Mechanical, structural and tribological characterisation of high nickel content alloys before and after arc activated plasma nitriding

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Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding

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<ul><li> 1. Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding aintech@ain.es Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding</li></ul><p> 2. Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding J. Fernndez, E. Almandoz, J. Arrikaberri, S. Kulkarni, J. F. Palacio, G.G. Fuentes, J.A. Garca, R. Rodrguez AIN Asociacin de la Industria Navarra, SpainIVC-19 / ICN+T 2013 and partner conferences 9th 13th September 2013, Paris (France) 3. Outline 1. Introduction 2. Objectives 3. Methodology 4. Characterization: Results and discussion 5. Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 3 4. Outline1.Introduction 2. Objectives 3. Methodology 4. Characterization: Results and discussion 5. Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 4 5. The alloys under study 1) Maraging Grade 300, which belongs to the group of maraging steels with 18% Ni and Co containing. C (%)Ni (%)Co (%)Mo (%)Ti (%)Al (%)Fe (%)Specified&lt; 0.0317-198.5-9.54.7-5.20.6-0.7&lt; 0.15BalanceMeasured0.00817.319.055.100.660.11BalanceChemical composition of Maraging Grade 300Samples 30.3 0.2 HRc after quenching at 820 C during 1 h 52.1 0.2 HRc after aging at 485 C during 3h Dimensions: = 35 mm; thickness = 5 mm Grinded and polished to Ra ~ 10 nm Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 5 6. The alloys under study 2) INCONEL alloy 600, which belongs to the group of nickel superalloys. C (%)Cr (%)Fe (%)Mn (%)Si (%)Cu (%)S (%)Ni (%)Specified&lt; 0.1514-176-101 0.50 0.50 0.015BalanceMeasured0.1216.39.10.540.430.320.011BalanceChemical composition of INCONEL alloy 600Samples 17.0 0.2 HRc Dimensions: = 40 mm; thickness = 5 mm Grinded and polished to Ra ~ 10 nmMechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 6 7. The alloys under study 3) INCONEL alloy 718, which belongs to the group of nickel superalloys. C (%)Cr (%)Fe (%)Mo (%)Ti (%)Al (%)Si (%)B (%)Specified 0.008017-21172.8-3.30.65-1.150.20-0.80 0.350.0060Measured0.00617.617.12.90.960.550.300.002Co (%)Cu (%)Mn (%)Nb (%)P (%)S (%)Ni (%)Specified 1.0 0.30 0.354.75-5.5 0.015 0.015BalanceMeasured0.750.220.265.10.0090.012BalanceChemical composition of INCONEL alloy 718Samples 41.8 0.8 HRc Dimensions: = 40 mm; thickness = 4 mm Grinded and polished to Ra ~ 10 nm Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 7 8. Outline 1. Introduction2.Objectives 3. Methodology 4. Characterization: Results and discussion 5. Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 8 9. Objectives Study the mechanical, structural and tribological properties of high nickel content alloys before and after an arc activated plasma nitriding process.What for? Increasing the superficial hardness Increasing the wear resistance (room &amp; high temperature) Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 9 10. Outline 1. Introduction 2. Objectives3.Methodology 4. Characterization: Results and discussion 5. Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 10 11. Arc activated plasma nitridingSpanish patent: ES 2 344 981 B1 in 2011 and European patent EP 2 369 028 B1 in 2013.1: Reactor 2: Samples 3: Electric arc discharge units 4: Heat source 5: Sample holder 6: Electron collector (anode) - 6.1: Electric field concentrator spirals 7: Gas inlet 8: Vacuum system 9: Pulsed DC current source 10: DC current source 11: DC power systemMechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 11 12. Arc activated plasma nitriding StepseIonized gas - N + Ar (+H ) e 2 2+ +e-+Vacuum: 5x10-3 Pa Pre-heating: 350 C Cleaning: Ar Nitriding: 1 Pa, 425 C, 60 min 90 sccm N2 &amp; Ar Cooling downPVD scheme Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 12 13. Arc activated plasma nitriding Characteristics High ionization rate Low pressureBenefits High ratio of active specimens Versatility for future treatments (DUPLEX treatments: nitriding + PVD, nitriding + oxidation) No formation of white layerLabelling MaterialNitridedMaraging 300MAR-3MAR-3NINCONEL 600 METAPLAS PVD MZR 323 equipmentUntreated INC-6INC-6NINCONEL 718INC-7INC-7NMechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 13 14. Outline 1. Introduction 2. Objectives 3. Methodology4. Characterization: Results and discussion 5. Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 14 15. Chemical analysis: GD-OES 70MAR-3NC Fe Mo N O Ti Co Ni60Atomic %50 40 30 20 10INC-6NINC-7N0 370C Cr Fe N O Si Ni Cu Mn60 50Atomic %640 30 20912Depth (microns)15 7018Al C Cr Fe Mo N O Ti Co Ni60 50Atomic %040 30 20 101000 0123Depth (microns)45012345Depth (microns)Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 15 16. Chemical analysis: GD-OES Nitrogen profiles MAR-3N1218INC-6N INC-7N16 14N (atomic %)N (atomic %)10 8 6 412 10 8 6 4220 024681012Depth(microns)141618200 0,00,51,01,52,02,5Depth (microns) MAR-3N shows longer profiles with less nitrogen concentration than INCONEL alloys, and a longer diffusion zone. Both INCONEL alloys show very similar nitrogen profile, with a plateau of ~ 14-15% of nitrogen content, that decreases drastically . Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 163,0 17. Microscopy: SEM of the fracture MAR-3INC-6INC-7MAR-3NINC-6NINC-7NMechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 17 18. Mechanical properties (Nanoindentation) Test parameters 10 x10 indents, 25 m space between indents Decreasing Loads from 10 mN to 100 N (in 100N steps) Loading rate constant Berkovich Tip radius (150 nm) E and H Oliver and Pharr MethodHYSITRON nanoindenter TI950Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 18 19. Mechanical properties (Nanoindentation) REFERENCES (Non nitrided samples): MAR-3, INC-6 &amp; INC-7 Er values between 150 GPa and 200 GPa for all the samples. MAR-3 INC-6 INC-7H values of ~ 10 GPa for MAR-3 and INC-7 and of ~ 7 GPa for INC-6. Sample MAR-352.1 0.2INC-617.0 0.2INC-7MAR-3 INC-6 INC-7HRc41.8 0.8Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 19 20. Mechanical properties (Nanoindentation) MAR-3 &amp; MAR-3NMAR-3N MAR-3Slightly lower Er compared to the as received MAR-3. Increase of hardness by 40%, especially at higher loads.MAR-3N MAR-3Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 20 21. Mechanical properties (Nanoindentation) INC-6 &amp; INC-6NSimilar Red. Modulus. INC-6N INC-6Dramatic increase of superficial hardness (more than x2) with respect to the as received INC-6.INC-6N INC-6Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 21 22. Mechanical properties (Nanoindentation) INC-7 &amp; INC-7NSimilar Red. Modulus INC-7N INC-7Dramatic increase of hardness (x2) with respect to the as received INC-7, especially at higher loads.INC-7N INC-7Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 22 23. XRD analysis MAR-3 &amp; MAR-3NCr K ( = 2.29110 ) BB, 40 KV, 30 mA Room T, 0.02 step, 0.5 s/stepThere is no austenitic phase 43.64, 50.76 &amp; 74.58 for (111), (200) &amp; (220).Fe3NFe4NFe- (101)a.u.Peaks of Fe4N, FeNi3N, Fe3N and Fe3NiN are observed.*MAR-3 MAR-3N40506070Fe3NXRD test conditionsFe- (200)80901001101202 Theta *K. Shetty, S. Kumar, P. Raghothama Rao, Surface &amp; Coatings Technol., 203 (2009) 1530-1536Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 23 24. XRD analysis INC-7 &amp; INC-7N (111)u.a. 5055606570758085905055602 Theta (2 0 0)INC-7 INC-7N (2 0 0)CrN (2 0 0) (1 1 1)INC-6 INC-6N (2 0 0)Fe4N (111)a.u. (1 1 1)INC-6 &amp; INC-6N6570758085902 Theta phase is observed in the as received samples, whereas in the nitrided samples a mixture of and N phases is present*. Fe4N is also formed in INC-6N and CrN is observed in INC-7N. *S. Chollet et al., Surface &amp; Coatings Technol., (2013) In press.Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 24 25. Wear (Room T) K wear at room temperaturePin-on-disc configuration Counter ball: alumina; = 6 mm 20000 cycles, 2N, 10 cm/s R = 7, 9 and 11 mm18-143m /Nm15Kwear x10Wear test conditions12Sample MAR-3MAR-3 MAR-3N INC-6 INC-6N INC-7 INC-7N0.099 0.008INC-70,1 0,014 4INC-6N32.6 0.2INC-663.8 0.5MAR-3N9Kwear x10-14 m3/Nm17 2INC-7N0.094 0.010SampleNitrided maraging does not show an improvement on wear resistance whereas both nitrided INCONEL alloys show an improvement of 2 orders of magnitude compared to their respective non-treated samples. Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 25 26. Wear and COF (RT) MAR-3MAR-3NWear test conditions Pin-on-disc configuration Counter ball: alumina; = 6 mm 20000 cycles, 2N, 10 cm/s R = 7, 9 and 11 mmINC-6INC-6N Sample MAR-30.85 0.05INC-60.84 0.06INC-6N0.86 0.06INC-70.67 0.07INC-7NINC-7N0.92 0.07MAR-3NINC-7COF0.66 0.04Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 26 27. Wear and COF (RT) MAR-3INC-6500 m500 mMAR-3NINC-7INC-7NINC-6N500 m500 m500 mMechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding500 mPage 27 28. Wear (at 450 C) 16Wear test conditions Pin-on-disc configuration Counter ball: alumina; = 6 mm 20000 cycles, 2N, 10 cm/s10 8Kwear x10312-14m /Nm146 4 2 0MAR-3NINC-6INC-6NINC-7INC-7NMAR-310.5 1.0MAR-3N13.2 1.0 8.2 3.8 3.1 0.3INC-78.1 2.0INC-7NMAR-3Kwear x10-14 m3/NmINC-6NSampleSampleINC-6MAR-3 MAR-3N INC-6 INC-6N INC-7 INC-7N2.7 0.5Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 28 29. Wear (at 450 C) MAR-3MAR-3NWear test conditions Pin-on-disc configuration Counter ball: alumina; = 6 mm 20000 cycles, 2N, 10 cm/sINC-6INC-6N MAR-3N shows no improvement compared to the non treated MAR-3INC-7INC-7NNitrided INCONEL alloys show a slight improvement.Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 29 30. On going work 18INC-714N (atomic %)When comparing with other processes (longer time, higher temperature):500 C, 1,5 h 480 C, 1,5 h INC-7N1612 10 8 6 4 2 0 480 C 1.5h 500 C 1.5h012345678Depth (microns)Nanoindentation results are similar at high loads, despite the thicker nitrided layers of the above mentioned processes. Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma Nitriding500 C, 1,5h 480 C, 1,5h INC-7N INC-7Page 30 31. On going work MAR-3MAR-3N 500 C -1.5h 480 C -1.5hSampleKwear x10-14 m3/Nm at RTMAR-33.8 0.5MAR-3N2.6 0.2480 C-1.5h1.4 0.5500 C-1.5hKwear x10-14 m3/Nm at 450 CMAR-310.5 1.0MAR-3N13.2 1.0480 C-1.5h8.1 0.8500 C-1.5h7.9 0.515 10 52.1 0.3SampleN (atomic %)200 01020304050607080Depth (microns)When comparing with other processes (longer time, higher temperature): 480 C 1.5h 500 C 1.5h Longer profiles with higher nitrogen concentration in the surface are obtained. Tribological tests show a slight improvement on wear resistance.Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 31 32. Outline 1. Introduction 2. Objectives 3. Methodology 4. Characterization: Results and discussion5.Summary 6. Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 32 33. Summary Arc activated plasma nitriding processes have been carried out for the nitriding of a series of high nickel content alloys (Maraging 300, INCONEL 600 and INCONEL 718). Chemical, mechanical, microstructural and tribological analysis of the non treated and nitrided samples has been done. Maraging steel 300 has shown long nitriding profiles. The formation of Fe nitrides explains the superficial hardness increase. INCONEL alloys 600 and 718 have shown short nitrogen profiles but with nitrogen concentrations up to 14-15%. The formation of N phase and Fe4N (INC-6N) and CrN (INC-7N) compounds permits to improve wear resistance of both alloys 2 order of magnitude at room temperature. Longer and higher nitrogen profiles are possible to obtain when varying different process parameters (temperature, time,) Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 33 34. Outline 1. Introduction 2. Objectives 3. Methodology 4. Characterization: Results and discussion 5. Summary6.Future work 7. Acknowledgments Mechanical, Structural and Tribological Characterisation of High Nickel Content Alloys before and after Arc Activated Plasma NitridingPage 34 35. Future workCharacterization of corrosion propertie...</p>