5 Parameter analysis of Modified 316 LN Stainless steel

By: Nicholas Bembridge1

Advisors: Dr Anthony Rollett2 & Dr Peter Kalu1

PhD Researchers: Mohammed Alvi2 Jason Gruber2 & Steven Downey1
(1)FAMU FSU College of Engineering (2) Carnegie Mellon University

Long term Goal

The long term goal of this research is to examine the microstructure and texture changes caused by heat treatment of modified 316LN stainless steel.

Current Goals
Examine grain boundary character distribution in M316LN stainless steel. Determine grain size and twin density with sufficient statistical confidence.

Background

Currently Modified 316 LN Stainless steel is used as a superconducting wire conduit in the 45 Tesla Hybrid Magnet System at the National High Magnetic Field Laboratory.

Conduit Processing
Annealed, Cold rolled As Received Cold worked
Jacket Formation (forming & welding) Magnet coil winding

Nb3Sn reaction Heat Treatment (100hrs at 700oC)

Produces superconductor from Cu-Nb wires and Tin Primary Selection Criteria for material use

Heat treatment Cu/Nb3Sn Superconductors

Cu-NB wires with thin layer of Sn

Material
Element
Chromium Nickel Molybdenum Manganese Silicon Nitrogen Carbon Niobium

316 LN Wt.% Modified 316LN* Wt%

16.00-18.00 10.00-14.00 2-3 2 max .750 max .130-.180 .03 max No spec. 17.22 13.26 2.06 1.51 .750 .147 .005 .08

Grain Boundary Character

Why do we need 5 parameters? - Describing a grain boundary requires a misorientation (3 parameters) and a normal (2 parameters). Why might the 5 parameter distributions be interesting? - This material has a high density of twins, so we would like to know if the twins are all coherent twins; also we would like to know if any other boundary types are favored
GBCD = Grain Boundary Character Distribution

Experimental Procedure
As received M316LN samples were furnace annealed in argon atmosphere at 700o C for varying lengths of time and water quenched.
*Received in cold rolled and annealed condition.

O.I.M. analysis done with Phillips XL-40 FEG SEM Orientation Imaging Microscope and TSL software. Between 300x300 and 350x350 micron scan area. 0.5 micron step size for good resolution.

OIM Overview
Electron diffraction gives grain orientation. Orientations are measured point by point across the samples surface.
1 1

3
2 2

Results
OIM IPF Maps Twin density data Grain size data Plots of GBCD for as-received, and comparison of as-received with 50 hours anneal

IPF Maps
IPF Map Legend

As Received

100 Hour

Texture is weak, therefore sample suitable for GBCD analysis

Twin density data

Typical twinned grain
Twin Fraction VS Annealing Time
0.5 0.45 0.4 0.35

Twin Fraction

0.3 0.25 0.2 0.15 0.1 0.05 0 -10 10 30 50 70 90 110 Annealing Tim e (hours)

Typical twin

Grain size data

Grain Diameter With Twins VS Annealing Time
7 6

Grain Diameter (microns)

5 4 3 2 1 0 -10 10 30 50 70 90 110 Annealing Tim e (hours)

 As Received [100]

300

400

450

500 Misorientations based on [100] show low frequencies; slight bias towards {111} and {110} normals.

600

 As Received [110]

200

300

400

500 Peaks present for [110] misorientations at 30, 40, with normals between (001) and (1-11); also 60 with (-111).

600

 As Received [111]

200

300

400

500
All [111] misorientations favor pure twist boundaries with (111) normals; only 60[111] shows a massive peak, corresponding to the coherent twin. Peak at (111)-50[111] may be leakage from the coherent twin in (111)-60[111].

600

Comparative MRD for selected misorientations

As Received [110] 50hr [110]

600 [111]

600 [111]

500

500

Comparison Continued
As Received 50hr

[111]

[111]

600

600

Peaks occur at similar locations Peaks have similar intensities No change in GBCD

Conclusions
GBCD is similar to other low stacking fault energy fcc metals such as brass. Negligible changes in Grain size and Twin density. Negligible changes in texture. Negligible changes in grain boundary character distribution as far as 50 hours. Annealing at 7000 C has essentially no effect on the microstructure.

Acknowledgements
Dr. Kalu 1 Dr. Rollett 2 Steven Downey 1 Mohammed Alvi 2 Jason Gruber 2 Herb Miller 2 Tricia Bennett 2
(2) Carnegie Mellon University

(1)FAMU/FSU College of Engineering

Any Questions?

Supplemental Slides

MRD Plots - As Received [100]

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MRD Plots - As Received [110]

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 As Received [110]

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MRD Plots - As Received [111]

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 As Received [111]

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