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Douglas Stauffer, Ph.D.
Cold and ColderNanoindentation Down to -120oC
Overview
In Operando Materials Testing
• Motivation
• Basic Principles
• Instrumentation
• Performance on reference sample
• Case Studies
• 1018 Steel, two phase materials
• PDMS, Tmelt
• Polymer thin film, Tg
USPO 61/659391
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
In Operando Testing:Material Behavior in the Environment of Operation
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
“high temperature resistance, ease of metallization, resistance to climatic effects and moisture, dimensional stability and processability”
DuPont.com
Coating 1: Protection from Chips
“How it’s made” ScienceGo
MotivationMechanical Properties at Small Length Scales
Coating 2: Adhesion Layer
“How it’s made” ScienceGo
Coating 3: Aluminized Reflector
“How it’s made” ScienceGo
Coating 4,5,6... Filament ~3200K
Brittanica.com
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Basic Nanoindentation Principles –Quasi-Static Nanoindentation
hf
A
SEr
2
Reduced Modulus
A
PH
Hardness
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
• Temperatures from -120 to 800oC
• Using xSol technology
• O2 and H20 < 1ppm [equivalent PO210-3 Torr]
Controlled Atmosphere Systems
xSol® - Heating, Cooling, HumidityHeating: 800°C • Cooling: -120°C • Humidity: 95% RH
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
System Performance
XPM Indentation on (100) Single Crystal Aluminum: • Average of 25 indents at each temperature
-120 -100 -80 -60 -40 -20 0 20 400
10
20
30
40
50
60
70
80
90
100
Er(GPa)
Reduced M
odulu
s (
GP
a)
Temperature (°C)
Aluminum (100)
0.00
0.25
0.50
0.75
1.00
Hard
ness (
GP
a)
1. XPM: High Speed Nanoindentation and Mechanical Property Mapping Webinarhttps://www.bruker.com/webinars
2. Simon, N.J., et al., (1991). Review of Cryogenic Mechanical and Thermal Properties of Al-Li Alloys and Alloy 2219 (United States, NIST)
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
[1] [2]
System Performance
-120 -100 -80 -60 -40 -20 0 20 400
10
20
30
40
50
60
70
80
90
100
Er(GPa)
Re
duce
d M
od
ulu
s (
GP
a)
Temperature (°C)
Aluminum (100)
0.00
0.25
0.50
0.75
1.00
Ha
rdn
ess (
GP
a)
0 50 100 150 200 250 300 3500
200
400
600
800
1000
Lo
ad
(µ
N)
Depth (nm)
-100oC -0oC
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
XPM Indentation on (100) Single Crystal Aluminum: • Average of 25 indents at each temperature
System Performance
Fused Quartz, F = 2mN
-140 -120 -100 -80 -60 -40 -20 0
-0.03
-0.02
-0.01
0.00
0.01
0.02
0.03
Drift
(n
m/s
)
Temperature (°C)0 10 20 30 40 50 60
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
0.4
0.6
0.8
Depth
(nm
)
Time (s)
Std Deviation Minimum Median Maximum
0.254 -0.897 -0.084 0.605
T = -80oC
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Temperature Effects on 1018 Steel
Mapping 3 Indents/s at 0oC SPM with the Cooling System at 0
oC
Hardness Contour Map1018 Steel
Hintsala, E.D., et al., JOM (2018) 70: 494
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
X (mm)
Y (
mm
)
Mapping 3 Indents/s at 0oC Hardness Frequency
Hardness Contour Map1018 Steel
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Temperature Effects on 1018 Steel
X (mm)
Y (
mm
)
Mapping 3 Indents/s at 0oC Hardness Frequency
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Hardness Contour Map1018 Steel
Temperature Effects on 1018 Steel
X (mm)
Y (
mm
)
Ferrite Phase: Sweeping Temperature
0.5s-1 constant ሶ𝜀04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
1018 Steel
Comparison of Three Steels
1018 Steel Nitronic 50 Sandvik 1RK 91
• Nitronic 50 shows no transition down to -73oC• Sandvik 1RK 91 exhibits a transition between -15oC and -25oC.
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Brief Review of nanoDMA III
c
s
A
kE
2'
c
s
A
CE
2''
S.A. Syed Asif, & J.B. Pethica, MRS Proceedings, 505,103 (1997)
s
s
k
C tan
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Ks KiCs Ci
Applied F
orc
e
Displacement
Reference Frequency Sweep
For long durations, “reference” technique may be employed to measurethe contact area periodically throughout the test.
c
s
A
kE
2'
)(Fkk ss
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
Amorphous Polymer TransitionsPolymer Melt
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
-60 -40 -20 0 200.02
0.04
0.06
0.08
0.10
0.12
0.14
0.16
0.18
0.20
Refe
rence S
tora
ge
Mod
ulu
s (
GP
a)
Temperature (oC)
301 Hz
171 Hz
74 Hz
42 Hz
10 Hz
~Tm PDMS
Refe
rence S
tora
ge
Mo
du
lus (
GP
a)
Temperature (oC)
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
-60 -40 -20 0 20 40 60 80 1000.01
0.1
1
Sto
rage M
odulu
s (
GP
a)
Temperature (oC)
Sto
rage
Mo
du
lus (
GP
a)
Temperature (oC)
-80 -60 -40 -20 0 20 40 60 80 100 1200.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
Tan D
elta
Temperature (Deg C)
1 Hz
15 Hz
101 Hz
260 Hz
Ta
n D
elta
Temperature (oC)
Amorphous Polymer TransitionsPolymer Film
Conclusions
• Instrumentation
• Performance
• Three materials, three different temperature transitions
• 1018 Steel athermal to thermal plasticity
• PDMS through the melting temperature
• Polymer film Tg
• Winter is Coming!
04/19/2018 Cold and Colder, Nanoindentation Down to -120°C | Bruker
© Copyright Bruker Corporation. All rights reserved.
www.bruker.com
© Copyright Bruker Corporation. All rights reserved. Cold and Colder, Nanoindentation Down to -120°C | Bruker