1、 ISO 2014 Surface chemical analysis Scanning- probe microscopy Determination of geometric quantities using SPM: Calibration of measuring systems Analyse chimique des surfaces Microscopie sonde balayage Dtermination des quantits gomtriques en utilisant des microscopes sonde balayage: talonnage des sy
2、stmes de mesure INTERNATIONAL STANDARD ISO 11952 First edition 2014-05-15 Reference number ISO 11952:2014(E) ISO 11952:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utiliz
3、ed 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 ISOs member body in the country of the requester. ISO copyright
4、 office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ISO 11952:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms and defini
5、tions . 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
6、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 inf
7、luences .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 (xy) and determination of deviations (xtx, yty, ywx)17 7.5 Cali
8、bration of the z-axis C z , xz , and yz , and determination of the deviations ztz, zwx, 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
9、)38 10 Report of results (form) .40 Annex A (informative) Ex ample of superposition of distur bing influenc es in the topography image .41 Annex B (informative) S ound in v estig ations: Effects of a sound pr oofing hood 43 Annex C (informative) Thermal isolation effect of a sound pr oofing hood/mea
10、suring 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)
11、 .50 Bibliography .56 ISO 11952:2014(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 bo
12、dy 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 Electrot
13、echnical 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 I
14、SO 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 r
15、esponsible 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 g
16、iven 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 ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the follo
17、wing 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 ISO 11952:2014(E) Introduction The progress of miniaturization in semiconductor structurin
18、g, together with the rapid advance of many diverse applications of nanotechnology in industrial processes, calls for reliable and comparable quantitative dimensional measurements in the micro- and submicrometre range. 9Currently, a measurement resolution, in or below the nanometre region, is frequen
19、tly 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
20、 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 1
21、2179). 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 prer
22、equisite 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 users SPM by means of traceably calibrated measurement standards is the object of this International Standard (
23、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 i
24、ntermolecular 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 defined pattern, 10while the signal of the interaction is recorded and
25、can be used to control the distance ISO 2014 All rights reserved v ISO 11952:2014(E) 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 ver
26、ification of the device characteristics necessary for the measurement of geometrical measurands and the calibration of the axes of motion (x, y, z), 11i.e. the traceability to the unit of length via measurement on traceable lateral, step height, and 3D measurement standards (see Figure 2). While thi
27、s 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 s
28、tandards 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) F i g u r e 2 V e r i f i c a t i o n a n d c a l i b r a t i o n o f s c a n n i n g - p r o b e
29、 m i c r o s c o p e s w i t h t e s t s p e c i m e n s a n d 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,
30、 with the final whiteprint of that guideline being released in June 2008.vi ISO 2014 All rights reserved INTERNATIONAL ST ANDARD ISO 11952:2014(E) Surface chemical analysis Scanning-probe microscopy Determination of geometric quantities using SPM: Calibration of measuring systems 1 Scope This Intern
31、ational 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 cal
32、ibration 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 define the minimum requirements for the calibration process a
33、nd the conditions of acceptance; to ascertain the instruments ability to be calibrated (assignment of a “calibrate-ability” category to the instrument); to define the scope of the calibration (conditions of measurement and environments, ranges of measurement, temporal stability, transferability); to
34、 provide a model, in accordance with ISO/IEC Guide 98-3, to calculate the uncertainty for simple geometrical quantities in measurements using a scanning-probe microscope; to define the requirements for reporting results. 2 Normative references The following documents, in whole or in part, are normat
35、ively 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 11039, Surface chemical analysis Scanning-probe microscopy
36、Measurement of drift rate ISO 18115-2, Surface chemical analysis Vocabulary Part 2: Terms used in scanning-probe microscopy IEC/TS 62622, Artificial gratings used in nanotechnology Description and measurement of dimensional quality parameters ISO/IEC Guide 98-3, Uncertainty of measurement Part 3: Gu
37、ide to the expression of uncertainty in measurement (GUM:1995) 3 T erms a nd definiti ons For the purposes of this document, the terms and definitions given in ISO 18115-2 and IEC/TS 62622 and the following apply. 3.1 scanner bow additional deflection in the z-direction when the scanner is displaced
38、 in the x-y-direction Note 1 to entry: Scanner bow is also known as out-of-plane motion (see also xtz, ytz in Clause 4). ISO 2014 All rights reserved 1 ISO 11952:2014(E) 3.2 look-up table table in which a set of correction factors for the scanner are filed for different modes of operation (scan rang
39、es, scan speeds, deflections, etc.) 3.3 step height height of an elevation (bar) or depth of a groove (ISO 5436-1), in atomic surfaces, the distance between neighbouring crystalline planes 3.4 levelling correction of the inclination between the ideal x-y-specimen plane and the x-y-scanning plane 4 S
40、ymbols x, y, z position value related to the respective axis C x , C y , C z calibration factors for the x-, y-, and z-axes h step height w width of a structure of the specimen N j i thpitch value in a profile used for the determination of the pitch/period (number of pitch values i over all lines j
41、= 1,., Nj) p x pitch or period in the x-direction p y pitch or period in the y-direction a x vector in the x-direction of a grating (not to be confused with p x ) a y vector in the y-direction of a grating (not to be confused with p y ) xy non-orthogonality of 2D gratings P-V peak-to-valley value r
42、radius Rq (Sq) root mean square deviation of the assessed roughness profile (Rq) or of the assessed area (Sq) T temperature m thermal expansion coefficient T L temperature of the air T m temperature of the specimen during measurement j x angle of rotation about the x-axis j y angle of rotation about
43、 the y-axis j z angle of rotation about the z-axis levelling angle x L value of the measurement standard for shift in the x-direction x m shift in the x-direction measured with the x-displacement transducer2 ISO 2014 All rights reserved ISO 11952:2014(E) xtx positional deviation x measured along an
44、x-coordinate line xty straightness deviation y measured along an x-coordinate line xtz straightness deviation z measured along an x-coordinate line xrx rotational deviation j xmeasured along an x-coordinate line xry rotational deviation j ymeasured along an x-coordinate line xrz rotational deviation
45、 j zmeasured along an x-coordinate line xwy measured rectangularity deviation in the coordinate plane x-y xwz measured rectangularity deviation in the coordinate plane x-z y L value of the measurement standard for displacement in the y-direction y m displacement measured with the y-displacement tran
46、sducer in the y-direction ytx positional deviation x measured along a y-coordinate line yty straightness deviation y measured along a y-coordinate line ytz straightness deviation z measured along a y-coordinate line yrx rotational deviation j xmeasured along a y-coordinate line yry rotational deviat
47、ion j ymeasured along a y-coordinate line yrz rotational deviation j zmeasured along a y-coordinate line ywz rectangularity deviation measured in the coordinate plane y-z z L value of the measurement standard for displacement in the z-direction z m displacement in the z-direction measured with z-dis
48、placement transducer ztx straightness deviation x measured along a z-coordinate line zty straightness deviation y measured along a z-coordinate line ztz straightness deviation z measured along a z-coordinate line zrx rotational deviation j xmeasured along a z-coordinate line zry rotational deviation
49、 j ymeasured along a z-coordinate line zrz rotational deviation j zmeasured along a z-coordinate line cos( i ) rotational correction, e.g. in pitch measurement cos( i ) tilt-related correction, e.g. in pitch measurement s short-wavelength filter (see ISO 4287 for details) c long-wavelength filter (see ISO 4287 for details) correlation length xy angle between the x- and y-direction, counterclockwise xz angle between the x- and z-direction, counterclockwise ISO 2014
