INTERNATIONAL ISO

STANDARD 25498

Second edition
2018-03

Microbeam analysis — Analytical

electron microscopy — Selected area
electron diffraction analysis using a
transmission electron microscope
Analyse par microfaisceaux — Microscopie électronique analytique
— Analyse par diffraction par sélection d'aire au moyen d'un
microscope électronique en transmission

Reference number
ISO 25498:2018(E)

© ISO 2018
ISO 25498:2018(E)


COPYRIGHT PROTECTED DOCUMENT

© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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 permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: [email protected]
Website: www.iso.org
Published in Switzerland

ii  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction................................................................................................................................................................................................................................. vi
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 3
4.1 General............................................................................................................................................................................................................ 3
4.2 Spot diffraction pattern.................................................................................................................................................................... 3
4.3 Kikuchi pattern........................................................................................................................................................................................ 6
4.4 Polycrystalline specimen................................................................................................................................................................. 7
5 Reference materials........................................................................................................................................................................................... 7
6 Equipment.................................................................................................................................................................................................................... 8
7 Specimens..................................................................................................................................................................................................................... 8
8 Experimental procedure............................................................................................................................................................................... 8
8.1 Instrument preparation................................................................................................................................................................... 8
8.2 Procedure for acquirement of selected area electron diffraction patterns......................................... 9
8.3 Determination of diffraction constant, Lλ .................................................................................................................... 12
9 Measurement and solution of the SAED patterns...........................................................................................................13
9.1 Selection of the basic parallelogram.................................................................................................................................. 13
9.2 Indexing diffraction spots............................................................................................................................................................ 15
10 180° ambiguity.....................................................................................................................................................................................................16
11 Uncertainty estimation..............................................................................................................................................................................16
11.1 Factors affecting accuracy........................................................................................................................................................... 16
11.2 Calibration with a reference material.............................................................................................................................. 17
Annex A (informative) Interplanar spacing................................................................................................................................................18
Annex B (informative) Spot diffraction patterns of single crystals for BCC, FCC and HCP
structure[7]...............................................................................................................................................................................................................19
Bibliography.............................................................................................................................................................................................................................. 38

© ISO 2018 – All rights reserved  iii

ISO 25498:2018(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 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 voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: www​.iso​.org/​iso/​foreword​.html.
This document was prepared by Technical Committee ISO/TC 202, Microbeam analysis, Subcommittee
SC 3, Analytical electron microscopy.
This second edition cancels and replaces the first edition (ISO 25498:2010), which has been technically
revised.
The main changes to the previous edition are as follows:
— the foreword has been revised;
— the introduction has been revised;
— the scope has been revised;
— the figure of Ewald construction has been deleted;
— the terms and definition of terminological entries 3.1, 3.2, 3.10, 3.11, 3.12, 3.13 and 3.14 have
been added;
— the subclause 4.1 has been added;
— Clause 5 has been revised;
— Clauses 4, 6, 7, and 10 and subclauses 8.1.5, 8.1.6, 8.2.1, 8.2.2, 8.2.4, 8.2.7, 8.2.8, 8.2.11 and 9.1.2 have
been editorially revised;
— the subclause 9.2.5 has been added;
— all formulae have been renumbered;
— Annex A has been revised;
— the subclause B.1 has been revised;

iv  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


— the figures have been modified;

— the bibliography has been updated.

© ISO 2018 – All rights reserved  v

ISO 25498:2018(E)


Introduction
Electron diffraction techniques are widely used in transmission electron microscopy (TEM) studies.
Applications include phase identification, determination of the crystallographic lattice type and
lattice parameters, crystal orientation and the orientation relationship between two phases, phase
transformations, habit planes and defects, twins and interfaces, as well as studies of preferred crystal
orientations (texture). While several complementary techniques have been developed, for example
microdiffraction, convergent beam diffraction and reflected diffraction, the selected area electron
diffraction (SAED) technique is the most frequently employed.
This technique allows direct analysis of small areas on thin specimens from a variety of crystalline
substances. It is routinely performed on most of TEM in the world. The SAED is also a supplementary
technique for acquisition of high resolution images, microdiffraction or convergent beam diffraction
studies. The information generated is widely applied in the studies for the development of new
materials, improving structure and/or properties of various materials as well as for inspection and
quality control purpose.
The basic principle of the SAED method is described in this document. The experimental procedure
for the acquirement of SAED patterns, indexing of the diffraction patterns and determination of the
diffraction constant are specified. ISO 25498 is intended for use or reference as technical regulation for
transmission electron microscopy.

vi  © ISO 2018 – All rights reserved

INTERNATIONAL STANDARD ISO 25498:2018(E)

Microbeam analysis — Analytical electron microscopy

— Selected area electron diffraction analysis using a
transmission electron microscope

1 Scope
This document specifies the method of selected area electron diffraction (SAED) analysis using a
transmission electron microscope (TEM) to analyse thin crystalline specimens. This document applies
to test areas of micrometres and sub-micrometres in size. The minimum diameter of the selected area
in a specimen which can be analysed by this method is restricted by the spherical aberration coefficient
of the objective lens of the microscope and approaches several hundred nanometres for a modern TEM.
When the size of an analysed specimen area is smaller than that restriction, this document can also
be used for the analysis procedure. But, because of the effect of spherical aberration, some of the
diffraction information in the pattern can be generated from outside of the area defined by the selected
area aperture. In such cases, the use of microdiffraction (nano-beam diffraction) or convergent beam
electron diffraction, where available, might be preferred.
This document is applicable to the acquisition of SAED patterns from crystalline specimens, indexing
the patterns and calibration of the diffraction constant.

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/IEC 17025, General requirements for the competence of testing and calibration laboratories

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​
3.1
Miller index
notation system for crystallographic planes and directions in crystals, in which a set of lattice planes or
directions is described by three axes coordinate
3.2
Miller-Bravais index
notation system for crystallographic planes and directions in hexagonal crystals, in which a set of
lattice planes or directions is described by four axes coordinate
3.3
(h k l)
Miller indices (3.1) of a specific set of crystallographic planes

© ISO 2018 – All rights reserved  1

ISO 25498:2018(E)


3.4
{hkl}
Miller indices (3.1) which denote a family of crystallographic planes
3.5
[uvw]
Miller indices (3.1) of a specific crystallographic direction or a zone axis
3.6
interplanar spacing
dhkl
perpendicular distance between consecutive planes of the crystallographic plane set (h k l) (3.3)
3.7
(uvw)*
notation for a set of planes in the reciprocal lattice
Note 1 to entry: The normal of the reciprocal plane (uvw)* is parallel to the crystallographic zone axis [uvw] (3.5).

3.8
reciprocal vector
ghkl
vector in the reciprocal lattice
Note 1 to entry: The reciprocal vector, ghkl, is normal to the crystallographic plane (h k l) (3.3) with its magnitude
inversely proportional to interplanar spacing d hkl (3.6).

3.9
R vector
Rhkl
vector from centre, 000 (the origin), to the diffraction spot, hkl, in a diffraction pattern
Note 1 to entry: See Figure 1.

3.10
camera length
L
effective distance between the specimen and the plane where diffraction pattern is formed
[SOURCE: ISO 15932:2010, 3.7]
3.11
camera constant
Lλ
product of the wavelength of the incident electron wave and camera length (3.10)
Note 1 to entry: Because of the small Bragg angle, the Bragg condition can be given in the first-order
approximation, R hkl ⋅ d hkl ≅ Lλ , where dhkl is the interplanar spacing of plane, (hkl), (3.3) and R hkl (3.9) is the
distance of the diffraction spot, hkl, from the incident beam.

[SOURCE: ISO 15932:2010, 3.8, modified]

3.12
bright field image
image formed using only the non-scattered beam, selected by observation of the back focal plane of the
objective lens and using the objective aperture to cut out all diffracted beams
[SOURCE: ISO 15932:2010, 5.6]

2  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


3.13
dark field image
image formed by a diffracted beam only by using the objective aperture for selection or by collecting
the diffracted beam with an annular dark-field detector
[SOURCE: ISO 15932:2010, 5.6]
3.14
energy-dispersive X-ray spectroscopy
EDS
analytical technique which enables the elemental analysis or chemical characterization of a specimen
by analysing characteristic X-ray emitted by the matter in response to electron irradiation
[SOURCE: ISO 15932:2010, 6.6]
3.15
eucentric position
specimen position at which the image exhibits minimal lateral motion resulting from specimen tilting

4 Principle

4.1 General
When an energetic electron beam is incident upon a thin crystallographic specimen in a transmission
electron microscope, a diffraction pattern will be produced in the back focal plane of the objective lens.
This pattern is magnified by the intermediate and projector lenses, then displayed on a viewing screen
and recorded (see Reference [3]). This pattern can also be displayed on a monitor if the TEM is equipped
with a digital camera system.

4.2 Spot diffraction pattern

The diffraction pattern of a single crystal appears as an array of “spots”, the basic unit of which is
characterized by a parallelogram. A schematic illustration of a spot diffraction pattern is shown in
Figure 1. Each spot corresponds to diffraction from a specific set of crystal lattice planes in the
specimen, denoted by Miller indices (hkl). The vector, Rhkl, is defined by the position of the diffracted
spot, hkl, relative to position on the pattern corresponding to the transmitted beam, i.e. the centre-
spot, 000, of the pattern. It is parallel to the normal of the reflecting plane, (hkl). The magnitude of Rhkl
is inversely proportional to the interplanar spacing, dhkl, of the diffracting plane, (hkl) (see References [4]
(
to [9]). In the context of this document, vectors R h1 k1 l1 , R h2k 2l2 , R h2k 2l2 − R h1 k1 l1 ) and

(Rh k l
2 22
+ R h1k1 l1 ) are simplified as R1, R2, R2−1 and R1+2, respectively. The included angle between
vectors, R1 and R2, is denoted by γ*. The basic parallelogram is defined by R1 and R2, where they are the
shortest and next shortest in the pattern respectively and not along a common line. The spot, h2k2l2, is
positioned anticlockwise around the centre spot relative to spot, h1k1l1.
Because the centre-spot is often very bright, it is often difficult to determine the exact centre of the
pattern. Therefore, a practical procedure is to establish the magnitude of R hkl by measuring the
distance between the spots, hkl and hk l on the diffraction pattern and dividing by two,
1
(
i.e. R hkl = R hkl + R
2 hk l )
. Figure 2 shows an example of the SAED pattern where the magnitude of R1,

R2 and R2−1 is obtained from

1
2
(
R1 + R1 ,
1
2
) (
R2 + R2 and
1
2
) ( )
R2−1 + R2−1 respectively.

© ISO 2018 – All rights reserved  3

ISO 25498:2018(E)


Key
R1 vector from 000 to spot, h1k1l1, the shortest vector in the diffraction pattern
R2 vector from 000 to spot, h2k2l2, the next shortest vector

NOTE The basic parallelogram is constituted by diffraction spots, h1k1l1, h2k2l2, (h1+h2, k1+k2, l1+l2), and
central spot, 000.

Figure 1 — Schematic spot diffraction pattern from a single crystal

Key
R1 vector from 000 to spot, h1k1l1, the shortest vector in the diffraction pattern
R2 vector from 000 to spot, h2k2l2, the next shortest vector

NOTE The basic parallelogram is constituted by R1 and R2.

Figure 2 — Example of SAED spot pattern

4  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


The relationship between the interplanar spacing, dhkl, and the magnitude, Rhkl, for a reflecting plane,
(hkl), can be approximately expressed as shown in Formula (1) (see References [7] and [8]):

 3 2
Lλ = R hkl × d hkl 1 − ( R hkl / L )  = R hkl × d hkl (1 − ∆ ) (1)
 8 
where

( R hkl / L ) 2 ;
3
∆ is equal to
8
L is the diffraction camera length and equal to fo × Mi × Mp;

where

fo is the focal length, in millimetres, of the objective lens in the microscope;

Mi is the magnification of the intermediate lens;

Mp is the magnification of the projector lenses;

Lλ is the camera constant (or diffraction constant) of the transmission electron microscope
operating under the particular set of conditions. This parameter can be determined from the
diffraction pattern of a crystalline specimen of known lattice parameters (see 8.3);

λ is the wavelength, in nanometres, of the incident electron beam which is dependent upon the
accelerating voltage and can be given by Formula (2) (see Reference [4]):

           λ ( nm ) =
1 , 226
(2)
(
V 1 + 0 , 978 8 × 10 −6 V )
where V is the accelerating voltage, in volts, of the TEM; the factor in parenthesis is the relativistic
correction.
For most work using a TEM, the value of Δ in Formula (1) is usually smaller than 0,1 % and, hence, a
more simplified Formula (3) may be used, namely
R hkl ⋅ d hkl ≅ Lλ (3)

For the derivation of the above equation, refer to the textbooks (see References [4] to [9]).
The use of Formula (3) requires measuring the length of Rhkl. Since, as mentioned earlier, the location of
the pattern centre may not be easily determined; it is recommended that the distance measurement
taken, 2R h1 k1 l1 , be from the h1k1l1 diffracted spot to the h1 k 1 l1 spot on the pattern. This is equivalent
to a diameter measurement on the ring pattern from a polycrystalline specimen. To obtain the
interplanar information, the measured distance, 2R h1 k1 l1 ,is halved and Formula (3) applied.
If the camera constant is known, the interplanar spacing, d hkl , of plane, (hkl), can be calculated.
The included angle between any two vectors, R h1 k1 l1 and R h2k 2l2 , can also be measured on the
diffraction pattern. This is equal to the angle between the corresponding crystallographic planes,
( h1 k1 l1 ) and ( h2k 2l2 ) .
Since diffraction data from a single pattern will provide information on a limited number of the possible
diffracting planes in a specimen area, it is necessary to acquire additional diffraction patterns from the
same area (or from different grains/particles of the same phase). This requires either the tilting of the
specimen or the availability of differently oriented grains or particles of the same phase.
Acquire a second diffraction pattern from another zone axis from the same area by tilting (or tilting and
rotating) the specimen so that the two patterns contain a common spot row (see 8.2.10 and Figure 5).

© ISO 2018 – All rights reserved  5

ISO 25498:2018(E)


Index the diffracted spots, and then select three non-planar spots in the two patterns to constitute
a reciprocal lattice, which, if the spots correspond to low values of Miller indices, may define the
primitive unit cell of the crystal lattice. Therefore, crystal lattice parameters can be determined and
the orientation of the grain or particle in the thin specimen can also be calculated.

4.3 Kikuchi pattern

When a specimen area is nearly perfect but not thin enough, Kikuchi lines may occur. They arise from
electrons scattered inelastically through a small angle and suffering only a very small energy loss being
scattered again, this time elastically. This process leads to local variations of the background intensity
in the diffraction pattern and the appearance of Kikuchi lines.
The Kikuchi patterns consist of pairs of parallel bright and dark lines, which are parallel to the
projection of the corresponding reflecting plane, (hkl). The bright (excess) line and dark (defect) line in
the Kikuchi pattern are denoted by K B −hkl and K D−hkl , respectively. Therefore, the line pair, K B −hkl
and K D−hkl , will be perpendicular to the vector, Rhkl from the corresponding crystallographic plane
(hkl). Namely they are perpendicular to the reciprocal vector, g hkl , of the plane, (hkl).
An example of a Kikuchi pattern is given in Figure 3, where the bright line, K B −hkl , and dark line,
K D−hkl , pair is superimposed on the spot pattern. The perpendicular distance, DK −hkl , between the
line pair, K B −hkl and K D−hkl , is related to the interplanar spacing, d hkl , and camera constant, Lλ, by
Formula (4).
DK −hkl ⋅ d hkl ≅ Lλ (4)

Key
KB−hkl bright line of Kikuchi pair
KD−hkl dark line of Kikuchi pair
D K −hkl distance between the line pair K B −hkl and K D −hkl
+ centre of the direct beam

Figure 3 — Kikuchi pattern from a steel specimen

The distance between the two Kikuchi lines equals to the distance between the diffraction spot, hkl,
and the central spot, 000. The angles between intersecting Kikuchi pairs are the same as the angles

6  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


between their corresponding diffraction spots, and can be measured accurately. These angles are also
equal to the angles between the relevant crystallographic planes.
When the specimen is tilted, the diffraction spots only gradually change the brightness, faint or increase
the intensity, but their positions are almost at the same place. Instead, Kikuchi lines are sensitive to
the tilting. Their movement is significant on the viewing screen. Hence, specimen tilting can be guided
by Kikuchi map from one zone axes to another one. The Kikuchi patterns present the real crystal
symmetry of the specimen. They can also be used in establishing crystal orientation with a very high
accuracy (see References [5] and [9]).
The problem is that Kikuchi patterns cannot always be observed in all of the specimens. In most cases,
the SAED studies rely mainly on the spot patterns, though they are not as accurate as Kikuchi patterns.

4.4 Polycrystalline specimen

For randomly oriented aggregates of polycrystals, the diffraction pattern is comprised of a series of
concentric rings centred on the spot, 000, of the direct beam. An example of the pattern from
polycrystalline gold (Au) specimen is given in Figure 4. Each diffracted ring arises from the diffraction
beams from differently oriented crystallographic planes of the form, {hkl}; each of these having an
identical interplanar spacing. From the diameter of each diffraction ring, the corresponding interplanar
spacing, d hkl , can be calculated using Formula (3). Indices of the diffraction rings can be ascribed and
then the lattice parameters can also be determined. For the method of indexing ring patterns, refer to
that used in X-ray powder diffraction (see Reference [9]).

Figure 4 — Diffraction ring pattern with indices from a polycrystalline Au specimen

5 Reference materials
A reference specimen is required for determining the diffraction constant, Lλ, of the microscope in
electron diffraction studies. In principle, any thin crystalline foil or powder could be considered as
the reference specimen, provided its crystalline structure and lattice parameters have been acquired
accurately and they are certified and stable under irradiation of the electron beam. It should be
ensured that the reference material, which is as thin as electrons can penetrate through it, has the same
crystallographic properties as the bulk material. In addition, a number of sharp diffraction rings or
spots with known indices can be observed. The thickness of the crystal foil or powder grain size should
be consistent with the beam energy and the quality of the diffraction pattern so that clear diffraction
patterns can be observed (when it is too thick, the pattern will lack sharpness).

© ISO 2018 – All rights reserved  7

ISO 25498:2018(E)


Reference materials in common use are polycrystalline specimens made from pure gold [which has a
face-centred cubic (FCC) lattice with parameter, a = 0,407 8 nm] or pure aluminium (Al) (FCC structure
with lattice parameter a = 0,404 9 nm). The mass fraction of Au or Al in the reference materials shall be
not less than 99,9 %. The reference specimen shall be prepared by evaporating a small piece of Au or Al
on a grid with a supporting film.
It is also feasible to evaporate a layer of the reference material onto a local surface area of the specimen,
which is to be analysed.

6 Equipment

6.1 Transmission electron microscope (TEM) shall be with double tilt or tilt rotation or double-tilt
rotate specimen holder.

6.2 Recording of SAED patterns and images.

The SAED patterns and images obtained on the transmission electron microscope shall be recorded on
the photographic films or imaging plates or an image sensor built in the digital camera.
When films are used, a darkroom with a negative developing and fixing outfit is required.

6.3 Facilities for specimen preparation.

7 Specimens

7.1 Most specimens are prepared as thin foils (see References [2] and [10]). Such specimens can be
obtained in the form of thin sections from a variety of crystalline substances including metallic and non-
metallic materials. The shape and external size of the specimen should match that of the TEM specimen
holder or, alternatively, it can be held by a support grid.

Fine powders and/or extraction replicas can also be used. These specimens shall be prepared on the
grid with supporting films.

7.2 An applicable area to be tested is in the sizes of micrometre and sub-micrometre. The area is
always defined by selected aperture. The selected area shall be thin enough for the electron beam to pass
through it and diffraction patterns can be observed on the viewing screen.

7.3 The surface of the specimen shall be clean, dry and flat without an oxidizing layer or any
contamination.

7.4 For those materials that are stable under energetic particle beam bombardment, contamination
on the specimen surface can be avoided or removed by ion beam sputtering or other techniques, such as
plasma cleaners, before the TEM observation.

7.5 Prepared specimens shall be labelled and placed in a special specimen box and preserved in a
desiccator or evacuated container.

8 Experimental procedure

8.1 Instrument preparation

8.1.1 The general working condition of the TEM laboratory shall comply with ISO/IEC 17025.

8  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


8.1.2 It is recommended to use the cold finger of TEM before conditioning in order to minimize
specimen contamination.

8.1.3 When the vacuum of the transmission electron microscope is suitable for operation, switch on
and select an appropriate accelerating voltage so that the incident electron beam can penetrate through
the specimen.

8.1.4 Carry out the axis alignment for the electron optical system.

8.1.5 The success of the selected area electron diffraction method relies on the validity of indexing
the diffraction patterns arising, irrespective of which axis in the specimen lies parallel to the incident
electron beam. Such analysis is therefore aided by specimen tilt and rotation facilities.

Place the specimen to be tested and the reference firmly in the double-tilting or tilting-rotation or
double-tilting rotation specimen holder, and insert the holder into the specimen chamber.
A specimen coated with an evaporated layer of reference material can be directly placed in the specimen
holder and inserted into the chamber.

8.1.6 When the SAED patterns need to be related to features observed in the corresponding micrograph,
the angle of rotation between the two may need to be determined and compensated for.

The method in common use is to take a diffraction pattern and a micrograph of a molybdenum trioxide
crystal specimen. The rotation angle of the image is then measured on the photographic plates, on which
the micrograph and superimposed diffraction pattern has been recorded. For details of the calibration
procedure, refer to the appropriate text books (see References [4], 5] and [9]).
When the rotation angle of the TEM has been compensated by the manufactory, the procedure in 8.1.6
may be ignored.

8.1.7 When a digital camera is equipped and to be employed for the study, set the camera in operating
condition by following the user’s guide of the manufacturer.

To avoid damaging the camera, reduce incident beam intensity and use beam stop to block the central
spot when acquiring SAED diffraction patterns.
For detail procedure of the operation and calibration, refer to instruction from the manufacturer.

8.2 Procedure for acquirement of selected area electron diffraction patterns

8.2.1 Obtain a magnified bright field image of the specimen on the viewing screen of the transmission
electron microscope. Adjust the specimen height to focus the image so that the image movement is
minimized during the tilting of the specimen. Namely, set the eucentric position of the specimen. The
procedure for establishing the eucentric position of the specimen may be obtained by consulting the
manufacturer's operating manual.
NOTE If the TEM is not equipped with a specimen height control function, this procedure can be omitted.

8.2.2 Adjust the magnification of the specimen image until details in the specimen can be observed
clearly. A suitable magnification for SAED analysis is usually from several thousands to tens of
thousands times. Focus the image and correct the astigmatism.

8.2.3 Insert the field limiting aperture (selected area aperture) and focus the image of this aperture.
Then focus the specimen image again. This makes the selected area aperture plane conjugate with the
image plane of the objective lens.

© ISO 2018 – All rights reserved  9

ISO 25498:2018(E)


8.2.4 Switch the microscope from image mode to the SAED mode, focus the image of the objective lens
aperture; that is, make this objective lens aperture coincide with the back focal plane of the objective
lens. Return to the bright field image mode and focus the image again.

8.2.5 Insert the reference (i.e. the calibration standard) and locate it at the eucentric position. Choose
a camera length, L, consistent with the capabilities of the subsequent measuring equipment and then
obtain a diffraction pattern from it. Focus the diffraction pattern and correct any astigmatism carefully to
make the diffraction pattern sharp. Record the diffraction pattern of the reference.

8.2.6 If the reference and test specimen are not in the same specimen holder, withdraw the reference
and insert the test specimen again, without changing the operating conditions and without switching the
microscope off. Again, locate it at the eucentric height.

8.2.7 Obtain a focused bright field image of the specimen again with an appropriate magnification.

Select a region of interest (ROI) on the specimen image using the field limiting aperture (selected area
aperture). Record the image of this ROI in the specimen. The phase boundaries and/or grain boundaries
in the specimen should be kept away from the selected ROI when a single crystal grain is analysed.

8.2.8 Switch the TEM to the SAED diffraction mode again, withdraw the objective lens aperture and
obtain a diffraction pattern on the viewing screen. Where possible, tilt the specimen slightly so that the
brightness of the spots in the diffraction pattern is evenly distributed, or where Kikuchi lines appear; the
Kikuchi line pairs are symmetrical about the pattern centre.

This pattern will then derive from a low index direction in the crystal approximately; the direction is
antiparallel to the incident electron beam. This crystal direction will be the zone axis, u1 v 1 w 1  , which
is the normal of the reciprocal plane, (u1 v 1 w 1 )* , i.e. the diffraction pattern (see References [4] to [7]).
NOTE The beam direction is defined as antiparallel to the incident electron beam.

Adjust (defocus) the second condenser lens current (the brightness knob) to sharpen the diffraction
spots, making them as sharp as possible.

8.2.9 Record the pattern or/and save the original uncompressed pattern in the computer system. Take
note of the reading on the X and Y axis of the specimen tilting device as X1 and Y1, respectively. Using
dark field conditions either by beam tilt or shifting the objective lens aperture, identify the source of the
pattern.

8.2.10 Insert the reference specimen and obtain a second diffraction pattern from the reference. Record
this diffraction pattern (see also 8.3), making sure that the same experimental conditions are used (i.e.
accelerating voltage, lens settings and, especially, the specimen height and camera length, L).

8.2.11 Obtain sufficient data for each phase of interest by either of the following procedures.

a) Specimen tilting procedure: obtain the second pattern by tilting the specimen.
Choose a row of close-spaced diffraction spots collinear with the central transmitted spot on the
diffraction pattern, which is denoted by indices of reciprocal plane, (u1 v 1 w 1 )* . Keep this row of
the spots visible on the viewing screen, while tilting the specimen until the second diffraction
pattern, (u2v 2w 2 )* appears. Make sure the brightness of the spots in the second pattern is evenly
distributed. The reciprocal space geometry of the two patterns is schematically illustrated in
Figure 5. The angle between the diffraction patterns, (u1 v 1 w 1 )* and (u2v 2w 2 )* , is Ψ, which
equals to the angle between the two zone axes, u1 v 1 w 1  and u2v 2w 2  . This angle can be
determined from the tilt angle of the specimen holder.

10  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


If Kikuchi patterns are visible, the specimen tilting can be guided by the Kikuchi map. The second
diffraction pattern (or more patterns) may be obtained directly.
With a rotate-tilt specimen holder or a double-tilting rotate holder, a chosen row of the spots can be
aligned with a tilt axis; the second diffraction pattern (or more patterns) may be obtained directly.
Repeat the procedure described in 8.2.8, recording the pattern and/or saving it on the computer
system. Take note of the reading on the X and Y axis of the specimen-tilting device as X2 and Y2,
respectively.
b) Multi grains procedure: obtain the patterns from several areas, i.e. different particles or grains of
the same phase. This procedure is recommended for any of the following situations:
1) the maximum tilting angle of the specimen holder is not large enough, so that the second
diffraction pattern cannot be reached by tilting;
2) the particles to be analysed in the specimen are too small;
3) the specimen is sensitive to the electron beam illumination, e.g. the selective area is
contaminated or decomposes following a short irradiation by the electron beam.
When this procedure is employed, the source of each diffraction pattern is necessary to confirm.
Choose appropriate diffraction spots to form a dark field image to check it. Further confirmation
can be achieved through simultaneous use of an EDX (energy dispersive X-ray spectrometry)
facility, when available.

8.2.12 When the diffraction patterns are recorded on negative films, develop, fix and dry the films in the
darkroom. Keep the negative films one by one in individual protective bags with labels.

8.2.13 When the diffraction patterns are recorded by digital camera or imaging plates, save the original
uncompressed diffraction patterns in the computer system as individual files with labels. All parameters
of the acquisition of this file shall be documented and reported.

8.2.14 Each pattern, either recorded on negative film or by digital camera as well as by imaging plate,
shall be numbered and labelled with the following information: specimen designation and serial number,
accelerating voltage, nominal camera length, L, tilting angles, operator, date, etc. All processing operations
of the diffraction patterns and images shall be reported.

© ISO 2018 – All rights reserved  11

ISO 25498:2018(E)


Key

ψ angle between the diffraction pattern ( u1 v 1 w 1 ) * and ( u 2 v 2 w 2 ) *

′
R1 = R 2
a Tilting axis.

Figure 5 — Reciprocal space geometry of the spot diffraction patterns

8.3 Determination of diffraction constant, Lλ

8.3.1 The procedure for the determination of the diffraction constant uses a reference specimen such
as polycrystalline pure gold or pure aluminium (see Clause 7). Figure 4 shows an example of the ring
patterns from a polycrystalline gold specimen. Record the diffraction pattern (see 8.2).

8.3.2 When diffraction patterns are recorded on photographic films, place the negative film on
which the diffraction pattern of the reference specimen was recorded, emulsion side up on the film
viewer. Measure the diameters of the diffraction rings on the film of the reference specimen when a
polycrystalline reference is used. Note the diameter of these rings from inner to outer as D1, D2, D3, D4, …
(mm), etc., respectively.

8.3.3 Indices, hkl, of the diffraction rings for a reference specimen with FCC structure are 111, 200,
220, 311, 222, 400, 331, 420, 422, … respectively from the inner to outer rings (see Figure 4). The
corresponding interplanar spacings, d hkl , are given for both Au and Al in Annex A or calculated by the
crystallographic formulae (see References [4] to [9]).

12  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


8.3.4 According to Formula (3), calculate the diffraction constants as follows:

L1 λ = D1 ⋅ d 111 / 2 (mm⋅nm)

L2 λ = D2 ⋅ d 200 / 2 (mm⋅nm)

L3 λ = D3 ⋅ d 220 / 2 (mm⋅nm) …, etc.

8.3.5 Plot the Lλ − D / 2 curve using the data in 8.3.2 and 8.3.4 (an example of the Lλ − D / 2 plot is
shown in Figure 6). This graph could be used for all reflections (spots) from the specimen being analysed
under completely identical conditions. Since the diffraction constant, Lλ , actually varies slightly with the
diffraction ring diameter, it is recommended either

a) to use the Lλ − D / 2 curve to obtain the value of Lλ corresponding to the same distance, D/2, as the
spot being measured, or
b) to use an average value of the camera constant and subsequently make allowance for the small
uncertainty this will produce in the d-value obtained.

8.3.6 When the diffraction patterns are recorded by the digital camera, the above measurements and
calculations can be carried out by the computer system.

Figure 6 — Lλ − D / 2 curve from a polycrystalline Au specimen

9 Measurement and solution of the SAED patterns

9.1 Selection of the basic parallelogram

9.1.1 When photographic films are used for recording diffraction patterns, place the film, on which the
diffraction pattern was recorded, on the film viewer with its emulsion side up.

9.1.2 Select two diffracted spots, h1 k 1 l1 and h2 k 2 l 2 , from the diffraction pattern with zone axis,
u1 v 1 w 1  , such that these spots are the nearest and next nearest to the central spot, 000, respectively.
They shall not be collinear with the centre-spot, 000. The spot, h2 k 2 l 2 , is positioned anticlockwise

© ISO 2018 – All rights reserved  13

ISO 25498:2018(E)


around the centre spot relative to spot, h1 k 1 l1 . The two diffracted spots, the centre-spot and the spot,
( h1 + h2 , k1 + k 2 , l1 + l2 ) , constitute a parallelogram (see Figure 1).
Measure the distance, 2R1 between the spots, h1 k 1 l1 and h1 k 1 l1 , and the distance, 2R2 , between the
spots, h2 k 2 l 2 and h2 k 2 l2 , to get the magnitude of the vectors, R1 and R2 (see Figures 1 and 2). The
corresponding angle, γ*, between R1 and R2 shall also be measured.
Where individual patterns are obtained, obtain the magnitude of the vectors, R1+2 and R2−1 (see
Figures 1 and 2). The angles between R1 and R2−1 , between R2−1 and R2 and the angle between R1
and R2 shall be measured. These are φ3 , φ2 and φ1 respectively, and φ3 + φ2 � = φ1 .

9.1.3 The angles φ3 , φ2 and φ1 can be calculated using Formulae (5), (6) and (7):

(
 )
φ1 = cos −1  R12 + R22 − R12+2 / 2R1 R2 

(5)

(
 )
φ2 = cos −1  R22 + R22−1 − R12 / 2R2 R2−1 

(6)

(
 )
φ3 = cos −1  4 R12 + R22−1 − R12+2 / 4 R1 R2−1 

(7)

If φ1 = φ2 � + φ3 within the tolerances set by the uncertainty, then proceed; otherwise, check R s and φ s .

9.1.4 Perform the same procedure as described in 9.1.3 on the second diffraction pattern with zone
axis, u2v 2w 2  (and on any others from different directions of the specimen). The basic parallelogram
on the second pattern is constituted by R1′ and R2′ and the centre-spot, 000. The vector, R1′ , shall be
superimposed over the vector, R2 , of the pattern with zone axis, �u1 v 1 w 1  , i.e. R1′ = R2 � (see Figure 5).
Measure the magnitude of R1′ and R2′ as well as the angle, β*, between R1′ and R2′ . The vectors, R1 , R2
and R2′ constitute a basic cell of the reciprocal space. If the corresponding diffraction spots possess the
lowest indices, then the reciprocal unit cell can be obtained.

9.1.5 When a digital camera is employed, measurement and calculation on the diffraction patterns
can be carried out by the computer system.

9.1.6 The angle, α*, between R1 and R2′ (see Figure 5) may be calculated using Formula (8):

cos α * = sin γ * × sin β * × cosψ + cos γ * × cos β * (8)

where

β * is the angle between R1′ and R2′ ;

γ * is the angle between R1 and R2 ;

is the angle between the diffraction patterns, ( u1 v 1 w 1 )* and ( u2v 2w 2 )* , or the zone axes,
ψ
u1 v 1 w 1  and u2v 2w 2  .

14  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


9.2 Indexing diffraction spots

9.2.1 Use Formula (3) to calculate the interplanar spacing, d hkl , corresponding to the above diffraction
spots. The interplanar spacing, d hkl , can also be acquired by measuring the distance, DK −hkl , between
the Kikuchi bright and dark line pair and using Formula (4).

9.2.2 ( ) ( )
Arbitrarily index two of the spots, say h1 k 1 l1 and h2 k 2 l 2 , and then confirm from the possible
indices of the other spots that:

h3 = h2 − h1, k3 = k2 − k1, l3 = l2 − l1, and

h4 = h2 + h1, k4 = k2 + k1, l4 = l2 + l1.

Make any allowance for the multiplicity of {h j k j l j } . If no solution is possible, then recheck the
determination of di and the angles (see 9.1.3) until one is found that satisfies these requirements within
the tolerances. All spots in a continuous pattern will come from a common zone, [uvw], and have a
common axis. This direction is given by Formula (9). The direction, [uvw], can be checked since for all
(hkl)'s indexed
hu + kv + lw = 0 (9)

9.2.3 Calculate the characteristic parameters of the two-dimensional primitive cell on each reciprocal
lattice plane of the crystal specimen in advance, namely the indices, �h1 k 1 l1 and h2 k 2 l 2 , of the primitive
reciprocal vector, g1 and g2 , ratio of the magnitudes, g2 : g1 , the included angle between the vectors
g1 and g2 and the zone axis index.

The zone axis index, [uvw], can be obtained using Formula (10):

 k1 l1 l1 h1 h1 k1 
u:v:w =  : :  = ( k 1 l 2 − l1 k 2 ):( l1 h2 − h1 l 2 ):( h1 k 2 − k 1 h2 )  (10)
k
 2 l2 l2 h2 h2 k 2  

The values of u, v, w should be integers without a common factor. The zone axis index, uvw  , is in
terms of the normal of reciprocal plane. It shall be converted to the crystallographic direction index,
UVW  , in real space by the crystallographic relation. The crystallographic formulae usually can be
obtained from the literature and/or handbooks (such as References [4], [5], [6], [7] and [9]). Only for
cubic crystals the index, uvw  , of the reciprocal space are not needed to convert, which is equal to the
index, UVW  , in the real space.
For the convenience of users of this document, the standard spot patterns of cubic systems and a
close-packed hexagonal system with low indices are given in Annex B. For those specimens with a
lower symmetry, reference to a diffraction database such as “The Powder Diffraction File 1997–2007”,
published by the International Centre for Diffraction Data (ICDD), is recommended (see Reference [11]).
Software is also very useful in establishing the reciprocal planes of the crystal specimen, especially in
one with low symmetry structure (see References [4] and [9]).
For an unknown specimen, the chemical composition should also be determined by microanalysis (e.g.
EDX analysis) and/or chemical analysis so that the specimen phase can be identified.

9.2.4 Compare the geometrical characteristics of the experimental diffraction patterns, including the
ratio, R2 / R1 and R2−1 / R1 , the included angle between R1 , R2 and R2−1 , respectively, with the
calculated characteristic parameters of the primitive cell. If the experimental value is consistent with the
known value within error, the diffraction spots can be indexed as �h1 k 1 l1 , h2 k 2 l 2 and

© ISO 2018 – All rights reserved  15

ISO 25498:2018(E)


( h2 − h1 , k2 − k1 , l2 − l1 ) , respectively. The indices of other diffraction spots can be obtained by the

summation of the corresponding vectors. Therefore, the zone axis index, [uvw], can be worked out.

9.2.5 For beam-sensitive nanocrystals, it is often incapable to collect a tilting series of the diffraction
patterns from a single nanocrystal. The method that uses randomly oriented diffraction patterns with
unknown angular relationships may apply. The key point of this approach is to construct a principal facet
by the lengths of the two basis vectors and the angle between them in the diffraction pattern. Based
on matching the observed crystal facets to model facets extracted from a simulated three-dimensional
lattice, the potential unit cell can be determined. The diffraction pattern can also be indexed. For detail
procedure of this algorithm, refer to references (see References [12] and [13]).

10 180° ambiguity
The indices in a diffraction pattern with only one zone axis from a single crystal are not decided
uniquely because of the 180° ambiguity created by the diffraction effect. Therefore, the spots, h1 k 1 l1
and h2 k 2 l 2 , can also be indexed as �h1 k 1 l1 and h2 k 2 l2 , respectively, and vice versa, except that higher
Laue zone diffraction spots can be obtained.
However, this ambiguity may be removed by the following methods.

a) After recording a diffraction pattern, u1 v 1 w 1  , tilt the specimen while keeping a row of spots
bright, containing the central spot, until another zone axis pattern, u2v 2w 2  , appears. Record the
second pattern and determine the included angle between the two patterns (see 8.2.11). Index the
two patterns so that all the indices are entirely self-consistent. The angle between the two patterns
shall coincide with the tilting angle.

b) Obtain a diffraction pattern with zone axis, u1 v 1 w 1  , which is superposed on another pattern,
u2v 2w 2  , from the same crystal. Index the two patterns self consistently.
c) Tilt the specimen to get three non-parallel Kikuchi line pairs in one pattern. Unambiguous indices
can be gained.

11 Uncertainty estimation

11.1 Factors affecting accuracy

The camera constant will change if the high voltage supply to the electron microscope fluctuates.
Normally, stabilization ratios are 105 to 1 or better and thus, this effect is minimal.
As discussed in Clause 4, the effective camera length is defined as Formula (11) (see Reference [7]):
L = fo × Mi × Mp (11)

where

Mi is the magnification of the intermediate lens;

Mp is the magnification of the projector lens;

fo is the focal length of the objective lens, the most sensitive factor which affects the
reproducibility of L.

16  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


In turn, f o depends on the plane of the object. The factors that control this are specimen holders of
different length, support grids that are not flat, thick and buckled specimens, and the effects due to
tilting the specimen.
Faulty lens settings will alter 2Lλ if the correct procedure for obtaining diffraction settings is not
followed. It can be shown in Formula (12):

∆L ∆f o ∆M i ∆M p
= + + (12)
L fo Mi Mp
where

ΔL/L is the proportional error in the camera length, L;

Δfo/fo is the proportional error in the focal length f o of the objective lens;

ΔMi/Mi is the proportional error in the magnification of the intermediate lens;

ΔMp/Mp is the proportional error in the magnification of the projector lens.

In some instruments, the strength of the projector lens is fixed so that ∆M p / M p = 0 . However, in other
instruments, the projector current is variable and the accuracy of the setting has a marked effect on
2Lλ. ΔMi/Mi is the error in re-adjusting the intermediate lens strength to image the diffraction pattern
from the back focal plane of the objective lens. This adjustment can be made with considerable accuracy,
so ΔMi/Mi is usually very small.

11.2 Calibration with a reference material

Measurement of “d” spacing involves the use of a reference material so that the camera constant, 2Lλ,
can be determined and the effects of variation in microscope parameters can be ignored, provided the
conditions for obtaining the diffraction pattern of the standard and unknown are identical. Thus, the
main errors involved in the determination of the camera constant, and consequently the d values, arise
from inaccuracies in the measurement of rings and spots.
Lens aberration may lead to distortion of diffraction rings into ellipses and thus, measurements of
diameter shall be made at least six positions when determining the Lλ − D / 2 curve to determine the
minimum and maximum values of the diameters (see 8.3.5). Thus, the standard deviation in the camera
constant value, S cc , can be determined from this calibration curve. Errors involved in the determination
of the spot or ring diameters can be estimated from replicate measurements of these values and an
evaluated standard deviation, S d . This uncertainty shall be combined with the calibration uncertainty
associated with the measuring instrument, S m , and thus yield an uncertainty related to spot or ring
dimensions. Thus, the combined uncertainty for determination of d values is expressed by Formula (13).

u = (s cc )2 + (s d )2 + (s m )2 (13)

© ISO 2018 – All rights reserved  17

ISO 25498:2018(E)


Annex A
(informative)

Interplanar spacing

A.1 Interplanar spacing of pure Au and Al

The interplanar spacings, d hkl , of pure gold and aluminium are listed in Table A.1.

Table A.1 — Interplanar spacing, d hkl , of pure Au and Al

Dimensions in nanometres
Miller indices of Interplanar spacing of Au Interplanar spacing of Al
crystallographic planes d hkl d hkl
{111} 0,235 50 0,233 80
{200} 0,203 90 0,202 40
{220} 0,144 20 0,143 10
{311} 0,123 00 0,122 10
{222} 0,117 74 0,116 90
{400} 0,101 96 0,101 24
{331} 0,093 58 0,092 89
{420} 0,091 20 0,090 55
{422} 0,083 25 0,082 66
{333}/{511} 0,078 00 —
NOTE 1   Lattice parameter for Au [face-centred cubic (FCC) structure, S.G: Fm3m(225)]: a = 0,407 8 nm.
See Reference [14].
NOTE 2   Lattice parameter for Al [FCC structure, S.G: Fm3m(225)]: a = 0,404 9 nm. See Reference [14].

18  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


Annex B
(informative)

Spot diffraction patterns of single crystals for BCC, FCC and HCP
structure[7]

B.1 Symbols and definitions

B.1.1 Zone axis, [uvw]
In a spot diffraction pattern, the symbol [uvw] denotes index of the zone axis, which is the normal of
this diffraction pattern.

B.1.2 Regulation for the reciprocal vectors

In this document, the symbols R1 and R2 of the R vectors in a spot diffraction pattern are specified as
follows:
R1 is the shortest vector in the diffraction pattern;
R2 is the next shortest vector, which is not along a common line with R1 and is positioned
anticlockwise around the centre spot relative to R1 . The relation between the vectors is as follows:
R3 = R2 − R1 and R3 ≥ R2 ≥ R1 .

B.2 Spot diffraction patterns for body-centred cubic (BCC) crystal,

(u2+v2+w2 ≤ 22)
Spot diffraction patterns from a single crystal with BCC structure are given in Figures B.1 to B.15.

R2/R1=1,0
R3/R1=1,414
[ uvw ] = [ 001]

Figure B.1

© ISO 2018 – All rights reserved  19

ISO 25498:2018(E)


R2/R1=1,414
R3/R1=1,732
[ uvw ] = [ 011]

Figure B.2

R2/R1=R3/R1=1,225
[ uvw ] = [ 012]

Figure B.3

20  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,581
R3/R1=1,871
[ uvw ] = [ 013]

Figure B.4

R2/R1=2,121
R3/R1=2,121
[ uvw ] = [ 014 ]

Figure B.5

R2/R1=1,871
R3/R1=1,871
[ uvw ] = [ 023]

Figure B.6

© ISO 2018 – All rights reserved  21

ISO 25498:2018(E)


R2/R1=1,0
R3/R1=1,0

[ uvw ] = [ 111 ]

Figure B.7

R2/R1=2,450
R3/R1=2,646

[ uvw ] = [ 112]

Figure B.8

22  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,732
R3/R1=1,732

[ uvw ] = [ 113]

Figure B.9

R2/R1=4,243
R3/R1=4,359

[ uvw ] = [ 114 ]

Figure B.10

© ISO 2018 – All rights reserved  23

ISO 25498:2018(E)


R2/R1=3,0
R3/R1=3,162

[ uvw ] = [ 122]

Figure B.11

R2/R1=1,291
R3/R1=1,826

[ uvw ] = [ 123]

Figure B.12

24  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=2,236
R3/R1=2,236

[ uvw ] = [ 133]

Figure B.13

R2/R1=4,123
R3/R1=4,243

[ uvw ] = [ 223]

Figure B.14

© ISO 2018 – All rights reserved  25

ISO 25498:2018(E)


R2/R1=4,690
R3/R1=4,796

[ uvw ] = [ 233]

Figure B.15

B.3 Spot diffraction patterns for face-centred cubic (FCC) structure

(u2+v2+w2 ≤ 22)
Spot diffraction patterns from a single crystal with FCC structure are given in Figures B.16 to B.30.

R2/R1=1,00
R3/R1=1,414
[ uvw ] = [ 001]

Figure B.16

26  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,000
R3/R1=1,155
[ uvw ] = [ 011]

Figure B.17

R2/R1=2,236
R3/R1=2,450
[ uvw ] = [ 012]

Figure B.18

© ISO 2018 – All rights reserved  27

ISO 25498:2018(E)


R2/R1=1,658
R3/R1=1,658
[ uvw ] = [ 013]

Figure B.19

R2/R1=4,123
R3/R1=4,243
[ uvw ] = [ 014 ]

Figure B.20

28  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=3,242
R3/R1=3,606
[ uvw ] = [ 023]

Figure B.21

R2/R1=1,00
R3/R1=1,00
[ uvw ] = [111 ]

Figure B.22

© ISO 2018 – All rights reserved  29

ISO 25498:2018(E)


R2/R1=1,633
R3/R1=1,915

[ uvw ] = [ 112]

Figure B.23

R2/R1=1,732
R3/R1=1,732

[ uvw ] = [ 113]

Figure B.24

30  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,173
R3/R1=1,173

[ uvw ] = [ 114 ]

Figure B.25

R2/R1=1,581
R3/R1=1,581

[ uvw ] = [ 122]

Figure B.26

R2/R1=2,517
R3/R1=2,828

[ uvw ] = [ 123]

Figure B.27

© ISO 2018 – All rights reserved  31

ISO 25498:2018(E)


R2/R1=2,236
R3/R1=2,236

[ uvw ] = [ 133]

Figure B.28

R2/R1=2,121
R3/R1=2,121

[ uvw ] = [ 223]

Figure B.29

32  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,173
R3/R1=1,541

[ uvw ] = [ 233]

Figure B.30

B.4 Spot diffraction patterns for hexagonal close-packed (HCP) structure for
c / a ≅� 1,633
Spot diffraction patterns from single crystal with HCP structure (for c / a = 8 / 3 ≅ 1 , 633 ) are given in
Figures B.31 to B.40. Miller-Bravais index is used for indexing the diffraction patterns of HCP crystals.
NOTE The symbol, ×, denotes the forbidden diffracted spots, which can occur due to the secondary
diffraction.

R2/R1=1,000
R3/R1=1,000
[UVTW ] = [ 0001]

Figure B.31

© ISO 2018 – All rights reserved  33

ISO 25498:2018(E)


R2/R1=1,633
R3/R1=1,915

[UVTW ] = [ 0110]

Figure B.32

R2/R1=1,000
R3/R1=1,288

[UVTW ] = [ 0111]

Figure B.33

34  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,530
R3/R1=1,828

[UVTW ] = [ 0112]

Figure B.34

R2/R1=1,880
R3/R1=1,880
[UVTW ] = [1211 ]

Figure B.35

© ISO 2018 – All rights reserved  35

ISO 25498:2018(E)


R2/R1=1,132
R3/R1=1,132

[UVTW ] = [1213 ]

Figure B.36

R2/R1=1,812
R3/R1=2,069

[UVTW ] = [ 1216 ]

Figure B.37

36  © ISO 2018 – All rights reserved

 ISO 25498:2018(E)


R2/R1=1,887
R3/R1=2,134

[UVTW ] = [ 2110 ]

Figure B.38

R2/R1=1,458
R3/R1=1,458

[UVTW ] = [ 2423]

Figure B.39

R2/R1=1,288
R3/R1=1,660

[UVTW ] = [5143]

Figure B.40

© ISO 2018 – All rights reserved  37

ISO 25498:2018(E)


Bibliography

[1] ISO 15932:2013, Microbeam analysis — Analytical electron microscopy — Vocabulary

[2] ASTM E 3-11, Standard practice for preparation of metallographic specimens
[3] Liu D.L.,Features of the ISO-25498: Method of Selected Area Electron Diffraction Analysis in
Transmission Electron Microscopy,Microsc. Microanal. 19, S5, 207–209, 2013
[4] Williams, D.B. and Carter, C.B. Transmission Electron Microscopy: A Textbook for Materials
Science, Plenum Press, New York 2009
[5] Edington, J.W. Practical Electron Microscopy in Materials Science, Vol. II, Electron Diffraction in
The Electron Microscope, Macmillan & Co Ltd, London, 1975
[6] Guo, K.X., Ye, H.Q., Wu, Y.K., Application of electron diffraction patterns in crystallography,
Science Press, China, 1983
[7] Andrews, K.W., Dyson, D.J., Keown, S.R. Interpretation of electron diffraction patterns, Second
Edition, 1971. (Publisher Hilger, London, ISBN-0-85274-170-7)
[8] Reimer, L., Transmission Electron Microscopy, 4th Edition, Springer, 2004
[9] Fultz, B, Howe, J., Transmission Electron Microscopy and Diffractometry of Materials, Springer-
Verlag, Berlin Heidelberg 2001
[10] Goodhew, P.J. Specimen preparation for transmission electron microscopy of materials, Oxford
University Press, Royal Microscopical Society, 1984
[11] The Powder Diffraction File 1997–2007, JCPDS, International Centre for Diffraction Data (ICDD)
[12] Jiang, L, Georgieva, D., Zandbergen, H.W. and Abrahams, J.P. (2009) Unit-cell determination from
randomly oriented electron-diffraction patterns. Acta Cryst. D, 625-632
[13] https:/​/​w ww​​.iucr​​.org/​resources/​other​​-directories/​software/​ediff
[14] Swanson, Tatge, Natl. Bur. Stand. (US), Circ. 539,1,11 (1953)

38  © ISO 2018 – All rights reserved

ISO 25498:2018(E)


ICS 71.040.50
Price based on 38 pages

© ISO 2018 – All rights reserved