1、BSI Standards PublicationBS ISO 13095:2014Surface Chemical Analysis Atomic force microscopy Procedure for in situcharacterization of AFMprobe shank profile used fornanostructure measurementBS ISO 13095:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13095:
2、2014.The UK participation in its preparation was entrusted to TechnicalCommittee CII/60, Surface chemical analysis.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract.
3、Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 67752 6ICS 71.040.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority o
4、f theStandards Policy and Strategy Committee on 31 August 2014.Amendments issued since publicationDate Text affectedBS ISO 13095:2014 ISO 2014Surface Chemical Analysis Atomic force microscopy Procedure for in situ characterization of AFM probe shank profile used for nanostructure measurementAnalyse
5、chimique des surfaces Microscopie balayage de sonde Procdure pour la caractrisation in situ des sondes AFM utilises pour mesurer la nanostructureINTERNATIONAL STANDARDISO13095First edition2014-07-15Reference numberISO 13095:2014(E)BS ISO 13095:2014ISO 13095:2014(E)ii ISO 2014 All rights reservedCOPY
6、RIGHT PROTECTED DOCUMENT ISO 2014All 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 permis
7、sion. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 13095:2014IS
8、O 13095:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms . 35 Procedure for probe characterization . 45.1 Methods for the determination of AFM probe shapes 45.2 Reference sample
9、 setting . 55.3 Requirements of AFM and AFM imaging 65.4 Measurement of probe shank profile 75.5 Uncertainty of the measurement of the probe shank profile 96 Reporting of probe characteristics .10Annex A (informative) Dependence of AFM images on measurement mode and settings 12Annex B (normative) Re
10、ference sample preparation 15Annex C (informative) Example of a reference structure .18Annex D (informative) Results of EPSC measurement repeatability test 20Annex E (informative) Plane correction for probe shank profile analysis 22Annex F (informative) Example of a report 23Bibliography .25BS ISO 1
11、3095:2014ISO 13095:2014(E)ForewordISO (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 i
12、n 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 Commis
13、sion (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 sho
14、uld 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 i
15、dentifying 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 con
16、venience 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 ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Forewor
17、d - Supplementary informationThe committee responsible for this document is Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 9, Scanning probe microscopy.iv ISO 2014 All rights reservedBS ISO 13095:2014ISO 13095:2014(E)IntroductionAtomic force microscopes (AFMs) are of incr
18、easing importance for imaging surfaces at the nanoscale. The imaging mechanism involves a dilation of the surface form by the AFM probe shape. In practice, the radii of probe tips are in the range of 1 nm to 200 nm, which is the same order of magnitude as that of many important surface features. AFM
19、 images may, therefore, be strongly affected by the shape and size of the AFM probe used for imaging. In addition, the mechanism used to control the distance between the AFM probe and the sample surface can create artefacts in AFM images, because the effective probe shape characteristic depends on t
20、he control parameters. The probe radius and its half-cone angle are often used for the specification of AFM probes. However, practical probes are often not described so simply. Therefore, a quantitative expression for probe shank shape is required. This International Standard describes two methods f
21、or the detailed determination of probe shank shape: a projection of the probe profile (PPP) and the effective probe shape characteristic (EPSC), both of which are projected onto a defined plane and which, in turn, include the effect of the probe controlling mechanism. The PPP provides a continuous p
22、rofile, whereas the EPSC provides a few discrete characteristic points. PPP, used in conjunction with a probe shape characteristic (PSC) measurement, gives the quality of the probe for general applications, whereas EPSC indicates the usefulness of the probe for depth measurements in narrow trenches
23、and similar profiles. The true surface shape can be recovered and estimated from the measured surface with an accurate model of the true probe shape. This International Standard provides methods for the quantitative determination of aspects of AFM probe shank shape, to ensure that the probe is adequ
24、ate to measure surfaces with narrow trenches and similar profiles and to ensure reproducible AFM imaging. ISO 2014 All rights reserved vBS ISO 13095:2014BS ISO 13095:2014Surface Chemical Analysis Atomic force microscopy Procedure for in situ characterization of AFM probe shank profile used for nanos
25、tructure measurement1 ScopeThis International Standard specifies two methods for characterizing the shape of an AFM probe tip, specifically the shank and approximate tip profiles. These methods project the profile of an AFM probe tip onto a given plane, and the characteristics of the probe shank are
26、 also projected onto that plane under defined operating conditions. The latter indicates the usefulness of a given probe for depth measurements in narrow trenches and similar profiles. This International Standard is applicable to the probes with radii greater than 5u0, where u0is the uncertainty of
27、the width of the ridge structure in the reference sample used to characterize the probe.2 Normative referencesThe 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
28、 undated references, the latest edition of the referenced document (including any amendments) applies.ISO 18115-2:2010, Surface chemical analysis Vocabulary Part 2: Terms used in scanning-probe microscopyISO/TS 80004-4:2011, Nanotechnologies Vocabulary Part 4: Nanostructured materials3 Terms and def
29、initionsFor the purposes of this document, the terms and definitions given in ISO 18115-2, ISO/TS 80004-4 and the following apply.NOTE Some of the terms and definitions are reprinted here for convenience.3.1aspect ratio of the proberatio of the probe profile length at a certain position to the probe
30、 profile width at that position3.2deflection sensitivitysensitivity factor converting the output of an AFM optical displacement detection system for a cantilever in the contact mode to the displacement of the tip3.3error signalfeedback control system signal whose amplitude and sign are used to corre
31、ct the position and/or alignment between the controlling and the controlled elements3.4effective probe shape characteristicEPSCrelationship between the probe profile width and probe profile length for a given probe, including the effects of the true probe shape, artefacts due to the feedback control
32、ling mechanism in the AFM modes employed, and other imaging mechanisms of AFM projected onto a defined planeNote 1 to entry: The defined plane is usually the x-z plane.INTERNATIONAL STANDARD ISO 13095:2014(E) ISO 2014 All rights reserved 1BS ISO 13095:2014ISO 13095:2014(E)3.5narrow-ridge structureis
33、olated plateau with thin width having wide gaps on either side3.6peak force modeAFM intermittent contact mode using frequencies well below resonance in which the maximum force is used for measurement or for imaging3.7probe apexstructure at the extremity of a probe, the apex of which senses the surfa
34、ce43.8probe profile widthprojected width of a probe at a defined probe profile length, which may be for a defined azimuth or projection planeNote 1 to entry: The defined projection plane is usually the x-z plane.3.9probe profile lengthlength, measured from the probe apex along the instruments z (ver
35、tical)-axis, to a defined point on the probe axis3.10probe shape characteristicPSCrelationship between the probe profile width and the probe profile length for a given probe projected onto a defined planeNote 1 to entry: The defined projection plane is usually the x-z plane.3.11projected probe profi
36、lePPPmeasured profile of the probe projected onto a defined planeNote 1 to entry: The defined projection plane is usually the x-z plane.Note 2 to entry: Figure 1 a) shows schematically the relationship between the probe profile width, w, and length, l, and b) the definition of the aspect ratio, a.2
37、ISO 2014 All rights reservedBS ISO 13095:2014ISO 13095:2014(E)wlProbeProbeapexAspect ratioa=l / wxyza) b)Probeprog976ile width Probe prog976ile length a = l / w X Y Z Figure 1 Probe profile width ( w), defined here for projection on the x-z plane, and probe profile length (l)4 Symbols and abbreviate
38、d termsIn the list of abbreviated terms below, note that the “M” in the abbreviation “AFM,” defined here as an abbreviation for “Microscopy,” also is used as an abbreviation for “Microscope” depending on the context. The following are the abbreviated terms.AFM atomic force microscopyAM amplitude mod
39、ulationEPSC effective probe shape characteristicCRM certified reference materialPID proportional integral derivative (controller)PSC probe shape characteristicPPP projected probe profileTEM transmission electron microscopyThe following are the symbols for use in the formulae and as abbreviations in
40、the text.A0free oscillation amplitude of the cantilever before approaching the probe to the sampleAsposcillation amplitude of the cantilever for AFM imaginga aspect ratio of the probeD0distance between the side wall of an isolated ridge structure and the adjacent wallDjline distance between the two
41、side walls of the jthtrench structureemmaximum error signal, in nanometres, measured during the recording of the probe shape data ISO 2014 All rights reserved 3BS ISO 13095:2014ISO 13095:2014(E)f numbers of the framesH0average depth of the trenches on either side of the ridge structureHjdepth of the
42、 jthtrench structurej index number for the jthmeasurement of trenchl length of the probe profileljmaximum measured depth for the jthtrenchL0width of the ridge structurem index number for mthmeasurement of the probe profile lengthn index number for nthmeasurement of the probe profile lengthpmprobe pr
43、ofile length at mthmeasurementpnprobe profile length at nthmeasurementq difference of probe profile length between PSC and EPSC datar corner radius of the reference samplerrcorner radius of the ridge structure provided by the CRM supplierrtmaximum corner radius of the trench structurerjcorner radius
44、 of the side wall of the jthtrench structure provided by the CRM suppliers maximum slope of the PSC curvesEmaximum slope estimated from the EPSC datau combined standard uncertainty of the measurement of the probe profile lengthu0standard uncertainty of the width of the ridge structureusstandard unce
45、rtainty of the random component obtained by the probe profile length measurementutstandard uncertainty of the gap width of the multiple-trench structurew projected profile width of the AFM probe in the x-z planew apparent width of the ridge structurewjmeasured width of the AFM probe at jthmeasuremen
46、tL error in l caused by the presence of a non-zero value of rr5 Procedure for probe characterization5.1 Methods for the determination of AFM probe shapesThere are two methods to determine AFM probe shank profiles:a) narrow-ridge method to determine the probe projected profile (PPP) and the probe sha
47、pe characteristic (PSC);b) multiple-trench method to determine the effective probe shape characteristic (EPSC) for depth measurement.4 ISO 2014 All rights reservedBS ISO 13095:2014ISO 13095:2014(E)Either one or both of the above methods shall be used to determine aspects of the probe shank profile.
48、Suitable applications for each method are given in Table 1. The approximate profile of an AFM probe tip, i.e. the profile obtained by removing that of the tip apex, is determined by the narrow-ridge method using a reference sample. The resulting profile is given as the PPP onto a given plane. The PS
49、C is an expression of the relationship between the probe profile width and length obtained from PPP. The EPSC is the PSC determined at a few points using a multiple-trench structure. The narrow-ridge method is used mainly for the evaluation of AFM measurements for convex nano-structures, i.e. protrusions, whereas the multiple-trench method, under the two-point contact condition, is mainly used for depth measurements in narrow trenches and similar profiles. The two methods generate results that differ to an extent that depend
