ISO 11952:2014
(Main)Surface chemical analysis — Scanning-probe microscopy — Determination of geometric quantities using SPM: Calibration of measuring systems
Surface chemical analysis — Scanning-probe microscopy — Determination of geometric quantities using SPM: Calibration of measuring systems
ISO 11952:2014 specifies methods for characterizing and calibrating the scan axes of scanning-probe microscopes for measuring geometric quantities at the highest level. It is applicable to those providing further calibrations and is not intended for general industry use, where a lower level of calibration might be required.
Analyse chimique des surfaces — Microscopie à sonde à balayage — Détermination des quantités géométriques en utilisant des microscopes à sonde à balayage: Étalonnage des systèmes de mesure
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INTERNATIONAL ISO
STANDARD 11952
First edition
2014-05-15
Surface chemical analysis — Scanning-
probe microscopy — Determination
of geometric quantities using SPM:
Calibration of measuring systems
Analyse chimique des surfaces — Microscopie à sonde à balayage
— Détermination des quantités géométriques en utilisant des
microscopes à sonde à balayage: Étalonnage des systèmes de mesure
Reference number
©
ISO 2014
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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Published in Switzerland
ii © ISO 2014 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols . 2
5 Characteristics of scanning-probe microscopes . 4
5.1 Components of a scanning-probe microscope . 4
5.2 Metrological categories of scanning-probe microscopes . 5
5.3 Block diagram of a scanning-probe microscope . 5
5.4 Calibration interval . 7
6 Preliminary characterization of the measuring system . 8
6.1 Overview of the instrument characteristics and influencing factors to be investigated . 8
6.2 Waiting times after interventions in the measuring system (instrument installation,
intrinsic effects, carrying out operation, warm-up, tip/specimen change, etc.) .10
6.3 External influences .11
6.4 Summary .11
7 Calibration of scan axes .12
7.1 General .12
7.2 Measurement standards .12
7.3 Xy-scanner guidance deviations of the x- and y-axes (xtz, ytz) .13
7.4 Calibration of x- and y-axis (Cx, Cy) and of rectangularity (ϕxy) and determination of
deviations (xtx, yty, ywx).17
7.5 Calibration of the z-axis C , ϕ , and ϕ , and determination of the deviations ztz, zwx,
z xz yz
and zwy . 25
7.6 3D measurement standards for alternative and extended calibration .32
8 Report of calibration results .37
9 Uncertainties of measurement .38
9.1 General .38
9.2 Vertical measurand (height and depth).38
10 Report of results (form) .40
Annex A (informative) Example of superposition of disturbing influences in the
topography image .41
Annex B (informative) Sound investigations: Effects of a sound proofing hood .43
Annex C (informative) Thermal isolation effect of a sound proofing hood/measuring cabin .45
Annex D (informative) Handling of contaminations in recorded topography images .47
Annex E (informative) Step height determination: comparison between histogram and
ISO 5436-1 method .48
Annex F (normative) Uncertainty of measurement for lateral measurands (pitch,
position, diameter) .50
Bibliography .56
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 201, Surface chemical analysis, Subcommittee
SC 9, Scanning probe microscopy.
iv © ISO 2014 – All rights reserved
Introduction
The progress of miniaturization in semiconductor structuring, together with the rapid advance of
many diverse applications of nanotechnology in industrial processes, calls for reliable and comparable
[9]
quantitative dimensional measurements in the micro- and submicrometre range. Currently, a
measurement resolution, in or below the nanometre region, is frequently required. Conventional optical
or stylus measurement methods or coordinate measuring systems are not able to offer this level of
resolution.
For this reason, scanning-probe microscopes (SPMs) are increasingly employed as quantitative
measuring instruments. Their use is no longer confined only to research and development, but has also
been extended to include industrial production and inspection.
For this category of measuring instrument, standardized calibration procedures need to be developed,
for example, as have been established already long ago for contact stylus instruments (see ISO 12179).
For efficient and reliable calibration of SPMs to be carried out, the properties of the measurement
standards used need to be documented and be accounted for in the calibration (see Figure 1) and, at the
same time, the procedure for the calibration should be clearly defined.
Only if this prerequisite is satisfied, will it be possible to perform traceable measurements of geometrical
quantities.
Figure 1 — Traceability chain for scanning-probe microscopes
NOTE The calibration of a user’s SPM by means of traceably calibrated measurement standards is the
object of this International Standard (done by the user).
A scanning-probe microscope is a serially operating measuring device which uses a probe with a tip of
adequate fineness to trace the surface of the object to be measured by exploitation of a local physical
interaction (such as the quantum-mechanical tunnel effect, interatomic or intermolecular forces, or
evanescent modes of the electromagnetic field). The probe and the object to be measured are being
displaced in relation to one another in a plane (hereinafter referred to as the x-y-plane) according to a
[10]
while the signal of the interaction is recorded and can be used to control the distance
defined pattern,
between probe and object. In this International Standard, signals are considered which are used for the
determination of the topography (hereinafter called the “z-signal”).
This International Standard covers the verification of the device characteristics necessary for the
[11]
measurement of geometrical measurands and the calibration of the axes of motion (x, y, z), i.e. the
traceability to the unit of length via measurement on traceable lateral, step height, and 3D measurement
standards (see Figure 2).
While this International Standard aims at axis calibrations at the highest level and is thereby intended
primarily for high-stability SPMs, a lower level of calibration might be required for general industry use.
Key
1 measurement standards for verification purposes
1a flatness
1b probe shape
2 measurement standards for calibration purposes
2a 1D and 2D lateral
2b step height
3 calibration of the measurement standards by reference instruments (certified calibration, measurement
value including uncertainty)
Figure 2 — Verification and calibration of scanning-probe microscopes with test specimens and
measurement standards
This International Standard is mainly based on the guideline VDI/VDE 2656, Part 1, drafted by a
guideline committee of the VDI (Verein Deutscher Ingenieure/Association of German Engineers) in the
years 2004 to 2008, with the final whiteprint of that guideline being released in June 2008.
vi © ISO 2014 – All rights reserved
INTERNATIONAL STANDARD ISO 11952:2014(E)
Surface chemical analysis — Scanning-probe microscopy
— Determination of geometric quantities using SPM:
Calibration of measuring systems
1 Scope
This International Standard specifies methods for characterizing and calibrating the scan axes of
scanning-probe microscopes for measuring geometric quantities at the highest level. It is applicable to
those providing further calibrations and is not intended for general industry use, where a lower level of
calibration might be required.
This International Standard has the following objectives:
— to increase the comparability of measurements of geometrical quantities made using scanning-
probe microscopes by traceability to the unit of length;
— to defi
...
DRAFT INTERNATIONAL STANDARD ISO/DIS 11952
ISO/TC 201/SC 9 Secretariat: KATS
Voting begins on Voting terminates on
2011-10-13 2012-03-13
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ ORGANISATION INTERNATIONALE DE NORMALISATION
Surface chemical analysis — Scanning probe microscopy —
Determination of geometric quantities using SPM: Calibration of
measuring systems
Analyse chimique des surfaces — Microscopie à sonde à balayage — Détermination des quantités
géométriques en utilisant des microscopes à sonde à balayage: Étalonnage des systèmes de mesure
ICS 71.040.40
In accordance with the provisions of Council Resolution 15/1993 this document is circulated in
the English language only.
Conformément aux dispositions de la Résolution du Conseil 15/1993, ce document est distribué
en version anglaise seulement.
To expedite distribution, this document is circulated as received from the committee
secretariat. ISO Central Secretariat work of editing and text composition will be undertaken at
publication stage.
Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du
secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au
Secrétariat central de l'ISO au stade de publication.
THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME
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RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
© International Organization for Standardization, 2011
ISO/DIS 11952
Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted
under the applicable laws of the user’s country, neither this ISO draft nor any extract from it may be
reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic,
photocopying, recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO’s
member body in the country of the requester.
ISO copyright office
Case postale 56 CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
ii © ISO 2011 – All rights reserved
ISO/DIS 11952
Contents Page
1 Scope .1
2 Normative references, terms and definitions .2
2.1 Normative references .2
2.2 Terms used.3
3 Symbols .4
4 Characteristics of scanning probe microscopes .5
4.1 Components of a scanning probe microscope .5
4.2 Metrological categories of scanning probe microscopes.6
4.3 Block model of a scanning probe microscope.6
4.4 Calibration intervals .8
5 Preliminary characterization of the measuring system.8
5.1 Overview of the device characteristics and influence factors to be investigated.8
5.2 Waiting times after interventions into the measuring system).9
5.2.1 Potential causes of drift .10
5.2.2 Procedure .10
5.3 External influences.10
5.3.1 Kinds of internal influences.10
5.3.2 Consequences of external influences and countermeasures .10
5.4 Summary.11
6 Calibration .11
6.1 Standards .11
6.1.1 Requirements for standards.12
6.1.2 Handling of standards.12
6.2 Guidance deviations of the x- and y-axes (xtz, ytz) .12
6.2.1 Definition of guidance deviations from the plane (z-plane) .12
6.2.2 Measurement strategy.13
6.2.3 Flatness standards .14
6.2.4 Measurements.14
6.2.5 Evaluation.14
6.2.6 Summary.14
6.2.7 Extended calibration measurements.14
6.3 Calibration of x- and y-axis (Cx, Cy), .15
6.3.1 Definition of pitch p and p and rectangularity φφ in the x-y-plane .15
φφ
x y xy
6.3.2 Measurement strategy.16
6.3.3 Selection of lateral standards.16
6.3.4 Basic calibration: adjustments and measurements.17
6.3.5 Extended calibrations (scan speed, angle, eccentric measurements) .18
6.3.6 Evaluation.19
6.3.7 Extended evaluations: non-linearity of the x-y-axis.21
6.3.8 Summary.22
iii
ISO/DIS 11952
6.4 Calibration of the z-axis Cz, φφφφ , φφφφ and determination of the deviations ztz, zwx, zwy .22
xz yz
6.4.1 Definitions of the step height.22
6.4.2 Measurement strategy .23
6.4.3 Selection of step height standards.23
6.4.4 Basic calibration: Adjustments and measurements.23
6.4.5 Extended calibrations .25
6.4.6 Evaluations .25
6.4.7 Summary .28
6.5 3D standards for alternative and extended calibration .28
6.5.1 Requirements for 3D standards.29
6.5.2 Selection of the 3D standards.30
6.5.3 Carrying-out of the basic calibration.30
6.5.4 Evaluation of the measurements .30
6.5.5 Extended calibrations .31
6.5.6 Advantages and disadvantages of the 3D standard.32
7 Report of calibration results.32
8 Uncertainties of measurement.33
8.1 Vertical measurand (height, depth) .33
9 Report of results (form) .35
Annex A (informative) Exemplary superposition of disturbing influences in the topography .36
Annex B (informative) Sound investigations: Effects of a sound proofing hood .37
Annex C (informative) Thermal isolation effect of a sound proofing hood/measuring cabin.39
Annex D (informative) Control parameters and scan speed; handling of contaminations .41
Annex E (informative) Step height determination: comparison histogram and ISO-5436 method .42
Annex F (normative) Uncertainty of measurement for lateral measurands .44
Bibliography…………………………………………….…………………………………………………………….49
iv
ISO/DIS 11952
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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee
SC 9, Scanning probe microscopy.
v
ISO/DIS 11952
Introduction
The progress of miniaturization in semiconductor structuring, just as the fast advance of the extremely
versatile nanotechnology applications, in a great number of industrial processes calls for reliable and
comparable quantitative dimensional measurements in the micro- and submicrometre range [1]. By now
resolutions in or even below the nanometre region are already frequently required, i.e. resolutions
conventional optical or stylus measurement methods or coordinate measuring systems are not able to offer.
This is why scanning probe microscopes (SPM) are increasingly employed as quantitative measuring
instruments, their use being no longer confined only to research and development but increasingly extended
also to industrial production and inspection.
For this category of measuring instruments, too, standardized calibration procedures therefore need to be
developed as have, for example, been est
...
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