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