Installation and commissioning of a high temperature ultra nanoindentation tester.
Date: 2015-11-12
Institutions: Institute for Energy and Transport
Subjects: composite materials, measuring equipment, metrology, physical sciences, research report, technical standard, testing

JRC Technical Systems 

Installation, Commissioning and 
Acceptance Testing of a High Temperature 
Ultra Nanoindentation Tester 

A. Ruiz Moreno, S. Ripplinger 
2 0 1 5  

Report EUR 26988 EN 

European Commission 

Joint Research Centre 

Institute for Energy and Transport   

Contact information 

Ana RUIZ MORENO 

Address: Westerduinweg 3, 1755LE Petten, The Netherlands 

E-mail: ana.ruiz-moreno@ec.europa.eu 

Tel.: +31 224 565097 

JRC Science Hub 

https://ec.europa.eu/jrc 

Legal Notice 

This publication is a Technical Report by the Joint Research Centre, the European Commission’s in-house science service.  

It aims to provide evidence-based scientific support to the European policy-making process. The scientific output 

expressed does not imply a policy position of the European Commission. Neither the European Commission nor any person 

acting on behalf of the Commission is responsible for the use which might be made of this publication. 

All images © European Union 2014 

This document replaces the previous report "Installation and Commissioning of a High Temperature Ultra Nanoindentation 

Tester" with ISBN number 978-92-79-44617-7 and PUBSY request number 93224. The new document additionally covers 

the acceptance testing of the high and low-temperature capabilities of the facility. 

JRC97612 

EUR 26988 EN 

ISBN 978-92-79-52779-1 (PDF) 

ISSN 1831-9424 (online) 

doi:10.2790/681051 

Luxembourg: Publications Office of the European Union, 2015 

© European Union, 2015 

Reproduction is authorised provided the source is acknowledged. 

Printed in The Netherlands  

Abstract 

The Institute for Energy and Transport (IET) of the Joint Research Centre (JRC) has purchased a modular Nanoindentation 

Test System for testing the physical properties of metallic, ceramic and composite materials at small length scales. The 

instrument allows the measurements of nanoindentation hardness  and  Young's modulus, creep, fracture toughness  and 

ductile-to-brittle  transition  temperature  at  nano  length  scales  from  cryogenic  to  high  temperatures  (-150  °C  ~  700  °C). 

Measurements  can  be  applied  to  characterize  the  properties  of  hard  coatings,  single  or  multi-layer  films,  bulk  soft 

materials, polymer films and multi-phase alloys. 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
1.  Introduction 

1.1.  Background 

The Institute for Energy and Transport (IET) decided to purchase a modular Nano-Indentation 
Test  System  to  support  its  activities  related  to  the  testing  of  the  physical  and  mechanical 
properties of metals, ceramics and composite materials. The equipment had to be capable of 
performing  the  classical  nano-indentation  experiments  based  on  instrumented  loading  and 
unloading  of  the  indenter  tip  onto  a  specimen  in  order  to  provide  indentation  hardness  and 
indentation modulus versus depth at precisely predefined positions on the specimen surface. 
The system had to allow measuring the indentation hardness, elastic modulus, creep, fracture 
toughness  and  Ductile-to  Brittle  Transition  Temperature  at  temperatures  ranging  from,  at 
least,  - 20°C up to 600°C. The equipment and measurements performed have to comply with 
ISO 14577 and ASTM E2546. 

In this scope, the IET launched a call for tenders requesting the following mandatory technical 
requirements: 

-  The equipment shall be modular constructed, capable to contain at least 3 different 
instruments attached to the frame. The load frame stiffness of the equipment shall 
be  ≥  1x10^7  N/m.  An  anti-vibration  table,  air  table  or  equivalent  shall  be  used  to 
minimize disturbances from the laboratory surrounding. 

-  The equipment shall be software controlled  for test execution,  data acquisition and 
data  analysis  and  include  the  following  loading  techniques:  force  control,  depth 
control, constant strain rate, step loading and depth profiling 

-  The equipment shall allow opting for a fully automated measurements program and 
testing  parameters  selectable  by  user,  including  at  least:  Initial  contact  load, 
maximum  load,  number  of  load  and  unload  increments,  holding  time  period,  final 
unload,  delayed  starting  of  a  test  (up  to  24h),  time  period  to  wait  after  each 
indentation,  number  of  indentations  and  spacing,  user  file  containing  custom  test 
schedule, user defined loading history including cyclic loading, matrix measurements 
by defining x, y coordinates or free settings via microscope. 

-  The equipment shall allow mounting and testing of multiple specimens with different 
heights  on  the  sample  holder.  Maximum  specimen  dimensions  (LxBxH):  >50mm  x 
50mm x 50mm. Usable inspection area (x, y): ≥ 50mm x 50mm 

-  The  following  standard  indenter  types  shall  be  mountable  on  the  equipment  and 
selectable  in  the  software:  Sphero-conical  indenter,  Berkovich  three-sided  pyramid 
indenter,  Vickers  four-sided  pyramid  indenter,  Knoop  four-sided  pyramid  indenter, 
Cube-corner three-sided pyramid indenter. 

-  The  equipment  shall  consist  of  either  a  vacuum  chamber  or  a  purge  chamber  to 

perform Nano-Indentation testing in oxygen reduced atmosphere.  

-  The equipment must allow the execution of tests at temperatures  from - 20° up to 
600°C  in  oxygen  reduced  atmosphere.  An  indenter-tip  heating  shall  be  provided  for 
elevated  temperature.  Sample  and  indenter  tip  temperature  within  the  temperature 
range  (room  temperature  –  maximum  temperature)  shall  not  differ  by  more  than 
3°C.  Thermocouples  or  equivalent  shall  be  installed  to  control  and  monitor 
temperatures of the sample, sample stage, indenter and other temperature sensitive 
parts.  Additional  merit  points  were  awarded  if  the  temperature  for  testing  could 
reach the range -150 °C ~ 800 °C. 

-  The  equipment  shall  provide  thermal  stability  under  normal  laboratory  conditions: 

thermal drift ≤ 0.3nm/min at room temperature and ≤ 20 nm/min at 600°C. 

-  The  maximum  usable  load  shall  not  be  lower  than  50mN  and  shall  not  exceed 
500mN. The continuously adjustable loading rate shall be at least 0 - 1000 mN/min. 
The load noise floor, under normal laboratory conditions, shall not exceed 0.5 μN in 
the  whole  range  of  test  temperatures.  The  load  resolution  shall  be  ≤  0.01  μN.  The 
equipment  shall  offer  a  minimum  contact  load  ≤  1  μN  in  the  whole  range  of  test 
temperatures. The minimum usable load shall not exceed 100 μN in the whole range 
of test temperatures. 

-  The equipment shall provide a minimum usable displacement of 100 µm to perform 
Nano-Indentation  testing.  The  displacement  noise  floor,  under  normal  laboratory 
conditions, shall be ≤ 0.2 nm. The displacement resolution shall be ≤ 0.01 nm. 

-  The  equipment  shall  provide  an  X-Y  positioning  resolution  of  the  specimen  stage  ≤ 
0.5μm. The specimen stage shall allow accommodating more than one specimen at a 
time for room temperature testing. The load frame shall be fitted with a z-axis drive 
to allow for positioning of samples with different thicknesses or sample heights. The 
stage shall allow computer controlled movement to and from the optical microscope 
re-position  accuracy  between  specimen  stage  and  optical 
or  AFM.  The 
microscope/AFM shall be ≤ 1 μm. 

-  The  optical  microscope  shall  provide  at  least  4  turret-mounted  lenses,  e.g.  5x,  10x, 
20x and 40x objectives that can be  positioned without the need for realignment of 
the  specimen  or  the  microscope.  High  temperature  filters  for  viewing  samples  at 
elevated temperatures shall be included. A colour CCD camera shall be attached on 
the optical microscope allowing live imaging and image capture. 

-  The  software  shall  allow  the  free  control  of  indentation  parameters,  the  use  of 
automated  measurement  sequences,  the  automatic  capture  of  pictures  of  each 
single indentation, the measurement of crack length after indentation, the real time 
monitoring of indentation curves, the recall of previous test cycles, and the means to 
generate  a  measurement  report  consisting  of  at  least  measurements  data, 
indentation curves, pictures and comments. Positioning of indentations shall be done 
either  by  setting  the  coordinates  or  by  using  the  optical  microscope.  Automated 
calibration  for  measuring  physical  distances  on  optical  microscope  (and  optional 
AFM) as well as indenter calibration shall be provided. A correction function for initial 
penetration, thermal drift, instrument compliance and indenter area function shall be 
available.  Real  time  display  of  indenter  coordination  position,  load,  displacement, 
temperature  of  sample  and/or  indenter,  parameter  of  environmental  chamber  shall 
be  selectable  by  user.  Automated  analysis  routines  shall  be  included  to  calculate 
indentation  data  for:  Vickers  Hardness,  Knoop  Hardness,  Rockwell  Hardness,  Brinell 
Hardness,  Stress/strain  data,  Creep,  Relaxation,  Plastic  and  elastic  work,  Fracture 
toughness, 3D mapping and profiling.  

-  Two  pieces  of  each  of  the  following  standard  indenters,  together  with  a  calibrated 
area function, shall be supplied: Berkovich and sphero-conical indenters, in diamond 
and in a material for high temperature tests compatible with carbon steel.  

-  The equipment shall be equipped with at least 2 different pieces standard reference 
blocks  according  to  ISO  14577  and  ASTM  E2546.  Each  reference  block  shall  be 
provided with certified values of dynamic Young's modulus and Poisson's ratio.      

As  options,  tenderers  were  invited  to  provide  quotations  for  a  Scratch  Tester  and  an  Atomic 
Force Microscope (AFM). 

 
 
 
1.2.  Call for tender 

The contract notice of the open call for tenders was published in the O.J. 2013/S 150-260077 
on 03/08/2013.  

Four  tenders  from  four  companies  were  received  and  evaluated  with  respect  to  their 
compliance  with the technical requirements. The  evaluation committee  decided  to award the 
contract to ST Instruments offering equipment from CSM Instruments, as the company offered 
the most competitive quotation while it provided solid documented evidence of their technical 
capabilities to meet the specifications beyond the mandatory technical requirements.. 

1.3.  Features of the instrument selected. 

The company awarded with the supply contract, ST Instruments, offered the delivery of a high 
temperature nanoindentation instrument from CSM Instruments, a company recently acquired 
by  Anton  Paar,  GmbH.  The  CSM  High  Temperature  Ultra  Noanoindentation  Tester  allows  the 
acquisition  of  accurate  load-displacement  data  up  to  temperatures  of  ≥  700  °C  thanks  to  a 
transducer  system  that  compensates  thermal  drift  keeping  it  below  10  nm/min.  The 
technology enables the measurement of hardness, Young's modulus, fatigue and creep data of 
materials at high temperatures at the nano scale.  

At  small  length  scales,  thermal  stability  becomes  the  more  important  problem  to  extract 
accurate  quantitative  mechanical  properties  from 
load-displacement  data.  The  CSM 
nanoindentation instrument solves the issue by using a unique referencing design that allows 
for  continuous  differential  depth  measurements,  thus  ensuring  a  very  good  thermal  stability 
and a fast indentation cycle. The referencing system is based on the principle of using an axis 
of  measurement  and  an  axis  of  reference,  each  one  having  its  own  actuator  and  depth  and 
force  sensors,  to  carry  out  active  referencing  of  the  surface  of  the  sample.  The  Ultra 
Nanoindentation  head  is  made  of  Zerodur,  a  ceramic  glass  with  an  extremely  low  thermal 
expansion  coefficient,  and  the  thermal  drift 
is  minimized  by  preheating  both  the 
nanoindentation tip and the sample. 

The  instrument  is  also  equipped  with  a  software  package  that  allows  performing  tests  in  a 
wide  variety  of  testing  modes,  i.e.  simple  loading,  multi-cycle  loading,  dynamic  mechanical 
analysis, automated matrixes or pinpointed location testing. 

The key features of the systems are the following: 

-  Active top referencing (Patented Design US 7,685,868,B2). 

-  Low thermal drift: the head is made of Zerodur glass and the electronic system has a 

drift rate of ≈ 1 ppm/°C. 

-  Load frame stiffness >> 108 N/m 

-  Two independent depth and load sensors 

-  High resolution and very low noise:  

o  Depth resolution: 0.0003 nm, noise floor: 0.03 nm 
o  Load resolution: 0.001 µN, noise floor: 0.13 µN 

-  Positional synchronization between the indentation head, the optical microscope head 

and the atomic force microscope head. 

-  Compliant to ISO 14577 and ASTM E2546. 

 
 
 
2.  Commissioning 

2.1.  Technical specifications 

ST  Instruments  has  provided  the  Ultra  Nanoindentation  Tester  on  a  modular  high  vacuum 
platform including heating (≥700 °C) and cooling (≤-150 °C) consisting of the following parts: 

-  Automated platform for secondary vacuum with secondary vacuum chamber, including 
adapted  automated  platform  and  frame  (X,  Y,  Z),  secondary  vacuum  chamber  and 
control, and optical observation. 

-  Ultra  Nanoindentation  Tester  Module  for  secondary  vacuum  and  compatible  with 
measurements at elevated temperatures (≥ 700 °C), including a Ultra Nano Hardness 
head with laser tip heating. 

-  High  temperature  stage  (≥  700  °C)  for  secondary  vacuum,  including  heating,  cooling 

and temperature controllers. 

-  Cryogenic  sample  stage  for  secondary  vacuum,  including  liquid  nitrogen  pump, 

connectors and tubing, allowing cooling the sample sown to -150 °C. 

-  Antivibration table for vacuum chamber. 

-  High  load  range  (maximum  load  of  100mN)  and  high  depth  range  (maximum 

penetration depth of 100 µm) sensors and actuators for Ultra Nanoindentation. 

-  Berkovich indenters of diamond and tungsten carbide. 

-  Spherical indenters of diamond and tungsten carbide. 

A  dedicated  AFM  (NaniteAFM,  from  Nanosurf)  for  the  direct  characterization  of  the 
nanoindentations  is  integrated  to  the  Ultra  Nanoindentation  Tester.  The  embedded  AFM  has 
the following features: 

-  Synchronised positioning of AFM - optical microscope – nanoindentation head 

-  Optical top and side view of cantilever and sample. 

-  Large scan area up to 110 x 110 mm, with 22 mm in Z range. 

-  Contact modes of contact force, height and force modulation. 

-  Dynamic modes of non-contact force, phase contrast, force modulation and magnetic 

force. 

2.2.  Delivery, installation and commissioning 

The  delivery,  installation  and  commissioning  has  been  carried  out  in  two  phases.  The  first 
phase, completed on 03.10.2014, encompassed the commissioning and acceptance testing of 
the  Ultra  Nanoindentation  Tester  only  with  regard  to  its  room  temperature  measurement 
capabilities.  

The second phase was delayed until 22.04.2014, due to a change in the design of the system 
by decision of the provider. In the final design the high temperature module included an infra-
red  source  to heat  the  tip,  while  in  the  original  design  the heating  of  the  tip was  done  by  a 
laser.  This  second  phase  then  addressed  the  commissioning  and  acceptance  tests  of  the 
modules needed to perform tests at low (≤ -150 °C) and high (≥ 700 °C) temperature. 

A first acceptance test of the load-displacement calibration was carried out by measuring the 
modulus  of  a  Fused  Silica  reference  sample  at  room  temperature.  The  certified  plane  strain 
modulus of the reference silica is E* = 75.4 ± 0.3 GPa and the calculated indentation modulus 
is EIT = 73.5 ± 0.3 GPa. Figure 1 shows the load-displacement curve applying a maximum load 

 
of 10 mN during 5 s, with loading and unloading rates of 20 mN/min. The measured moduli 
were within the errors of the certified values:    E* = 75.3 GPa ;  

EIT = 73.4 GPa 

Figure 1. Load-displacement curve during Nanoindentation on a fused silica reference sample 

Further  acceptance  tests  were  carried  out  to  validate  the  temperature  range,  stability  and 
noise levels.  Table 1 below lists the parameters tested: 

Parameter 

Requirement 

High temperature 
indentation, including tip 
and reference heating 
Sub-zero indentation 
Secondary vacuum 
Thermal stability 

Tmax: ≥700°C 
∆T of indenter to sample  ≤ 3°C 

Tmin: ≤ -150°C 
≤ 1 x 10-5 mbar 
Room temperature (RT): ≤0.3nm/min 
Thermal drift at 600°C:  ≤ 20nm/min 

Load noise floor 

≤ 0.5μN in the whole temperature 
range 

Displacement noise floor 

≤ 0.2nm  

Achieved during 
tests 
T = 700°C 
∆T = 2°C 

T = -195°C 
7 x 10-6 mbar 
RT: 0.18 nm/min 
600°C: 2.8 nm/min 
(Figure 2) 
0.19 µN at RT 
0.27 µN at 600°C 
(Figure 3) 
0.14 nm (Figure 4)  

The temperature range was measured on a circumferential 316L bulk sample. Temperatures 
from  -150  °C  up  to  700  °C  were  achieved.  700°C  were  observed  at  an  output  power  of  the  
heater of 82%. The temperature difference between indenter and sample was around 2°C, i.e. 
below the value required in the technical specifications (≤ 3°C). 

The  thermal  stability  at  room  and  high  temperatures  was  checked  doing  a  load  controlled 
indentation test on fused silica and calculating the thermal drift from the displacement signal. 
Variations  lower  than  0.3  nm/min  and  20  nm/min  were  measured  at  RT  and  600  °C, 
respectively, as required in the technical specifications (Fig. 2). 

05010015020025030035040001234567891011   Depth (nm)Force (mN) Fused Silica 
 
 
 
The  load  noise  floor  is  calculated  from  the  load  curve  during  the  indenter  approach  and  the 
displacement  noise  floor  from  the  displacement  curve  during  the  pause.  Figures  3  and  4 
highlight the data regions used for the estimation of the noise.   

Figure 2. Evaluation of the thermal drift. 

1802002202408586878889900.51.01.5drift = 0.18 nm/min88.27 nmFn (mN)Pd (nm)t (s)88.45 nmThermal drift RT  608010012056058060062064029303132Fn (mN)Pd (nm)t (s)Thermal drift 600 °C drift = 2.8 nm/min 613.0 nm615.8 nm 
 
 
 
 
 
 
Load noise floor (RT) 

noise = 0.19 µN 

Load noise floor (600°C) 

noise: 0.27 µN 

Figure 3. Evaluation of the compliance with the load noise floor value at room temperature and at 600 °C. 

 
 
 
 
 
 
Displacement noise floor 

noise: 0.14 nm 

Figure 4. Evaluation of the compliance with the displacement noise floor value. Data acquired at room 
temperature. 

2.3.  Sample tests 

A basic measurement of a metallic  sample was carried out during the commissioning of the 
equipment. Alloy 800 HT, a solid solution strengthened iron-nickel-chromium alloy, was used 
for the tests. The specimen had been coated with a layer of NiCrAlY by plasma spraying with 
the  aim  of  improving  the  surface  mechanical  and  corrosion  properties.  The  sample  was 
mounted  in  bakelite  and  polished.  Figure  5  shows  a  SEM  cross  section  of  the  sample  and 
Figure 6 the load-displacement curves of indentations performed on the base material (alloy 
800 HT) and on the coating (plasma spray NiCrAlY) applying a maximum load of 10mN during 
10s,  with  loading  and  unloading  rates  of  20mN/min.  Table  2  summarises  the  measured 
mechanical  properties.  The  indentation  hardness,  HIT,  is  expressed  by  the  ratio  between  the 
applied  load  and  the  contact  area  and  is  a  measure  of  the  resistance  to  permanent 
deformation.  EIT  and  E*  are  the  indentation  modulus  and  the  plane  strain  modulus, 
respectively. The plane strain modulus is unaffected by elastic anisotropy. E  IT is calculated by 
multiplying E* by a factor of one minus the square of Poisson's ratio. The results show a lower 
modulus  of  the  coating  and  a  much  higher  hardness  as  compared  to  the  base  material,  in 
accordance to expectations. 

Table 2. Measured hardness and moduli of a 800 HT stainless steel sample and its NiCrAlY coating.  

800 HT 

NiCrAlY coating 

HIT (MPa) 

EIT (GPa) 

E* (GPa) 

3118.9 

185.13 

203.44 

5551 

168.27 

184.91 

 
 
 
 
 
 
55 µm 

Figure 5. SEM image of the NiCrAlY-coated 800 HT alloy sample. 

Figure 6. Load-displacement curves during nanoindentation on a 800 HT stainless steel sample coated 
with NiCrAlY 

05010015020025030035040001234567891011  Force (mN)Displacement (nm) 800 HT NiCrAlY coating 
 
 
 
 
 
 
 
 
 
The  following  additional  sample  tests  of  different  materials  were  also  carried  out  to  verify  the 
capabilities of the equipment at low and high temperatures: 

Test  1: Matrix measurement on oxide-dispersion strengthened steel MA956 bulk sample at room 
temperature 

  Number of indents: 144 (12 x 12) 
 
Indenter material: Diamond   
  Test parameters:  

o  x / y spacing: 15µm 
o  Load controlled 
o  Loading rate: 20mN/min 

  Max load: 10mN 
  Pause: 10s 
  Unloading rate: 20mN/min  

A  delayed  start  (at  7  pm)  of  the  measurement  was  programmed.  Single  indents  were  evaluated 
and  faulty  indents  were  removed.  A  hardness  mapping  and  Young's  modulus  mapping  was 
presented,  concluding  that  the  functionality  and  capabilities  of  the  equipment  to  perform 
indentation test matrices and automated measurements was sufficiently demonstrated. 

Test 2: High temperature indentation tests on 316L bulk sample. 

  Number of indents: 7 (single indents) 
  Test temperature: room temperature, 600°C and 700°C 
 
  Test parameters: 

Indenter material: Tungsten Carbide 

o  Load controlled 
o  Loading rate: 120mN/min 

  Max load: 30mN 
  Pause: 120s 
  Unloading rate: 120mN/min 

Figure  7  shows  the  loading  and  unloading  curves  recorded  at  600  °C  and  700  °C,  proving  the 
capabilities  of  the  equipment  to  carry  out  high  temperature  indentation  tests  up  to  700°C  as 
required.  

Figure 7. Load-displacement curves during Nanoindentation on 316L stainless steel at 600 °C and 700 °C 

01002003004005006007008000102030  Force (mN)Depth (nm) 600 °C 700 °C 
 
 
 
 
Test 3: Sub-zero test on Cu bulk sample at -100°C and -150°C 

  Test temperature: -100°C, -150°C 
 
Indenter material: Diamond 
  Sample material: Cu 
  Test parameters: 

o  Load controlled 
o  Loading rate: 120mN/min 

  Max load: 30mN 
  Pause: 10s 
  Unloading rate: 120mN/min 

Figure  8  shows  the  load-displacement  curves  recorded  at  -100  °C  and  -150  °C.  The  tests  have 
proven  the  capabilities  of  the  equipment  to  carry  out  sub-zero  indentation  tests  as  requested  in 
contract 111171. 

Figure 8. Load-displacement curves during Nanoindentation on Cu at -100 °C and -150 °C 

3.  Conclusions 

The  delivery,  installation,  commissioning  and  acceptance  testing  of  a  High  Temperature  Ultra 
Nanoindentation  Tester,  coupled  to  a  dedicated  Atomic  Force  Microscope,  have  been  successfully 
completed  on  22.04.2014.  The  system  was  able  to  perform  fully  automated  measurements.  The 
temperature range, vacuum level, thermal stability and noise levels of the equipment were tested 
and  met  the  technical  requirements.  The  delay  in  submitting  some  of  the  parts,  in  particular  the 
temperature-controlled tip and stages was due to the decision of the company to modify the initial 
design during production in order to deliver a more performing instrument. 

020040060080010000102030  Force (mN)Depth (nm) -100 °C -150 °C 
 
 
 
 
 
 
 
 
 
 
 
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European Commission 

EUR 26988 EN– Joint Research Centre – Institute for Energy and Transport 

Title: Installation, Commissioning and Acceptance Testing of a High Temperature Ultra Nanoindentation Tester 

Authors: Ana RUIZ MORENO, Stefan RIPPLINGER 

Luxembourg: Publications Office of the European Union 

2015 – 16 pp. – 21.0 x 29.7 cm 

EUR – Scientific and Technical Research series – ISSN 1831-9424 (online) 

ISBN 978-92-79-52779-1 (PDF) 

doi: 10.2790/681051 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
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 doi: 10.2790/681051 
ISBN 978-92-79-52779-1