PHASE FORMANTION AFTER NITRIDING OF AUSTENITIC STAINLESS STEEL BY PULSED LEII
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1 PHASE FORMANTION AFTER NITRIDING OF AUSTENITIC STAINLESS STEEL BY PULSED LEII D. Manova, J.W. Gerlach, S. Mändl, H. Neumann e for Surface Modification, Leipzig, Germany 1
2 Table of Content Motivation Experiment LEII + electronic beam switch Results phase formation, lattice expansion, FWHM Vegard s low? influence of ion energy influence of duty cycle / ion current density Conclusion 2
3 State of Art Nitriding of austenitic stainless steel hard and wear resistant surface no compromised corrosion resistance large field of applications: food, oil, textile, automotive Phase formation solid solution of nitrogen up to 38 at. %, expanded phase anisotropic lattice expansion normal to the surface of up to 8.5% and 12 % for (111) and (200) oriented grains, respectively broad expanded XRD peaks with FWHM of PIII vs. LEII treatment of 3D samples in PIII PIII: high voltage up to 20 kv, bias on substrate LEII: low voltage < 2 kv, high current, high sputtering experience in PIII and d.c. LEII for > 10 years Idea pulsed LEII reduced sputtering, roughness, but additional heating necessary 3
4 Experiment Concept of electronic beam switch: decoupling of plasma generation & ion flux at fixed extraction voltage by temporal switching electrostatic potential of ion optics Beam switch parameters: 2 A, 2 kv, frequency khz, PLM 2 98% Additional external heating to decouple ion flux from thermal balance: fast control loop necessary J. Dienelt, K. Zimmer, F. Scholze, B. Dathe, H. Neumann, Plasma Source Sci. Technol. 12 (2003) 489. Phase formation depending on process? 4
5 Experiment Heater Gas Supply (N 2 ) Vacuum Chamber Ion beam Sample Holder Low Energy Implantation ECR ion source Plasma Excitation MW Power Base pressure Working pressure Ø 125 mm 2.45 GHz 300 W Pa 2 (6) 10-2 Pa, Beam switch 1 khz, 30% PLM, 300 µs Ion energy kev Beam switch 1 khz, 5 100% PLM Ion energy 0.8 kev Pyrometer Ground Potential Pump Analysis methods: XRD phase formation GDOS depth elemental distribution Temperature Process time 455 C (calibrated pyrometer) 90 min Substrate /304 (X5CrNi18.10) External heating, rotation of sample holder, variation in incidence angle, 5
6 Phase Formation LEI, 1 khz, 30% PLM, 455 C, 90 min Expanded austenite formed for all ion energies Intensity (a.u.) γ(111) γ N (111) γ N (200) γ(200) 1.1 kev PIII 350 C 1.4 kev 1.7 kev 2.0 kev austenite CrN Similar lattice expansion, independent of ion energy Very narrow peaks for expanded austenite No formation of CrN indicating no compromised corrosion resistance Corrosion resistance proved by corrosion test for 24 hours at 40 C in 3% NaCl Angle 2θ ( ) Hardness 15 GPa, (excellent value) 6
7 Lattice Expansion LEI, 1 khz, 30% PLM, 455 C, 90 min Lattice expansion (%) (111) lattice plane Lattice expansion (%) (200) lattice plane 0 1,0 1,2 1,4 1,6 1,8 2,0 Ion Ehergy (kev) 0 1,0 1,2 1,4 1,6 1,8 2,0 Ion Energy (kev) Lattice expansion calculated from simulation of the measured XRD peaks using commercial software Very small variation in expansion for both (111) and (200) lattice planes Values of ~ 6% and ~ 8% for (111) and (200) lattice plane Lattice expansion independent of ion energy 7
8 Phase Structure LEI, 1 khz, 30% PLM, 455 C, 90 min 1,5 1,5 FWHM (deg) 1,0 0,5 base material FWHM (deg) 1,0 0,5 FWHM (200) FWHM (111) 0,0 1,0 1,2 1,4 1,6 1,8 2,0 Ion Energy (kev) 0,0 1,0 1,2 1,4 1,6 1,8 2,0 Ion Energy (kev) FWHM of base material ~ 0.6 ; FWHM of expanded austenite by PIII ~ 2.5 Very narrow peaks for expanded phase, comparable with base material Negligible influence of ion energy on FWHM of expanded peaks FWHM of expanded peaks ~ 1 and ~ 0.7 for (111) and (200) planes, respectively 8
9 Phase Formation LEI, 1 khz, 0.8 kev, 455 C, 90 min Intensity (a.u.) % 25 % 10 % 30 % 15 % 50 % 20 % 100 % austenite CrN ferrite Working pressure Pa Expanded austenite formed for all PLM Increased lattice expansion with increasing of PLM 15% Saturation observed for PLM > 15% 30 Very narrow symmetrical peaks for expanded austenite Angle 2θ (deg) No formation of other phases Hardness 15 GPa 9
10 Phase Formation Intensity (a.u.) LEI, 1 khz, 0.8 kev, 455 C, 90 min Angle 2θ (deg) 5 % 25 % 10 % 30 % 15 % 50 % 20 % 100 % austenite CrN ferrite Working pressure Pa Expanded austenite formed for all PLM for higher working pressure Increased lattice expansion with increasing of PLM 15% Again, saturation observed for PLM > 15% Very narrow symmetrical peaks for expanded austenite No other phases observed Hardness 15 GPa 10
11 Lattice Expansion LEI, 1 khz, 0.8 kev, 455 C, 90 min low pressure high pressure Lattice expansion (%) (111) (200) Lattice expansion (%) (111) (200) PLM (%) PLM (%) Increased lattice expansion with PLM up to 15% for both working pressures Similar behaviour for (111) and (200) lattice plane Saturation observed for PLM > 15% for both working pressure No influence of working pressure on the lattice expansion 11
12 Phase Structure LEI, 1 khz, 0.8 kev, 455 C, 90 min FWHM (deg) 1,5 1,0 0,5 (111) low pressure high pressure base material Intensity (a.u.) kv austenite 1.7 kv CrN 1.4 kv Ferrit 1.1 kv base material 0, PLM (%) Angle θ/2θ ( ) Very narrow expanded peaks with FWHM of about 0.9 for (111) plane Negligible influence of PLM on the FWHM for (111) and (200) lattice plane Most probably influence of the additional to the beam heating No influence of working pressure on the values of FWHM 12
13 Expansion vs. Concentration Gitterkonstante (A) 4, , ,50 4, ,25 Vegard's law (lattice constant linear in fraction) Retger's law (unit cell linear in fraction) Approximation of Vegard's law for low N content LP g-fe Nitriding (200) of thin foil LP (111) HP PVD FeN (200) (NaCl) deposition octaeder HP of "SS-N" (111) sites FeN (ZnS) tetraeder sites ,00 3, ,75 3, , , , , ,6 0, ,8 0, ,0 Stickstoffgehalt [x]: FeN x Nitrogen concentration measured by GDOS No direct correlations observed for all nitrided samples Nitrogen amount in expanded phase should not be calculated from the lattice expansion Independent methods as GDOS or RBS are required for determining the nitrogen content in nitrided austenitic steel 13
14 Depth Profiles Nitrogen concentration (at.%) LEI, 1 khz, 0.8 kev, 455 C, 90 min PLM 5%, LP: low expansion PLM 30%, LP: high expansion Depth (µm) Nitrogen depth profiles obtained from GDOS measurements Nearly typical erfcdiffusion profile for PLM 5%: single curvature, perhaps hint of kink Plateau followed by tail for PLM 30%: turning point in curve near 3.25 µm Additionally, good corrosion resistance only observed for PLM 30%. 14
15 Conclusions No influence of ion energy or PLM on the phase formation during nitriding of austenitic stainless steel Use of Vegard s low to determine nitrogen content from lattice expansion can lead to wrong results: independent concentration/expansion values not rarely found in literature Formation of expanded phase not influenced by pulsed mode: no difference 300 nm between pulsed low energy implantation, d.c. low energy implantation and 300 nm PIII results of pulsed LEI identical to alternatives preferable method for industrial applications 2 min 4 min 6 min However: reduced ion bombardment + additional heating has other consequences (PLM 100% is also with heating!) o better surface quality, less sputtering, thicker layers, high hardness o threshold in nitrogen flux necessary to obtain typical depth profiles o less peak broadening in XRD influence on stress distribution? influence on stress corrosion cracking in modified surfaces? influence on Cr diffusion? 15
16 Transfer to Industry LEI Chamber 16
17 Acknowledgments Frank Scholze, Ronny Woyciechowski, Johanna Lutz European Fund for Regional Development (EFRE) & Free State of Saxony (project 12613/2085) German Federation of Industrial Research Associations (AiF, project KF FK7) 17
18 Mechanical and electrical parameter Faraday Cup Array probe diameter : 3,2 mm number of probes : 256 (16x16) distance between two probes : 11 mm (vertical), 19 mm (horizontal) measurement area : 200 x 300 mm 2 sampling rate : ~10 measurements per second graphic program array measurements allow a short beam profile snap shot and are useful for determination of the influence of electric and gas parameter on broad beam profile of ion sources 18
19 256 Probe Faraday Cup Array Ceramics Baseplate 256 Probe Array GraphiteProbes Graphite Ground Shielding Electronics Electronics 19
20 Screenshot of the Special Software 20
21 Phase Formation Different treatments with and without external heating kv austenite 1,7 kv CrN 1,4 kv Ferrit 1,1 kv LEI base material PIII Intensity (a.u.) Angle θ/2θ ( ) 21
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