1、BS ISO 19606:2017Fine ceramics (advancedceramics, advanced technicalceramics) Test method forsurface roughness of fineceramic films by atomic forcemicroscopyBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 19606:2017 BRITISH STANDARDNational forewordThis Britis
2、h Standard is the UK implementation of ISO 19606:2017.The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport t
3、o include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 86440 7 ICS 81.060.30 Compliance with a British Standard cannot confer immunity from legal obligations
4、.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 19606:2017 ISO 2017Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for
5、surface roughness of fine ceramic films by atomic force microscopyCramiques techniques Mthode dessai pour la rugosit de surface des films cramique fins par microscopie force atomiqueINTERNATIONAL STANDARDISO19606First edition2017-02Reference numberISO 19606:2017(E)BS ISO 19606:2017ISO 19606:2017(E)i
6、i ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll 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
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8、 09 47copyrightiso.orgwww.iso.orgBS ISO 19606:2017ISO 19606:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Test environment . 25 Roughness measurement specimens 26 Test apparatus . 26.1 Cantilever . 26.2 Scanner 26.3 Specimen stage . 37 Test apparatus
9、 calibration . 38 Probe-tip diameter evaluation standard plate . 49 Calibration of X-Y and Z scan axes 410 Probe-tip error evaluation . 510.1 Outline of probe-tip error evaluation 510.2 Measurements of preliminary Ra and RSm .610.3 Evaluation of probe-tip diameter 610.4 Evaluation of error in roughn
10、ess measurements 811 Roughness measurements of specimen 1312 Test report 14Annex A (normative) Determination of D from D .16Annex B (informative) Method to determine criteria for probe-tip error .18Bibliography .24 ISO 2017 All rights reserved iiiContents PageBS ISO 19606:2017ISO 19606:2017(E)Forewo
11、rdISO (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 technica
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17、 .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 206, Fine ceramics.iv ISO 2017 All rights reservedBS ISO 19606:2017ISO 19606:2017(E)IntroductionSurface roughness measurements of fine ceramic thin films in nanometer scale by atomic force microscopy have become one
18、of the techniques widely applied to quality control and assurance in industries.One of the problems most frequently occurring in roughness measurements by atomic force microscopy resulting from its scale dependency is the deviation of roughness due to the wear of the probe tip or the deviation in th
19、e curvature of commercially available probe tips. This problem makes it difficult to obtain a reliable and reproducible result of the roughness measurement. Therefore, it is highly desirable to standardize a method to evaluate probe tip diameter or curvature radius.This document covers the evaluatio
20、n of probe-tip diameter and provides a method to judge the adequateness of a probe tip for use in day-to-day roughness measurements of fine ceramic thin films with a certain arithmetical mean roughness in the range needing the use of atomic force microscopy in production lines or quality assurance p
21、rocesses.It should be noted that because surface roughness is a scale-dependent metrology parameter, it is unavoidable that the probe-tip evaluation process contains some contradictory procedures, namely the adequateness of the probe tip for a roughness measurement depends on unmeasurable true rough
22、ness in a scale of interest.In this document, the parameters based on roughness profiles are used. The roughness profile is obtained by using a low-pass filter according to ISO 16610-21. The process to obtain the sampling length, which is identical to cut-off wavelength, is given in ISO 4288. Some d
23、ifferent sampling lengths to process a primary profile can be applied to obtain appropriate values of arithmetic mean deviation of a roughness profile, if necessary. ISO 2017 All rights reserved vBS ISO 19606:2017BS ISO 19606:2017Fine ceramics (advanced ceramics, advanced technical ceramics) Test me
24、thod for surface roughness of fine ceramic films by atomic force microscopy1 ScopeThis document describes a method to evaluate the adequateness of a probe tip for fine-ceramic thin-film surface roughness measurements by atomic force microscopy, of surfaces with an arithmetical mean roughness, Ra, in
25、 the range of about 1 nm to 30 nm and a mean width of roughness profile elements, RSm, in the range of about 0,04 m to 2,5 m.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated
26、references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parametersISO 4288, Geometric
27、al Product Specifications (GPS) Surface texture: Profile method Rules and procedures for the assessment of surface textureISO 11039, Surface chemical analysis Scanning-probe microscopy Measurement of drift rateISO 11952, Surface chemical analysis Scanning-probe microscopy Determination of geometric
28、quantities using SPM: Calibration of measuring systemsISO 18115-2, Surface chemical analysis Vocabulary Part 2: Terms used in scanning-probe microscopyISO 25178-2, Geometrical product specifications (GPS) Surface texture: Areal Part 2: Terms, definitions and surface texture parameters3 Terms and def
29、initionsFor the purposes of this document, the terms and definitions given in ISO 4287, ISO 4288, ISO 18115-2, ISO 11039, ISO 11952 and ISO 25178-2 and the following apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available
30、 at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp3.1evaluation lengthln(X), ln(Y)length of surface profile in the X or Y direction3.2probe-tip diameter evaluation standard plateplate on which needle-shaped spikes are formedNote 1 to entry
31、: The plate is used to evaluate the probe-tip diameter (3.3).INTERNATIONAL STANDARD ISO 19606:2017(E) ISO 2017 All rights reserved 1BS ISO 19606:2017ISO 19606:2017(E)3.3probe-tip diameterDdiameter of a probe tip at a distance of 10 nm from the tip end4 Test environmentTesting shall be carried out on
32、ly where temperature change, sound noise and mechanical vibration of the floor or walls are small enough to perform the measurements. The following installation environment is recommended:a) temperature: 18 C to 25 C;b) humidity: 70 % or less;c) noise level: 60 dB or less;d) mechanical vibration of
33、the floor or the wall: 1 103m/s2(100 Hz) or less.5 Roughness measurement specimensSpecimens for roughness measurements are ceramic thin films on a substrate. Any kinds of substrate material can be used, such as metal, glass, polymer, etc. The specimen shall be no larger than the specimen stage of th
34、e instrument being used.6 Test apparatus6.1 CantileverThe cantilever shall be exclusively dedicated for a dynamic mode and commercially available. The resonant frequency should be higher than 100 kHz.6.2 ScannerThe scanner shall be capable of scanning cantilever or specimen stage by shifting the XYZ
35、 position. The scanning area should be larger than 10 m 10 m in the XY plane.Figure 1 shows an example of a measurement system having a specimen stage scan mechanism. Position in the Z direction is controlled using a Z-position control circuit that keeps a constant separation between the probe and t
36、he specimen surface. For this purpose, a light beam from a laser diode illuminates the cantilever and the reflected beam position is monitored by a light detector. Surface profile is measured by scanning the specimen stage in the XY plane.2 ISO 2017 All rights reservedBS ISO 19606:2017ISO 19606:2017
37、(E)Key1 laser diode 6 specimen stage2 light detector 7 X, Y and Z scanner3 cantilever 8 Z-position control circuit4 probe tip 9 X-Y scan circuit5 specimenFigure 1 Schematic of AFM system6.3 Specimen stageThe specimen stage shall be capable of supporting a specimen horizontally. The test area of the
38、specimen should be in the centre of the specimen stage. Scanning should be performed near the centre of the X, Y and Z axes of the scanner used.7 Test apparatus calibrationThis document only describes a method to evaluate the adequateness of a probe tip for fine-ceramic thin-film surface roughness m
39、easurements by atomic force microscopy. If the apparatus needs to be calibrated, refer to standards describing calibration criteria and methods for a scanning probe microscope; see ISO 4288, ISO 11039 and ISO 11775. ISO 2017 All rights reserved 3BS ISO 19606:2017ISO 19606:2017(E)8 Probe-tip diameter
40、 evaluation standard plateA standard for probe-tip diameter evaluation is a plate on which a number of needle-shaped spikes, arranged in a square matrix, are formed. The needle-shaped spikes are typically as follows: tip curvature radius: 10 nm; tip aperture angle: 20 or 50; tip height: 300 nm to 60
41、0 nm; distance between any two nearest neighbour tips: 2,12 m; plate size: 5 mm 5 mm.9 Calibration of X-Y and Z scan axesThe calibration of the X-Y scanner and Z scanner should be carried out by measuring the X, Y and Z profile of a certified calibration standard. The standard should have a grating
42、with a certain pitch and a step with a certain height.The standard sample is a specimen with calibrated height and pitch, which are certified and traceable with uncertainty data attached. It is recommended that the grating pitch is less than 2 m and that the step height is less than 20 nm.The calibr
43、ation standard should be stored in a clean and dry box and be handled with care.The calibration shall be carried out in the following sequence using the dynamic mode.a) Mount the calibration standard in such a way that the grating is oriented to the X-Y axes of the scanner and that its plane lies ne
44、arly parallel to the X-Y plane of the scanner.b) Set the number of picture elements at 512 512 or 256 256.c) Scan an area of about 10 m square of the calibration standard and store the surface profile data. An example is shown in Figure 2 a).d) From the surface profile data, draw a surface profile a
45、long the X direction at a selected Y position where the surface profile contains several steps on the calibration standard and level off the one-dimensional profile along the X direction. An example is shown in Figure 2 b).e) Measure profile peak height at the centre of top and bottom sections of th
46、e profile. Calculate mean height for at least five successive profile elements in the profile along the X direction.f) Measure a pitch along the X direction by measuring the distance between the mid-points of two successive rising or falling parts of the profile.g) From the surface profile data, dra
47、w a surface profile along the Y direction at a selected X position where the surface profile contains several steps and level off the one-dimensional profile along the Y direction.h) Measure profile peak heights at the centre of top and bottom sections of the profile. Calculate mean height for at le
48、ast five successive profile elements in the profile along the Y direction.i) Measure a pitch along the Y direction by measuring the distance between the mid-points of two successive rising or falling parts of the profile.j) If an X- or Y-pitch measured is out of the range of uncertainty needed for r
49、oughness measurements, correct X or Y values by obtaining an X- or Y-axis calibration factor.k) If the mean height obtained is out of the range of uncertainty needed for roughness measurements, correct Z values by obtaining a Z-axis calibration factor.4 ISO 2017 All rights reservedBS ISO 19606:2017ISO 19606:2017(E)a) Surface profile b) Surface profile along the X directionFigure 2 Examples of surface profile data for the calibration of the X-Y scanner and Z scanner10 Probe-tip erro
