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W-Steel Interfacial Bond Strength, & MC-Simulation of IEC He-Implantation. Shahram Sharafat * , with significant contributions from A. Hyoungil, A. Takahashi 1 , J. El-Awady, Q. Hu, J. Qua, G. Romanowski 2 , and N. Ghoniem, and collaborative interactions with
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W-Steel Interfacial Bond Strength, &MC-Simulation of IEC He-Implantation Shahram Sharafat*, with significant contributions from A. Hyoungil, A. Takahashi1, J. El-Awady, Q. Hu, J. Qua, G. Romanowski2, and N. Ghoniem, and collaborative interactions with G. Kulcinski3, R. Radel3, S. Gulobov2, N. Parikh4, and L. Snead2 Mechanical and Aerospace Engineering Department University of California Los Angeles 1 Tokyo University of Science 2 Oak Ridge National Laboratory 3University of Wisconsin – Madison 4University of North Carolina at Chapel Hill 15th High Average Power Laser Workshop General Atomics San Diego, CA Aug. 9 – 10, 2006 *shahrams@ucla.edu This work was supported by the US Navy/Naval Research Laboratories through a grant with UCLA.
OUTLINE • W – Steel Interface Bond Strength • Review HIP’d W-F82H • Report on VPS-W • Monte Carlo Simulation of IEC Results • Issues for Low-Energy He Implantation • Survey of Low-E He Implantation • KMC Simulation Results
Photodiode voltage is used to determine the Displacement profile of the coating surface Al Layer Coating Coating surface velocity is calculated by differentiating the displacement profile Nd:YAG Laser 1064 nm Compression The stress can then be calculated using: s = ½(r c v) Finally, tensile failure stress failure is then evaluated using FEM Tension • Al layer melts and rapidly expands • Launching a compressive stress waves through substrate into film layer • Compressive waves are reflected as tensile waves from free surface • If tensile stress is sufficient interface failure will occur. SiO2 Substrate The Laser Spallation: Determine Interface Bond Strength Density and Elastic Properties of both coating and substrate are required to determine accurate failure stresses
D = 20 mm 1.1 mm W coating ~50 um thick F82H substrate Time: } Interfacial Crack 1050 MPa Bond Strength:Depends on Coating Elastic Properties & Density sbond 450 MPa W (HIP) F82H Since Elastic properties of the coating depend on processing in a statistical manner Predicted interfacial strengths will have statistical variations HIP’d W-F82H Sample (ITER, JAEA) • Hot Isostatic Pressure (HIP) bonded Tungsten to F82H Sample from ITER Development JAEA (Japan) Reported 14th HAPL
TEST MATRIX: VPS W-Coated Steel Samples VPS-W Test Matrix (PPSI/ORNL) • Vacuum Plasma Sprayed (VPS) samples supplied by PPI (S. O’Dell). • W-Coatings were polished to ~50 mm thickness at ORNL(G. Romanoski)
Powder Feed Substrate Plasma Flame Plasma Spray Coating Process • Powder melts in Plasma Flame • Molten droplets are acceleratedtowards substrate • Droplets solidify on substrate • A new layer of molten droplets solidifies Modified from Ghansen Comp. In Phys. COMPUTERS IN PHYSICS, VOL. 12, NO. 1, JAN/FEB 1998
Plasma Spray Coating Process • Powder melts in Plasma Flame • Molten droplets are acceleratedtowards substrate • Droplets solidify on substrate • A new layer of molten droplets solidifies Powder Feed Substrate Plasma Flame Modified from COMPUTERS IN PHYSICS, VOL. 12, NO. 1, JAN/FEB 1998
Plasma Sprayed Micro-composite Thermal Barrier Coatings (TBC)* Al2O3 Al2O3 ZrO2 ZrO2 Substrate – Interface Porosity Pore Pore Interface Pore Interface Pore Substrate 500 X *S. Sharafat, Vacuum 65 (2002) 415 Interface between Substrate & Coating is Porous Simulated Plasma Sprayed Coating Substrate – Interface Porosity Substrate Substrate
Nano-porousVPS-W Deposits1 1S. O’Dell, PPI 2004 Factors Influencing Coating Bond Strengths • Elastic properties of the coating depends on processing: • HIP’ing results in high density (r) high Young’s modulus (E) • Plasma Spray results in low r and low E • Substrate/Coating interface topography: • HIP’ing results in high fraction of interface coverage • Plasma Spray shows reduction of interface coverage • Present analysis based on: • Published VPS-W E*: EVPS = 54 GPa (ESolid= 410 GPa) • Coating Density Range: 80% – 60% • Interface Coverage Range: 100% – 40 % We need coating properties (E, r) and interface topography *Matejicek, 2005; **Estimate
80% Dense W-Coating 60% Dense W-Coating VPS-Sample #02:r= 11,548 kg/m3 E = 27 GPa * ELaser = 160.6 mJ Preliminary Interfacial Strengths of VPS-W VPS-Sample #02:r= 15,397 kg/m3 E = 54 GPa * ELaser = 160.6 mJ VPS-W Coating Delamination Stress*: 140 MPa – 616 MPa HIP-W Interface Cracking Stress** : 450 MPa – 1050 MPa *Based on 3VPS-W samples and uncertain coating material properties and interface topgraphy **Based on 1 HIP-W sample uncertain E.
2 mm HIP (avg.) Example of “Popped”VPS-W Coating 80% Dense Coating No Interface Porosity 60% Dense Coating IP: Interface Porosity VPS-W Coating Failure Example of Complete Coating Delamination VPS-W Coating Surface Bonding of Plasma Sprayed Coating is weaker than that of the HIP’d Coatings: May require development of Interface Layer
Future Work • Elastic properties of coatings need to be measured including: • Densities, Young’s modulus, and Interface Bond Coverage • Determine minimum stress for ONSET of interface cracks in VPS-W (reported results are for complete failure of coatings) • Cross section and micrograph tested VPS samples (# 01, 02, 05) ORNL • Test remaining samples (# 03 – 04 & 06 – 09) • Present/Publish at the TOFE 17(ANS, Nov 13-14, Albuquerque NM)
OUTLINE • W – Steel Interface Bond Strength • HIP’d W-F82H Sample (ITER, JAEA) • VPS W-Steel Sample (PPS/ORNL) • Monte Carlo Simulation of IEC Results • Issues for Low-Energy He-Implantation • Survey of Low-E He Implantation • Simulation Results
Issues for Low-Energy He Implantation • Results can not be explained by conventional rate theory models because pores sizes are too large (X10) and densities are tool low. • Speculations regarding effects of sputtering on surface: • Sputtering increases with decreasing incidence angle (avalanche) • Surface Erosion Via Ion-Sputtering*: From initial ripples morphology to a rough morphology • Surface Temperatures are too low for rapid and large bubble formation (usually occurs above ~0.6 TM; for W: 730 oC ~ 0.26 TM) • Need to measure/calculate the residual trapped Helium. * R. Cuerno, H. A. Makse, S. Tomassone, S. Harrington, and H. E. Stanley, Stochastic Model for Surface Erosion via Ion-Sputtering: Dynamical Evolution from Ripple Morphology to Rough Morphology, Phys. Rev. Lett. 75, 4464-4476 (1995);
OUTLINE • W – Steel Interface Bond Strength • HIP’d W-F82H Sample (ITER, JAEA) • VPS W-Steel Sample (PPS/ORNL) • Monte Carlo Simulation of IEC Results • Issues for Low-Energy He-Implantation • Survey of Low-E He Implantation • Simulation Results
Low Energy He Implantation of Cu* Copper: 30 keV He 1.2-2.4x1016/cm2 annealed 973 K for 1800 s. He range ~130 nm; peak 1.68 at.%. Pinhole Diamavg ~ 150 nm (predicted ~ 14 nm) … surprising result that after annealing at 973 K, 80% of the helium was released and surface pinholes seen, even though the average bubble size predicted from migration and coalescence theory was 14 nm …* *Evans, Nuclear Instruments and Methods in Physics Research B 217 (2004) 276–280
Survey of Low Energy He Implanted Tungsten Survey of Low Energy He Implanted Tungsten
Tungsten 10 – 30 eV Helium (Nishijima, 2004) • Low Energy Helium (~ 10 to 30 eV) on PM Tungsten; high dose 2.6 x 1027 He/m2 X 5000 • Cross section of sample W1 which shows holes or passage to neighboring bubbles. D. Nishijima et al. / Journal of Nuclear Materials 329–333 (2004) 1029–1033
(a) 2mm (b) Tungsten 19 keV Helium (Tokunaga, 2004) • SEM images of surface (a) and cross section (b) taken from the sample irradiated to 3.3 x 1023 He/m2 at the peak temperature of 2600 ℃. • The energy of He is 19 keV. He beam flux and heat flux at the beam center is 2.0 x 1021 He/m2s and 6.0 MW/m2, respectively. Beam duration is 3.0 -3.9 s and interval of beam shot start is 30 s. K. Tokunaga et al. / Journal of Nuclear Materials 329–333 (2004) 757–760
1 mm 1 mm 1 mm IEC Results (Cipiti & Kulcinski, 2004) : 730 °C 2.2x1015 He/cm2-s 30 min. 990 °C 8.8x1015 He/cm2-s 7.5 min. 1160 °C 2.6x1016 He/cm2-s 2.5 min. Steady State: 40 KeV He 510184He/cm2 Temperature Pore Size Pore Density dave ~15 nm dave ~50 nm dave ~150 nm
Pore Diameter vs. Temperature Pore Diameter vs. Time IEC Results (Cipiti & Kulcinski, 2004) : Time to Pore Temperature 730 C 1160 C 150 s 1800 s
OUTLINE • W – Steel Interface Bond Strength • HIP’d W-F82H Sample (ITER, JAEA) • VPS W-Steel Sample (PPS/ORNL) • Monte Carlo Simulation of IEC Results • Issues for Low-Energy He-Implantaion • Survey of Low-E He Implantation • Simulation Results
MC Simulation of IEC He-Implantation • Migration and Coalescence (M&C) of He-bubbles is based on Brownian bubble motion • Initial bubble density and avg. bubble radius from HEROS code • Differentiate between near surface and bulk processes by calculating He-pressure based on: – Ideal gas law (near surface) – Hard-sphere model (bulk material)
InitializeModel Calculate diffusion probability of He-bubble Sum probabilities: Diffusion, Coalescence & Implantation for each He Examine one event (Diffusion of a bubble or Implantation) Jump with constant distance Grow He-bubbles by implantation Check Coalescence tn+1 = tn + Dt Surface diffusion rate MC – Calculation Procedure Diffusion Migration: Bubble diffusion rate Es: Activation energy, 2.5eV* D0: Pre-expon 1.25x10-2cm2/s Coalescence: Instantaneous Equilibrium Size: Growth by Implantation: R: Uniform random number (0:1) *Evans, 2004
Temperature Bubble Density He-Implantation Init. Radius Simulation Volume730 C 10171/cm3 2.2 x 1015 1/cm2-s 0.5 nm 0.2 x 1.0 x 1 mm3 990 C 1015 1/cm3 8.8 x 1015 1/cm2-s 1.0 nm 0.2 x 2.5 x 1 mm31160 C 1014 1/cm3 2.6 x 1016 1/cm2-s 1.5 nm 0.2 x 5.0 x 1 mm3 GaussianDensity Distribution Front View Side View He Helium 40 keV He – W: Range: 1.6 nm Straddle: 0.63 nm 1 mm 0.2 mm KMC Model for the 730 oC IEC Case: Simulation Volume
Helium Evolution of Bubble Size for the 730 oC IEC Case (~2000 s): Front View ( 1 mm) Side View ( 0.2 mm) Bubble Color:Red = Matrix BubbleBlue= Surface Pore
Time Sequence of Pore Evolution (730 oC IEC) 3e-4 s 1.5 s 68 s 383 s 562 s 2000 s
T = 730 oC t = 1800 s 990 oC 450 s 1160 oC 150 s Pore Diameter vs. Time KMC Simulation of ICE Experiments 1 mm 2.5 mm 5 mm
IEC IEC IEC IEC Surface Pore Evolution • KMC simulates the trend of surface pore size and density
Bubble Size Near Surface vs Bulk * • 1000 appm He Implanted in Ni at RT. • Uniform He implantation using degrader Al-foil (28 MeV He) • Annealing time: 0.5 – 1.5 hr Near Surface Abundance of Near Surface Vacancies promotes rapid and large bubble growth Bulk *CHERNIKOV, JNM 1989
Sub-Surface Break-Away Swelling He He Avg. Bubble Radius Surface Pore Formation Sub-Surface Break Away Swelling Contribution • BREAK-AWAY Swelling (very rapid growth of bubbles) occurs at the subsurface • However, because the bubbles bisect the surface the swelling is stopped by venting He. • Time to BREAK-AWAY swelling DECREASES with higher Temps.
Probable Explanation of IEC Results • Abundance of near surface vacancies allow bubbles to grow rapidly to equilibrium size: Large bubbles & low He-pressure • Near the surface, Migration & Coalescence (M&C) plus rapid growth results in super-size bubbles. • Super-large bubbles bisect the surface, thus providing a probable explanation for surface deformation and large subsurface bubbles. • A network of deep interconnecting surface pores is rapidly set up which results in drastic topographical changes of the surface
Abstracts Submitted to TOFE 17 • “Surface Roughening Mechanisms for Tungsten Exposed to Laser, Ion, and X-ray Pulses”Michael Andersen and Nasr M. Ghoniem • “Modeling Space-Time Dependent Helium Bubble Evolution in Tungsten Armor under IFE Conditions”Q. Hu, S. Sharafat, and N. Ghoniem • “Measurement of Interface Bond Strength between Tungsten Coatings and Steel Substrates for HAPL FW Armor”Jaafar El-Awady, Jennifer Quang, Shahram Sharafat, and Nasr Ghoniem • “MC Simulation of Tungsten Surface Pores Formed by Low-Energy Helium Implantation”Akiyuki Takahashi, Shahram Sharafat, Nasr Ghoniem, J. Kulcinski, and R. Radel
VPS Interface Bond Strengths *Matejicek, 2005; **Estimated EW = 410 GPa No Interface Pores r = 15,397 kg/m3 EW = 54 GPa No Interface Pores r = 15,397 kg/m3
Laser Energy HIP Coating:1050 mJ to Onset of Failure 2.00 1.50 1.00 0.50 0 Compr. Stress to Failure (GPa) VPS Coating:167 mJ to Complete Delamination Example of Complete Coating Delamination VPS-W Coating Failure VPS-W Coating Surface 2 mm Example of “Popped”VPS-W Coating Bonding of Plasma Sprayed Coating is weaker than that of the HIP’d Coating
Plasma Sprayed Tungsten Coating Material Properties • H. You, T. Hoschen, S. Lindig, “Determination of elastic modulus and residual stress of plasma-sprayed tungsten coating on steel substrate,” J. Nucl. Mater. 348 (2006) 94–101 • Jirı Matejıcek ,Yoshie Koza, Vladimır Weinzettl, “Plasma sprayed tungsten-based coatings and their performance under fusion relevant conditions,” Fus. Eng. Des. 75–79 (2005) 395–399 • “The aim of this work is to measure Youngs modulus of a plasma-sprayed thick porous tungsten coating deposited on a steel (F82H) substrate.” [1]
Low Energy He on W Experiments: Nishijima(2004) Tokitani (2005) Iwakiri (2003) Tokunaga (2003)
GOAL of STUDY • IEC implants Low-Energy (<110 keV) Helium in Tungsten • All forms of W examined at 730 °C - 1150 °C showed extensive surface deformation (EHe: 30-40 keV). • Both, steady state or pulsed operation show deformation: • Steady state @ 6 mA ≈ 1014/cm2s; • Pulsed mode @ 10Hz, 1 ms, 60 mA ≈ 1013/cm2 per pulse OBJECTIVES: • Provide a potential explanation for the development of MASSIVE Surface Pores (~10 X predicted He-bubble size). • If possible, provide mitigating measures against these MASSIVE surface deformations.
SEM image (High temp./Low fluence) 2μm 20mm Slide from: K. Tokunagaa ICFRM-11, Dec. 7-12, 2003, Kyoto, Japan For HAPL: R=6.5m Chamber: ~8x1022He/m2/day ~2600℃、1.7x 1022 He/m2 3.5s/30s( 8S) 18.7 keV, 6.7x 1020 He/m2s WF-6(20x20x0.1mm) • The color of surface becomes to be white from metallic sliver color by the irradiation up to ~1022 He/m2. • Fine uneven morphology and small holes are observed on the surface.
SEM image (High temp./High fluence) ~2600℃、 3.3x 1023 He/m2 3.5s/30s( 145S) 18.7 keV, 6.7x 1020 He/m2s WF-2(20x20x0.1mm) Slide from: K. Tokunagaa ICFRM-11, Dec. 7-12, 2003, Kyoto, Japan For HAPL: 3.3x1023 He/m2 in ~4.5 day 2μm 20mm • When fluence is beyond ~1023 He/m2, the color of surface becomes to be black • The surface is modified resulting in a fine uneven morphology and holes with a diameter of about 50 nm are observed on the surface. 1μm
SEM image of cross section Surface 20μm 1μm ~2600℃、3.3x 1023 He/m2 3.5s/30s( 145S), 18.7 keV, 6.7x 1020 He/m2s, WF-2(20x20x0.1mm) K. Tokunagaa ICFRM-11 Dec. 7-12, 2003 Kyoto Japan • Grain growth by re-crystallization occurs. • Many horn-like protuberances with a width of about 300 nm and a length of about 1 μm are observed at the surface. In addition, He bubbles with a diameter of about 50 -500 nm are observed near surface. • The surface modification is considered to be formed by the He bubbles and their coalescence, the migration of He bubbles near surface.
Low E-He on Copper UKAEA FUS 499 EURATOM/UKAEA Fusion Kinetics of bubble growth and point defect migration in metals J.H. Evans October 2003
Low E-He on Copper (Evans, 2004) Evans, Nuclear Instruments and Methods in Physics Research B 217 (2004) 276–280
New HEROs code gives information about pore sizes: R ~ 100 nm R ~ 50 nm R ~ 16 nm
Bubble Density …(corrected!) 4E15 5E14 6E13