of expanded austenite

                    Typical cross section
                    optical micrograph




Typical top view
SEM micrograph
Microhardness testing
                         Typical instrumented
                         hardness test curves




     Typical load
bearing capacity
Microhardness indents
                          Tough carbon
                          expanded austenite




Brittle nitrogen
expanded austenite
Wear testing




Dry sliding pin-on-disc test, 10 N normal load, WC
  counterpart, 0.03 m/s sliding speed; 4.5 hours
Wear results
AISI 316 UT                  AISI 316 PC
Morphology of the wear tracks


AISI 316 UT         AISI 316 PC
Wear track of AISI 316 UT
Wear track of AISI 316 PC
Wear debris




  Untreated sample: metallic debris       Treated sample: oxide debris


Wear debris       Colour        Size   Magnetic         Possible phases
  Treated      Red / Orange   <20um      No       alpha-Fe2O3     Hematite
Un treated         Black      >20um      Yes        Fe3O4         Magnetite
Wear debris – TEM SAD pattern
Wear conclusions

• The wear resistance of carbon expanded austenite
is 2 orders of magnitude higher than AISI 316 UT

• The wear mechanism changes from adhesive wear
in AISI 316 UT to oxidational wear in AISI 316 PC

• The layer of carbon expanded austenite reduces
the subsurface deformation and supports the
protective oxide layer
Corrosion testing

                Immersion corrosion
                Boiling H2SO4 (16%)
                    1 to 20 hours
Corrosion results
 AISI 316 UT                          AISI 316 PC




After 1 hour immersed in boiling sulphuric acid (16%)
Corrosion mechanisms
Corrosion mechanisms - Schematic
Macrographs of corroded samples
   AISI 316 UT   AISI 316 DCPC   AISI 316 ASPC




                 AISI 316 DCPC   AISI 316 ASPC



Macrographs
“as treated”
Corrosion conclusions

• Carbon expanded austenite exhibits higher corrosion
resistance to boiling sulphuric acid than AISI 316 UT

• The corrosion mechanisms are defect-controlled
(MnS inclusions, slip bands and grain boundaries)

• The AS treated samples performed better than the
DC ones through the elimination of edge effects
Active screen plasma treatments

                             Active Screen experimental
                             setting inside a conventional
                             DC plasma furnace / reactor




Nitriding mechanisms of
Active Screen - schematics
DC and AS plasma reactors
Industrial AS plasma furnace
AS typical treatment cycle
Processing conditions
Benefits of AS treatment
DC – edge effect          DC – arcing damage         AS – feature less




AS –rusty components before ASPN      AS – rusty components after ASPN
Active Screen conclusions

• AS plasma treatments can produce superior
surface quality than DC treatments (no edge effect or
arcing damage)

• AS treatments are less sensitive to the surface
condition of components (rust, oil, etc.)

• AS plasma shows potential to further improve the
results obtained with DC or other plasma treatments
Acknowledgements

This project was sponsored by:

         EU scholarships for Latin America
         Techint group
         The University of Birmingham

         Universidad Tecnológica Nacional
Thank you very much indeed

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Plasma Surface Engineering

  • 1. Plasma Surface Engineering Santiago Corujeira Gallo Universidade de Caxias do Sul September 2009
  • 2. Birmingham - UK Founded in middle age (7th century) Population ca 2,500,000 Traditional industrial centre Cultural diversity powered by google maps
  • 3. University of Birmingham Founded in 1900 Research oriented Ranked 12th in UK (RAE) Multicultural over 4000 Intl students from 150 countries Colleges Arts and Law Engineering and Physical Sciences Life and Environmental Sciences Medical and Dental Sciences Social Sciences
  • 4. Surface Engineering Group (2007) Composition of the group: 1 Professor 1 Senior Lecturer / Reader 2 Research fellows 1 Visiting research fellow 7 PhD students 2 MSc students 2 Undergraduate students Topics of research: - Plasma diffusion treatments - Thermal oxidation - PVD coatings - Nanoindentation
  • 5. Active screen plasma surface engineering of austenitic stainless steel for enhanced tribological and corrosion properties • Austenitic stainless steel • Plasma surface engineering • Tribological and corrosion properties • Active screen
  • 6. Austenitic stainless steel • Typical composition: 18% Cr – 8% Ni • AISI 316: 17% Cr – 12% Ni – 2% Mo Typical properties: • Excellent corrosion resistance • Non-magnetic • No ductile-to-brittle transition • Poor mechanical properties • Low wear resistance
  • 7. Surface engineering treatments Benefits of surface engineering • Improved performance • Use cheaper materials • Increase design flexibility Diffusion treatments: • No sharp interface - gradient • Slow (temperature – time)
  • 8. Plasma surface engineering C or N containing gas Conventional gas nitriding ~ 550oC Treated substrate Conventional gas carburising ~ 950oC C or N containing gas at low pressure - - Cr23C6 + Cr1-2N - Treated substrate - cathode (-)
  • 10. XRD - phase identification S-phase or expanded austenite
  • 11. Micrographs of expanded austenite Typical cross section optical micrograph Typical top view SEM micrograph
  • 12. Microhardness testing Typical instrumented hardness test curves Typical load bearing capacity
  • 13. Microhardness indents Tough carbon expanded austenite Brittle nitrogen expanded austenite
  • 14. Wear testing Dry sliding pin-on-disc test, 10 N normal load, WC counterpart, 0.03 m/s sliding speed; 4.5 hours
  • 15. Wear results AISI 316 UT AISI 316 PC
  • 16. Morphology of the wear tracks AISI 316 UT AISI 316 PC
  • 17. Wear track of AISI 316 UT
  • 18. Wear track of AISI 316 PC
  • 19. Wear debris Untreated sample: metallic debris Treated sample: oxide debris Wear debris Colour Size Magnetic Possible phases Treated Red / Orange <20um No alpha-Fe2O3 Hematite Un treated Black >20um Yes Fe3O4 Magnetite
  • 20. Wear debris – TEM SAD pattern
  • 21. Wear conclusions • The wear resistance of carbon expanded austenite is 2 orders of magnitude higher than AISI 316 UT • The wear mechanism changes from adhesive wear in AISI 316 UT to oxidational wear in AISI 316 PC • The layer of carbon expanded austenite reduces the subsurface deformation and supports the protective oxide layer
  • 22. Corrosion testing Immersion corrosion Boiling H2SO4 (16%) 1 to 20 hours
  • 23. Corrosion results AISI 316 UT AISI 316 PC After 1 hour immersed in boiling sulphuric acid (16%)
  • 26. Macrographs of corroded samples AISI 316 UT AISI 316 DCPC AISI 316 ASPC AISI 316 DCPC AISI 316 ASPC Macrographs “as treated”
  • 27. Corrosion conclusions • Carbon expanded austenite exhibits higher corrosion resistance to boiling sulphuric acid than AISI 316 UT • The corrosion mechanisms are defect-controlled (MnS inclusions, slip bands and grain boundaries) • The AS treated samples performed better than the DC ones through the elimination of edge effects
  • 28. Active screen plasma treatments Active Screen experimental setting inside a conventional DC plasma furnace / reactor Nitriding mechanisms of Active Screen - schematics
  • 29. DC and AS plasma reactors
  • 33. Benefits of AS treatment DC – edge effect DC – arcing damage AS – feature less AS –rusty components before ASPN AS – rusty components after ASPN
  • 34. Active Screen conclusions • AS plasma treatments can produce superior surface quality than DC treatments (no edge effect or arcing damage) • AS treatments are less sensitive to the surface condition of components (rust, oil, etc.) • AS plasma shows potential to further improve the results obtained with DC or other plasma treatments
  • 35. Acknowledgements This project was sponsored by: EU scholarships for Latin America Techint group The University of Birmingham Universidad Tecnológica Nacional
  • 36. Thank you very much indeed