Metallic materials - Instrumented indentation test for hardness and materials parameters - Part 2: Verification and calibration of testing machines (ISO 14577-2:2015)

This part of ISO 14577 specifies the method of verification and calibration of testing machines for
carrying out the instrumented indentation test in accordance with ISO 14577-1:2015.
It describes a direct verification method for checking the main functions of the testing machine and an
indirect verification method suitable for the determination of the repeatability of the testing machine.
There is a requirement that the indirect method be used in addition to the direct method and for the
periodic routine checking of the testing machine in service.
It is a requirement that the indirect method of verification of the testing machine be carried out
independently for each test method.
This part of ISO 14577 is also applicable for transportable testing machines.

Metallische Werkstoffe - Instrumentierte Eindringprüfung zur Bestimmung der Härte und anderer Werkstoffparameter - Teil 2: Prüfung und Kalibrierung der Prüfmaschinen (ISO 14577-2:2015)

Dieser Teil von ISO 14577 legt das Verfahren zur Prüfung und Kalibrierung von Prüfmaschinen für die
instrumentierte Eindringprüfung entsprechend ISO/DIS 14577-1:2012 fest.
Er beschreibt ein direktes Prüfverfahren zur Überprüfung der Hauptfunktionen der Prüfmaschine und ein
indirektes Prüfverfahren, das zur Bestimmung der Wiederholpräzision der Prüfmaschine geeignet ist. Das
indirekte Verfahren ist zusätzliche zum direkten Verfahren sowie für regelmäßige Routineüberprüfungen der
Prüfmaschine im Betrieb anzuwenden.
Die indirekte Prüfung der Prüfmaschine muss für jedes Verfahren separat durchgeführt werden.
Dieser Teil von ISO 14577 ist auch bei tragbaren Prüfmaschinen anwendbar.

Matériaux métalliques - Essai de pénétration instrumenté pour la détermination de la dureté et de paramètres des matériaux - Partie 2: Vérification et étalonnage des machines d'essai (ISO 14577-2:2015)

L'ISO 14577-2:2015 spécifie la méthode de vérification et d'étalonnage des machines d'essai destinées à la réalisation de l'essai de pénétration instrumenté conformément à l'ISO 14577‑1:2015.
Elle décrit une méthode de vérification directe pour contrôler les fonctions principales de la machine d'essai et une méthode de vérification indirecte appropriée pour la détermination de la répétabilité de la machine d'essai. Il est exigé que la méthode indirecte soit utilisée en sus de la méthode directe et pour le contrôle de routine périodique de la machine d'essai en service.
Il est exigé que la méthode indirecte de vérification de la machine d'essai soit réalisée de façon indépendante pour chaque méthode d'essai.
L'ISO 14577-2:2015 est également applicable aux machines d'essai transportables.

Kovinski materiali - Instrumentirano vtiskanje pri preskušanju trdote in drugih lastnosti materialov - 2. del: Overjanje in kalibriranje preskuševalnih strojev (ISO 14577-2:2015)

Ta del standarda ISO 14577 določa metodo za overjanje in kalibriranje preskuševalnih strojev za
izvajanje preskušanja z instrumentiranim vtiskanjem v skladu s standardom ISO 14577-1:2015.
Opisuje neposredno metodo overjanja za preverjanje glavnih funkcij preskuševalnih strojev in posredno metodo overjanja, primerno za ugotavljanje ponovljivosti za preskuševalni stroj. Vključena je zahteva, da se mora posredna metoda uporabiti poleg neposredne metode ter da je treba redno izvajati rutinska preverjanja preskuševalnega stroja, ki se uporablja.
Zahteva se, da se posredna metoda overjanja preskuševalnega stroja opravi neodvisno za vsako preskusno metodo. Ta del standarda ISO 14577 se uporablja tudi za premične preskuševalne stroje.

General Information

Status
Published
Publication Date
07-Sep-2015
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
03-Sep-2015
Due Date
08-Nov-2015
Completion Date
08-Sep-2015

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SLOVENSKI STANDARD
SIST EN ISO 14577-2:2015
01-oktober-2015
1DGRPHãþD
SIST EN ISO 14577-2:2004
Kovinski materiali - Instrumentirano vtiskanje pri preskušanju trdote in drugih
lastnosti materialov - 2. del: Overjanje in kalibriranje preskuševalnih strojev (ISO
14577-2:2015)
Metallic materials - Instrumented indentation test for hardness and materials parameters
- Part 2: Verification and calibration of testing machines (ISO 14577-2:2015)
Metallische Werkstoffe - Instrumentierte Eindringprüfung zur Bestimmung der Härte und
anderer Werkstoffparameter - Teil 2: Prüfung und Kalibrierung der Prüfmaschinen (ISO
14577-2:2015)
Matériaux métalliques - Essai de pénétration instrumenté pour la détermination de la
dureté et de paramètres des matériaux - Partie 2: Vérification et étalonnage des
machines d'essai (ISO 14577-2:2015)
Ta slovenski standard je istoveten z: EN ISO 14577-2:2015
ICS:
77.040.10 Mehansko preskušanje kovin Mechanical testing of metals
SIST EN ISO 14577-2:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 14577-2:2015

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SIST EN ISO 14577-2:2015

EUROPEAN STANDARD
EN ISO 14577-2

NORME EUROPÉENNE

EUROPÄISCHE NORM
July 2015
ICS 77.040.10 Supersedes EN ISO 14577-2:2002
English Version
Metallic materials - Instrumented indentation test for hardness
and materials parameters - Part 2: Verification and calibration of
testing machines (ISO 14577-2:2015)
Matériaux métalliques - Essai de pénétration instrumenté Metallische Werkstoffe - Instrumentierte Eindringprüfung
pour la détermination de la dureté et de paramètres des zur Bestimmung der Härte und anderer Werkstoffparameter
matériaux - Partie 2: Vérification et étalonnage des - Teil 2: Überprüfung und Kalibrierung der Prüfmaschinen
machines d'essai (ISO 14577-2:2015) (ISO 14577-2:2015)
This European Standard was approved by CEN on 16 April 2015.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14577-2:2015 E
worldwide for CEN national Members.

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SIST EN ISO 14577-2:2015
EN ISO 14577-2:2015 (E)
Contents
Page
European foreword .3


2

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SIST EN ISO 14577-2:2015
EN ISO 14577-2:2015 (E)
European foreword
This document (EN ISO 14577-2:2015) has been prepared by Technical Committee ISO/TC 164 “Mechanical
testing of metals” in collaboration with Technical Committee ECISS/TC 101 “Test methods for steel (other
than chemical analysis)” the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by January 2016, and conflicting national standards shall be withdrawn at
the latest by January 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 14577-2:2002.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 14577-2:2015 has been approved by CEN as EN ISO 14577-2:2015 without any modification.

3

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SIST EN ISO 14577-2:2015

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SIST EN ISO 14577-2:2015
INTERNATIONAL ISO
STANDARD 14577-2
Second edition
2015-07-15
Metallic materials — Instrumented
indentation test for hardness and
materials parameters —
Part 2:
Verification and calibration of
testing machines
Matériaux métalliques — Essai de pénétration instrumenté pour la
détermination de la dureté et de paramètres des matériaux —
Partie 2: Vérification et étalonnage des machines d’essai
Reference number
ISO 14577-2:2015(E)
©
ISO 2015

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 General conditions . 1
3.1 Preparation . 1
3.2 Functional installation . . 1
3.3 Indenter . . 2
3.4 Application of the test force . 2
4 Direct verification and calibration . 2
4.1 General . 2
4.2 Calibration of the test force . 2
4.3 Calibration of the displacement measuring device . 3
4.4 Verification and calibration of the machine compliance . 4
4.4.1 General. 4
4.4.2 Procedure . 4
4.5 Calibration and verification of the indenter . 5
4.5.1 General. 5
4.5.2 Vickers indenter . 5
4.5.3 Berkovich, modified Berkovich, and corner cube indenters . 7
4.5.4 Hard metal ball indenters . 8
4.5.5 Spherical tipped conical indenters . 9
4.6 Verification of the indenter area function .10
4.6.1 General.10
4.6.2 Procedure .10
4.7 Verification of the testing cycle .10
5 Indirect verification .11
5.1 General .11
5.2 Procedure .12
6 Intervals between calibrations and verifications .14
6.1 Direct verification and calibration .14
6.2 Indirect verification .15
6.3 Routine checking .15
7 Verification report/Calibration certificate .15
Annex A (informative) Example of an indenter holder .16
Annex B (normative) Procedures for determination of indenter area function .17
Annex C (informative) Examples for the documentation of the results of indirect verification .19
Annex D (normative) Machine compliance calibration procedure .21
Bibliography .25
© ISO 2015 – All rights reserved iii

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT), see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 164, Mechanical testing of metals, Subcommittee
SC 3, Hardness testing.
This second edition cancels and replaces the first edition (ISO 14577-2:2002), which has been
technically revised.
ISO 14577 consists of the following parts, under the general title Metallic materials — Instrumented
indentation test for hardness and materials parameters:
— Part 1: Test method
— Part 2: Verification and calibration of testing machines
— Part 3: Calibration of reference blocks
— Part 4: Test method for metallic and non-metallic coatings
iv © ISO 2015 – All rights reserved

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

Introduction
Hardness has typically been defined as the resistance of a material to permanent penetration by
another harder material. The results obtained when performing Rockwell, Vickers, and Brinell tests are
determined after the test force has been removed. Therefore, the effect of elastic deformation under the
indenter has been ignored.
ISO 14577 (all parts) has been prepared to enable the user to evaluate the indentation of materials by
considering both the force and displacement during plastic and elastic deformation. By monitoring the
complete cycle of increasing and removal of the test force, hardness values equivalent to traditional
hardness values can be determined. More significantly, additional properties of the material, such as
its indentation modulus and elasto-plastic hardness, can also be determined. All these values can be
calculated without the need to measure the indent optically. Furthermore, by a variety of techniques, the
instrumented indentation test allows to record hardness and modulus depth profiles within a, probably
complex, indentation cycle.
ISO 14577 (all parts) has been written to allow a wide variety of post test data analysis.
© ISO 2015 – All rights reserved v

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SIST EN ISO 14577-2:2015

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SIST EN ISO 14577-2:2015
INTERNATIONAL STANDARD ISO 14577-2:2015(E)
Metallic materials — Instrumented indentation test for
hardness and materials parameters —
Part 2:
Verification and calibration of testing machines
1 Scope
This part of ISO 14577 specifies the method of verification and calibration of testing machines for
carrying out the instrumented indentation test in accordance with ISO 14577-1:2015.
It describes a direct verification method for checking the main functions of the testing machine and an
indirect verification method suitable for the determination of the repeatability of the testing machine.
There is a requirement that the indirect method be used in addition to the direct method and for the
periodic routine checking of the testing machine in service.
It is a requirement that the indirect method of verification of the testing machine be carried out
independently for each test method.
This part of ISO 14577 is also applicable for transportable testing machines.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 376, Metallic materials — Calibration of force-proving instruments used for the verification of uniaxial
testing machines
ISO 3878, Hardmetals — Vickers hardness test
ISO 14577-1:2015, Metallic materials — Instrumented indentation test for hardness and materials
parameters — Part 1: Test method
ISO 14577-3, Metallic materials — Instrumented indentation test for hardness and materials parameters —
Part 3: Calibration of reference blocks
3 General conditions
3.1 Preparation
The machine shall be designed in such a way that it can be verified.
Before verification and calibration of the testing machine, it shall be checked to ensure that the conditions
laid down in 3.2 to 3.4 are met.
3.2 Functional installation
The testing machine shall be configured to operate in compliance with and shall be installed in an
environment that meets the requirements of this part of ISO 14577, ISO 14577-1:2015, and, where
applicable, ISO 14577-3. The testing machine shall be protected from vibrations. For testing in the
© ISO 2015 – All rights reserved 1

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

micro and nano ranges, the testing machine shall also be protected from air currents and temperature
fluctuations.
The influence of environment on the data, i.e. the noise floor, shall be estimated by performing a low force
(e.g. equivalent to the usual initial contact force) indentation on a CRM and analysing the displacement
over time. The force variability is the indent stiffness (obtained from force removal curve) multiplied
by the standard deviation of the displacement once any background drift in mean displacement has
been subtracted. These uncertainties shall then be included in the total combined uncertainty tests as
calculated in ISO 14577-1:2015, Clause 8 and Annex H.
3.3 Indenter
In order to get repeatable measurements of the force/indentation depth data set, the indenter holder
shall be firmly mounted into the testing machine.
The indenter holder should be designed in such a way that the contribution to the overall compliance is
minimized (see Annex A).
3.4 Application of the test force
The test force shall be applied and removed without shock or vibration that can significantly affect the
test results. It shall be possible to verify the process of increasing, holding, and removal of the test force.
4 Direct verification and calibration
4.1 General
4.1.1 Direct verification and calibration shall be carried out at the constant temperature of use, typically
10 °C to 35 °C, but preferably in the range (23 ± 5) °C. If a range of operating temperatures is required, then
direct calibration and verification should be carried out at suitable points over that temperature range
to determine the calibration validity as a function of temperature. If necessary, a calibration correction
function or a set of calibrations valid at specific operating temperatures can be determined.
4.1.2 The instruments used for direct calibration and verification shall be traceable to National
Standards as far as available.
4.1.3 Direct verification and calibration involves
a) calibration of the test force,
b) calibration of the displacement measuring device,
c) verification and calibration of the machine compliance,
d) verification of the indenter,
e) calibration and verification of the indenter area function, if the indentation depth is less than 6 µm, and
f) verification of the test cycle.
4.2 Calibration of the test force
4.2.1 Each range of force used shall be calibrated over the whole force range for both application and
removal of the test force. A minimum of 16 evenly distributed points in the test force range shall be
calibrated, i.e. 16 during application and 16 during removal of the test force. The procedure shall be
repeated at least three times and the average calibration value shall be used. The maximum difference in
calibration values shall not exceed half of the tolerances given in Table 1.
2 © ISO 2015 – All rights reserved

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

4.2.2 The test force shall be measured by a traceable method, for example, the following:
a) measuring by means of an elastic proving-device in accordance with class 1, or better of, ISO 376;
b) balancing against a force, accurate to within ±0,2 % applied by means of calibrated masses with
mechanical advantage;
c) electronic balance with a suitable accuracy of 0,1 % of the minimum calibrated test force or 10 µg
(0,1 µN) for the nano range.
For each measured point used for calibration, the difference between the measured and the nominal test
force shall be within the tolerances given in Table 1.
Table 1 — Tolerances for test forces
Range of the test force
Tolerances
F
%
N
F ≥ 2 ±1,0
0,001 ≤ F < 2 ±1,0
a
F < 0,001 ±2,5
a
For the nano range, a tolerance of ±1 % is strongly recommended.
4.3 Calibration of the displacement measuring device
4.3.1 The resolution required of the displacement measuring system depends on the size of the smallest
indentation depth being measured. For the micro range, this value is by definition h = 0,2 µm; for the
macro range it is typically ≥2 µm.
The scale of the displacement measuring device shall be graduated to permit a resolution of indentation
depth measurement in accordance with Table 2.
4.3.2 The displacement measuring device shall be calibrated on the testing machine for every range
used by means of a suitable method and a corresponding system. The device shall be calibrated at a
minimum of 16 points in each direction evenly distributed throughout its travel. The procedure shall be
repeated three times.
The following methods are recommended for the measurement of the relative displacement of the
indenter: laser interference method, inductive method, capacitive method, and piezotranslator method.
For each measured point used for calibration, the difference between the measured and the nominal
displacement shall be within the tolerances given in Table 2.
Table 2 — Resolution and tolerances of the displacement measuring device
Resolution of the displacement
Range of application measuring device Tolerances
nm
Macro ≤100 1 % of h
Micro ≤10 1 % of h
a
Nano ≤1 2 nm
a
   For the nano range, a tolerance of <1 % of h (indentation depth) is strongly recommended.
4.3.3 Changes in temperature are commonly a dominant source of displacement drift. To minimize
thermally induced displacement drift, the temperature of the instrument shall be maintained such that the
displacement drift rate remains constant over the time period of one calibration cycle. The drift rate shall
© ISO 2015 – All rights reserved 3

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SIST EN ISO 14577-2:2015
ISO 14577-2:2015(E)

be measured during, immediately before, or immediately after each calibration cycle, e.g. by monitoring
displacement during a suitable hold period. The displacement calibration data shall be corrected for
thermal drift and the product of variation in drift rate and the duration of one calibration cycle shall be
less than the tolerance given in Table 2. The drift rate uncertainty shall be included in the displacement
calibration uncertainty calculation.
4.4 Verification and calibration of the machine compliance
4.4.1 General
See Annex D and ISO 14577-1:2015, Annex C.
This verification and calibration shall be carried out after the test force and the displacement measuring
system have been calibrated in accordance with 4.2 and 4.3.
4.4.2 Procedure
The calibration and verification of machine compliance is carried out by the measurement of indentation
modulus at a minimum of five different test forces. Method 3 as described in Annex D is recommended.
In all cases, a suitable Certified Reference Material (CRM) shall be mounted into the instrumented
indentation test system in the same way as future test samples will be mounted. This is to ensure that
the CRM provides a faithful reproduction of each particular total machine compliance.
The compliance of the testing machine can be affected by the particular construction and mounting of an
indenter and also the method used to mount a sample. For instance, mounting in plastics (e.g. PVC) can
introduce an extra compliance into the measurement loop. The verification and calibration of machine
compliance should be performed using the indenter that will be used for subsequent measurements.
For indentation depths, h > 6 µm, it is not necessary to take into account the real contact area function.
c
For the verification and calibration of the machine compliance, a reference material with certified
indentation modulus, independent from the indentation depth, shall be used. A material with a high
ratio of EH/ (such as tungsten) is recommended. The range for the test force is defined by the
IT IT
minimum test force that correlates to 6 µm indentation depth and the maximum possible test force of
the testing machine. Large indentation depths have the advantage that errors in the area function are
likely to be smaller; however, care shall be taken that the test is not biased by pile-up in the reference
material. The measured compliance of the indentation shall then be compared with the calculated
compliance for the indentation using the certified value of modulus. To recalibrate machine compliance,
the product of the applied force and the detected difference in machine compliance is applied to the
displacement data to refine the estimate of contact depth and, therefore, the machine compliance
estimate at each force. This process is iterated until self-consistent values of machine compliance and
contact depth are reached.
For indentation depths, <6 µm, the method above shall be applied, except that the actual area of contact,
as calculated from the calibrated indenter area function, shall be used to calculate the contact compliance
using the certified modulus of the CRM.
In many nano and micro range instruments, the machine compliance value is independent of force.
However, if this is not the case, then a machine compliance function can be determined using the above
procedure but a wider range of forces. The range for the test forces is defined by the indentation depths,
>0,5 µm, and the maximum test force of the testing machine or the maximum test force for which no
...

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