Yufan Xu ​ 1 Ken Flanagan ​ 1 Jason Milhone​ 1 Cary Forest ​ 1 Mike Clark 1 Paul Nonn ​ 1 Steven Hardcastle ​ 2 ​ 1: University of Wisconsin-Madison ​ 2: University of Wisconsin-Milwaukee PIII Sample Group1.0 Analysis

Schematics PCX Chamber N + HV Pulser ECH System Gas Supply Triple Probe Target Sample PIII Probe Plasma Density: cm -3

PCX-U Plasma Density: ~10 11 cm -3 Temperature: e-: 5-10 eV Ion+: eV (1 eV = K) Plasma is made by injecting up to 12 kW of microwaves at torr

Simulation:

Calculation:

Implanting Results The total operating time: 14h 44min ( implantations in 605 shots of plasma) Implantation dose according to the data: e+18 cm -2 Automatically controlled by LabView Executive Loop Cycle: 90 seconds Plasma on: 8 seconds per loop Pulse On-time: 8μs at 60Hz2.323 seconds in total Average Pulsing Current: ~1.4A A few Argon shots prior to the actual implantation to clean the surface. Theoretically, Current density J = A/cm 2 Current = 0.213A Total charge = C That gives total number of ions= e+18 Dose= e+17 cm -2

Voltage & Current Pulse Waveform in Oscilloscope Voltage (yellow)Current ~ 10μs ~ 8μs

Executive Loop Cycle Sample

Testing Procedure Surface Microscopic Observation X-ray Photoelectron Spectroscopy (XPS) Nano-indenting Surface Hardness Testing

Testing Sample Material: Alloy Steel 9310 (Polished and cut) Dimension: Implanting: 1 inch * 7/8 inch * 5/16 inch Testing: 9mm*9mm*8mm Group: Blank & Implanted C%Mn%P%S% Si%Ni%Cr%Mo% max

Surface Microscopic Observation Blank:Implanted: X20X50X20

X-ray Photoelectron Spectroscopy (XPS) data 1 Binding energy C1s 285eV O1s 532eV O2s 25eV Fe 2p3/2 710eV, Fe 2p1/2 723eV, Fe 3S 93eV, 3P 55eV Augers 553, 608, 660eV N1s 400eV Cr 2p3/2 575eV Ar 240eV Fe seems also to have small Auger peaks 408eV and 398eV XPS sputter implanted sample 3 times. For blank sample after 2 min sputter N/Fe ratio From above N is found mostly on top 10 nm. By 24nm very little N implanted. Sputter time(min)~Sputter depth (nm)N/Fe atomic ratioNote Very little C, O Same as blank

Blank vs. Implanted Asis (survey) BlankImplanted

Blank vs. Implanted Asis (local) N 1s BlankImplanted

Blank vs. Implanted Spt 4nm (survey) BlankImplanted

Blank vs. Implanted Spt 4nm (local) N 1s Blank Implanted

Implanted Spt 12nm Survey Local N 1s

Implanted Spt 24nm Surveylocal N 1s

Cr 2p 12nm24nm

Atomic % Charts (Surface 0 nm): Blank Implanted

4 nm BlankImplanted

Implanted 12nm and 24nm 12 nm24nm

Compare to the Previous Research PIII 20keV N in Alloy 9310

Nano-indenting Surface Hardness Testing Agilent G200 Because Nitride layer is too thin 30nm However, we are able to get modulus and hardness of both samples at 30~50nm. It represents the property of the material 9310 itself.

Blank Modulus (GPa) GPa

Blank Hardness (GPa) GPa

Implanted Modulus (GPa) GPa

Implanted Hardness (GPa) GPa

Conclusion The Nitrogen layer implantation was successful but thinner than expected. Need to find a new way to test the hardness if possible. Need larger voltage (>50kV) and higher frequency pulser.