high temperature nanoindentation up to 810 c: … paar talk uicu... · high temperature...

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High temperature nanoindentation up to 810°C:

Experimental Optimization

N. X. Randall, M. Conte, B. Bellaton, Jarod Zhao

Anton Paar TriTec SA, Rue de la Gare 4, Peseux CH2034, Switzerland

[email protected]

G. Mohanty, J. Schwiedrzik, J. M. Wheeler, J. Michler

EMPA, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of

Materials and Nanostructures, Feuerwerkerstrasse 39, Thun CH3602, Switzerland

mailto:[email protected]




1 • Background to High Temperature Indentation Testing

2 • Current Challenges

3 • How does UNHT3 HTV address such challenges?

4 • Basic system overview

5 • Validation of specifications over entire temp. range

6 • Application examples

7 • Conclusions

Summary


Background to high temperature testing

Industrial applications are:

▸ Cutting tools hard coatings for high speed machining;

▸ Semiconductors;

▸ Thermal barrier coatings;

▸ Nuclear materials

Academic applications are:

▸ Investigation on dislocation induced by high temperature and deformation;

▸ Creep and fatigue changes with temperature;

▸ Hardness variation with temperature;

▸ Etc.


Current challenges to high temperature indentation

Sample and tip oxidation

J. M. Wheeler and J. Michler, Review of

Scientific Instruments 84, 101301 (2013)

Tip Hardness decay

Diamond tip

after contact with

steel sample at

500 °C

J. M. Wheeler and J. Michler, Review of

Scientific Instruments 84, 101301 (2013)

Sample and tip interaction

Courtesy of UTC, France

Tip contamination

High Vacuum or Inert gas

environment

Tip material opportune choice depending on the

sample material

Tip cleaning process


UNHT3 HTV High Vacuum System Features

• Ultimate Vacuum: 10-7 mbar

• Process Vacuum: 10-6 mbar

• Vacuum chamber Volume: 100 liters

• Pumping speed: 800 l/s

• Primary pump is rotary vane

• Secondary pump is turbo molecular

with magnetic levitation bearings

• Partial pressure mixture gas control:

10-900 mbar

• Flow gas mixture control rate: 0-2000

sccm

• User available additional ports

• Integrated compressed air-pistons

Vacuum

Buffer

P1

P2


UNHT3 HTV High Vacuum System Features

Active air pads

Damped frame

Integrated

electronics

High Vacuum enclosure

Ultimate vacuum 2x10-7 mbar

Water cooling

circuit


Some pictures


UNHT3 HTV Adjustable sample holder

Cement vs clamping

Patent pending PCT/EP2017/051035


Stage

sample

A1

I

A2

R Reference contact

A1 & A2: piezoelectric actuators

Motorized Z table

Feedback loop for accurate low force

sensing

Feedback loop on force sensor FN

Dz

Load-depth curve

UNHT3 HTV Head Design


UNHT3 HTV Head Features

Infra Red Heaters (x2)

Water Cooled Jacket Reflective Mirror

Long Shaft Indenter

& Reference

Pending Patent EP14191443.2: UNHT3 HT Tip heating design

Pending Patent EP14191442.4: UNHT3 HT Design of heated probe

Vacuum Compatible Piezos

Zerodur frame ensures negligible thermal

expansion (0 – 100°C)

Cu-Be Springs, range 0 – 100 mN


Indentation/reference tips

Tip

heating

system

Sample heating

module Sample

A comprehensive approach is needed: the problem is not only the heating up but also controlling the

temperature and keeping it stable for a long time. The whole system must be considered.

UNHT3 HTV Heating System Features: IR Bath

Pending Patent EP16151845.1: UNHT3 HT Sample holder arrangement


UNHT3 HTV Temperature Management

Reference

Thermocouple

Sample

Thermocouple *

Sample Holder

Thermocouple

[Security]

Indenter

Thermocouple

UNHT3 HT Head

Thermocouple

[Security for head < 40°C]

Sample Heater

Power

* Two thermocouples are available:

(1) Under sample holder

(2) On sample surface

User can choose which of the 2

thermocouples to use for regulation

Indenter, Reference and Sample temperatures can be regulated independently in 3 ways:

(1) Power regulation (e.g., constant wattage control, user definable)

(2) Target temperature (via PID control, user definable)

(3) Slope or heating ratio (°/min, user definable)


UNHT3 HTV Temperature Management

Z0


High Purity Molybdenum (Raw Data)

Thermal drift measurements

(raw data) on pure

Molybdenum at 810°C

showing < 2 nm/min. average

drift rate over a 300 s pause at

10% of maximum applied load.


High Purity Molybdenum (Raw Data)

23°C 810°C

23°C

810°C


Titanium Nitride (TiN) on WC substrate

TiN thickness: 3 µm

Maximum load: 30 mN, holding time 10 sec


Titanium Nitride (TiN) on WC substrate (Raw Data)

TiN thickness: 3 µm

Maximum load: 30 mN, holding time 10 sec

RT 200C 400C 600C

Hardness (GPa): 27.3 21.4 18.3 7.6

Elastic Modulus (GPa): 397 321 289 183


Alumina (Al2O3) on WC substrate

Al2O3 thickness: 10 µm

Maximum depth: 400 nm, holding time 10 sec

Loading/Unloading speed: 150 nm/min


THANK YOU

high temperature nanoindentation up to 810 c: … paar talk uicu... · high temperature...

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