ISO 19606:2017

INTERNATIONAL ISO
STANDARD 19606
First edition
2017-02
Fine ceramics (advanced ceramics,
advanced technical ceramics) — Test
method for surface roughness of
fine ceramic films by atomic force
microscopy
Céramiques techniques — Méthode d’essai pour la rugosité de surface
des films céramique fins par microscopie à force atomique
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
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ii © ISO 2017 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Test environment . 2
5 Roughness measurement specimens . 2
6 Test apparatus . 2
6.1 Cantilever . 2
6.2 Scanner . 2
6.3 Specimen stage . 3
7 Test apparatus calibration . 3
8 Probe-tip diameter evaluation standard plate . 4
9 Calibration of X-Y and Z scan axes . 4
10 Probe-tip error evaluation . 5
10.1 Outline of probe-tip error evaluation . 5
10.2 Measurements of preliminary Ra and RSm .6
10.3 Evaluation of probe-tip diameter . 6
10.4 Evaluation of error in roughness measurements . 8
11 Roughness measurements of specimen .13
12 Test report .14
Annex A (normative) Determination of D from D’ .16
Annex B (informative) Method to determine criteria for probe-tip error .18
Bibliography .24
Foreword
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This document was prepared by Technical Committee ISO/TC 206, Fine ceramics.
iv © ISO 2017 – All rights reserved

Introduction
Surface roughness measurements of fine ceramic thin films in nanometer scale by atomic force
microscopy have become one 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 the 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 evaluation 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 processes.
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 roughness
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 different sampling lengths to
process a primary profile can be applied to obtain appropriate values of arithmetic mean deviation of a
roughness profile, if necessary.
INTERNATIONAL STANDARD ISO 19606:2017(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Test method for surface roughness of fine
ceramic films by atomic force microscopy
1 Scope
This 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 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 μm to 2,5 μm.
2 Normative references
The 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 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 parameters
ISO 4288, Geometrical Product Specifications (GPS) — Surface texture: Profile method — Rules and
procedures for the assessment of surface texture
ISO 11039, Surface chemical analysis — Scanning-probe microscopy — Measurement of drift rate
ISO 11952, Surface chemical analysis — Scanning-probe microscopy — Determination of geometric
quantities using SPM: Calibration of measuring systems
ISO 18115-2, Surface chemical analysis — Vocabulary — Part 2: Terms used in scanning-probe microscopy
ISO 25178-2, Geometrical product specifications (GPS) — Surface texture: Areal — Part 2: Terms, definitions
and surface texture parameters
3 Terms and definitions
For 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 at http:// www .electropedia .org/
— ISO Online browsing platform: available at http:// www .iso .org/ obp
3.1
evaluation length
ln(X), ln(Y)
length of surface profile in the X or Y direction
3.2
probe-tip diameter evaluation standard plate
plate on which needle-shaped spikes are formed
Note 1 to entry: The plate is used to evaluate the probe-tip diameter (3.3).
3.3
probe-tip diameter
D
diameter of a probe tip at a distance of 10 nm from the tip end
4 Test environment
Testing shall be carried out only 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;
−3 2
d) mechanical vibration of the floor or the wall: 1 × 10 m/s (<100 Hz) or less.
5 Roughness measurement specimens
Specimens 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 the instrument being used.
6 Test apparatus
6.1 Cantilever
The cantilever shall be exclusively dedicated for a dynamic mode and commercially available. The
resonant frequency should be higher than 100 kHz.
6.2 Scanner
The scanner shall be capable of scanning cantilever or specimen stage by shifting the XYZ position. The
scanning area should be larger than 10 μm × 10 μm 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 the 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 reserved

Key
1 laser diode 6 specimen stage
2 light detector 7 X, Y and Z scanner
3 cantilever 8 Z-position control circuit
4 probe tip 9 X-Y scan circuit
5 specimen
Figure 1 — Schematic of AFM system
6.3 Specimen stage
The specimen stage shall be capable of supporting a specimen horizontally. The test area of the
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 calibration
This document only describes a method to evaluate the adequateness of a probe tip for fine-ceramic
thin-film surface roughness measurements 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.
8 Probe-tip diameter evaluation standard plate
A 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 600 nm;
— distance between any two nearest neighbour tips: 2,12 μm;
— plate size: 5 mm × 5 mm.
9 Calibration of X-Y and Z scan axes
The 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 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 μm and that the
step height is less than 20 nm.
The calibration 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 nearly 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 μm 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 along 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 the 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, draw 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 least 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 roughness 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
...