ISO4967-non-metallic Inclusion
ISO4967-non-metallic Inclusion
STANDARD 4967
Second edition
1998-10-01
A Reference number
ISO 4967:1998(E)
ISO 4967:1998(E)
Contents Page
1 Scope ........................................................................................ 1
2 Principle .................................................................................... 1
3 Sampling ................................................................................... 3
4 Preparation of specimens ......................................................... 5
5 Determination of the content of inclusions ................................ 6
6 Expression of results ................................................................ 8
7 Test report ................................................................................ 9
© ISO 1998
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [email protected]
Printed in Switzerland
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© ISO ISO 4967:1998(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.
This second edition cancels and replaces the first edition (ISO 4967:1979),
which has been technically revised.
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1 Scope
This International Standard specifies a micrographic method of determining the nonmetallic inclusions in rolled or
forged steel products having a reduction ratio of at least 3 using standard diagrams. This method is widely used to
assess the suitability of a steel for a given use. However, since it is difficult to achieve reproducible results owing to
the influence of the test operator, even with a large number of specimens, precautions should be taken when using
the method.
NOTE For certain types of steel (e.g., free cutting steels), the standardized diagrams described in this International Standard
may not be applicable.
This International Standard also provides for the determination of nonmetallic inclusions by image analysis
technologies (see annex D).
2 Principle
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The method consists of comparing the observed field to the chart diagrams defined in this International Standard
and taking in consideration separately each type of inclusion. In the case of image analysis, fields will be rated
according to the relationships given in annex D.
The chart pictures correspond to square fields of view, each with an area of 0,50 mm2, as obtained with a
longitudinal plane-of-polish and as observed at 100 ¥.
According to the shape and distribution of the inclusions, the standard diagrams are divided into five main groups,
bearing the reference A, B, C, D and DS.
These five groups represent the most commonly observed inclusion types and morphologies:
— Group A (sulfide type): highly malleable, individual grey particles with a wide range of aspect ratios
(length/width) and generally rounded ends;
— Group B (aluminate type): numerous non deformable, angular, low aspect ratio (generally < 3), black or bluish
particles (at least three) aligned in the deformation direction;
— Group C (silicate type): highly malleable, individual black or dark grey particles with a wide range of aspect
ratios (generally > 3) and generally sharp ends;
— Group D (globular oxide type): non deformable, angular or circular, low aspect ratio (generally < 3), black or
bluish, randomly distributed particles;
— Group DS (single globular type): circular, or nearly circular, single particle with a diameter > 13 µm.
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ISO 4967:1998(E) © ISO
Non-traditional inclusion types may also be rated based on their morphology compared to the above five types and
a statement about their chemical nature. As an example, globular sulfides would be rated as a D type and a
descriptive subscript (e.g., Dsulf ) defined in the test report. Dcas would indicate globular calcium sulfides; DRES would
indicate globular rare earth sulfides; DDup would indicate globular duplex inclusions, such as calcium sulfide
surrounding an aluminate.
Types of precipitate such as borides, carbides, carbonitrides or nitrides may also be rated based on their
morphology compared to the above five types and a statement about their chemical nature as described in the
previous subclause.
NOTE Examination at a magnification greater than 100 ¥ may be used to identify the nature of the non-traditional inclusions
before performing the test.
Each main group on the chart consists of two subgroups, each made up of six diagrams representing increasing
inclusion content. This division into subgroups is merely intended to give examples of different thicknesses of
nonmetallic particles.
These chart diagrams carry an index number, i, from 0,5 to 3, the numbers increasing with the inclusion or stringer
lengths (Groups A, B, C) or by the number (Group D) or by the diameter (Group DS), as defined in table 1, and by
thickness, as defined in table 2. For example, the diagram A 2 indicates that the shape of the inclusions observed
under the microscope is in accordance with group A and that their distribution and quantity are in accordance with
number 2.
Inclusion group
Chart diagram A B C D DS
index total length total length total length count diameter
i µm µm µm number µm
0,5 37 17 18 1 13
1 127 77 76 4 19
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Fine Thick
Group type Minimum width Maximum width Minimum width Maximum width
µm µm µm µm
A 2 4 4 12
B 2 9 9 15
C 2 5 5 12
D 3 8 8 13
NOTE For type D the maximum dimension is defined as the diameter.
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© ISO ISO 4967:1998(E)
3 Sampling
The shape of the inclusion depends to a large extent on the degree of reduction of the steel; therefore, comparative
measurements may only be carried out on prepared sections taken from samples with a similar amount of
deformation.
The polished surface of the specimen used to determine the content of inclusions shall be approximately 200 mm2
(20 mm ¥ 10 mm). It shall be parallel to the longitudinal axis of the product and shall be located halfway between the
outer surface and the centre.
The method of sampling shall be defined in the product standard or subject to agreement between the parties. The
test surface, in the case of plates, shall be approximately at a quarter of the width.
— bar or billet with diameters greater than 40 mm: the surface to be examined consists of a part of diametral
section located halfway between the outer surface and the centre (see figure 1);
— bar with a diameter greater than 25 mm and less than or equal to 40 mm: the surface to be examined consists
of half the diametral section (from the centre to the edge of the sample) (see figure 2);
— bar with a diameter less than or equal to 25 mm: the surface to be examined consists of the full diametral
section of length sufficient to obtain a surface of about 200 mm2 (see figure 3);
— plates with a thickness less than or equal to 25 mm: the surface to be examined consists of the whole
thickness, and located at the quarter of the width (see figure 4),
— plates with a thickness greater than 25 mm and less than or equal to 50 mm: the surface to be examined
consists of half the thickness from the surface to the centre and is located at the quarter of the width
(see figure 5);
— plates with a thickness greater than 50 mm: the surface to be examined consists of quarter the thickness and is
located halfway between the outer surface and the middle of the thickness and at the quarter of the width
(see figure 6).
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The number of samples to be taken is defined in the product standard or by special agreement.
For any other product, the sampling procedures shall be subject to agreement between the parties.
Dimensions in millimetres
Figure 1 — Sample from bar or billet with a diameter or length of side > 40 mm
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ISO 4967:1998(E) © ISO
Figure 2 — Sample from bar or billet with a diameter or length of side > 25 mm and < 40 mm
r = width
Figure 4 — Sample from plate with thickness < 25 mm
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© ISO ISO 4967:1998(E)
r = width
Figure 5 — Sample from plate with thickness > 25 mm and < 50 mm
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r = width
Figure 6 — Sample from plate with thickness > 50 mm
4 Preparation of specimens
The specimen shall be cut so as to obtain a surface for examination. In order to achieve a flat surface and to avoid
rounding the edges of the specimen when polishing, the specimen may be held mechanically or may be mounted.
When polishing specimens, it is important to avoid any tearing out or deformation of the inclusions, or contamination
of the polished surface, so that the surface is as clean as possible and the shape of the inclusions is not affected.
These precautions are of particular importance when the inclusions are small. It is advisable to use diamond paste
for polishing. In certain cases it may be necessary for the specimen to be heat treated before polishing in order to
give it the maximum possible hardness.
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ISO 4967:1998(E) © ISO
If the image is projected onto a ground glass or similar device, the magnification must be 100 ¥ ± 2 ¥ on the ground
glass. Place a clear plastic overlay (figure 7) of a 71 mm square (0,50 mm2 true area) over or behind the ground
glass projection screen. The image within the test square is compared to the standard pictures on the chart
(annex A).
If the inclusions are examined through the microscope eyepieces, insert a reticle with the test pattern shown in
figure 7 in the microscope at the appropriate location so that the test grid area is 0,50 mm2 at the image plane.
NOTE In special cases, a magnification greater than 100 may be used, provided that the same magnification is applied for
the standard diagrams, and shall be recorded in the test report.
Dimensions in millimetres
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© ISO ISO 4967:1998(E)
5.2.1 Method A
The entire polished surface is examined and, for each type of inclusion, a note is made of the reference number
which lies to the side of the standard diagram which corresponds to the worst field examined, in the fine and thick
series.
5.2.2 Method B
The entire polished surface is examined and each field of the specimen is compared with the standard diagrams.
The reference number of the field (indicated to the side of the standard diagrams) which best corresponds to the
field examined for each type of inclusion is noted, in the fine and thick series.
In order to minimize the cost of examination, it may be agreed upon to make a partial examination of the specimen
by studying a reduced number of fields, distributed in accordance with a fixed scheme. Both the number of fields
examined and their distribution shall be arranged by prior agreement.
Each field observed is compared with the standard diagrams. If a field of inclusions falls between two standard
diagrams, it is rated following the lower diagram.
Individual inclusions or stringers that have a length greater than the field width (0,710 mm) or a width or diameter
greater than the thick series maximum (see table 2) will be rated as oversized by length, width or diameter. The
oversized dimensions of the inclusion or stringer shall be noted separately. However, these inclusions shall still be
part of the overall rating of that field.
of DS type) and counts (D types) are made. Use a grid overlay or reticle, as shown in figure 7, the measurement
limits in tables 1 and 2, and the morphological descriptions in section 2, as illustrated in the chart.
Non-traditional inclusion types are rated according to the chart group (A, B, C, D, DS) that best corresponds to their
morphology. Compare the length, number, thickness or diameter of the inclusions to each group shown in annex A
or determine their total length, number, thickness or diameter, and use tables 1 and 2 to assign the appropriate
inclusion content number and thickness class (fine, thick or oversize). Then indicate the nature of the non-traditional
inclusion with a subscript to the group type. Define the subscript in the test report.
For type A, B and C inclusions, two individual inclusions or stringers of lengths l1 and l2 and which are, or are not, in
line are considered as one inclusion or stringer if the distance d is lower than or equal to 40 µm and if the distance s,
(the distance between centres of inclusions/stringers) is lower than or equal to 10 µm (see figures 8 and 9).
In the case of a stringer with inclusions of different width, the width to be considered is the width of the biggest
inclusion.
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ISO 4967:1998(E) © ISO
6 Expression of results
6.1 General
Unless otherwise stated in the product standard, the results may be expressed in the following ways.
The results are expressed with the index numbers relating to each specimen and on their basis the arithmetic mean
is assessed per cast for each type of inclusion and for each thickness series. This method is used in combination
with the method described in 5.2.1.
6.2 Method A
Indication of the reference number corresponding to the worst field for each type of inclusion and for each thickness
series (see annex B).
The reference symbol for the group of inclusions is followed by the reference number of the worst field, the
presence of thick inclusions being indicated by the letter e, the presence of inclusion oversized (see 5.2.3) being
indicated by the letter s.
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© ISO ISO 4967:1998(E)
6.3 Method B
Indication of the total number of fields for a given index, per type of inclusion and per thickness series for a given
number of fields observed (N).
The full set of total numbers of fields for a given index relative to the various types of inclusions may be used in
special methods for expressing results, such as total index, itot, or mean index, imoy, subject to agreement between
the parties.
EXAMPLE :
then
itot = (n1 ¥ 0,5) + (n2 ¥ 1) + (n3 ¥ 1,5) + (n4 ¥ 2) + (n5 ¥ 2,5) + (n6 ¥ 3)
i
imoy = tot
N
7 Test report
The test report shall contain the following information:
e) the method selected (method of observation, method of examination, method of expressing results);
h) the results of the examination (including the number, size and type of oversize inclusions or stringers);
k) name of operator.
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ISO 4967:1998(E) © ISO
Annex A
(normative)
A
(Sulfide type)
Magnification = 100 ¥
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©
ISO
Magnification = 100 ¥
ISO 4967:1998(E)
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ISO 4967:1998(E)
Magnification = 100 ¥
©
ISO
© ISO ISO 4967:1998(E)
B
(Aluminate type)
Magnification = 100 ¥
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ISO 4967:1998(E)
Magnification = 100 ¥
©
ISO
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©
ISO
Magnification = 100 ¥
ISO 4967:1998(E)
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ISO 4967:1998(E) © ISO
C
(Silicate type)
Magnification = 100 ¥
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©
ISO
Magnification = 100 ¥
ISO 4967:1998(E)
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ISO 4967:1998(E)
Magnification = 100 ¥
©
ISO
© ISO ISO 4967:1998(E)
D
(Globular type oxides)
Magnification = 100 ¥
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ISO 4967:1998(E)
Magnification = 100 ¥
©
ISO
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ISO
Magnification = 100 ¥
ISO 4967:1998(E)
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ISO 4967:1998(E) © ISO
DS
(Globular type oxides)
Diameter > 13 mm to 76 mm
Minimum diameter
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Magnification = 100 ¥
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ISO
Magnification = 100 ¥
ISO 4967:1998(E)
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ISO 4967:1998(E)
Magnification = 100 ¥
©
ISO
© ISO ISO 4967:1998(E)
Annex B
(informative)
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ISO 4967:1998(E)
If the inclusion or stringer is oversized by width or diameter (type D inclusions), the inclusion should be part of the
thick series rating for that field (see Figure B.2 b).
For the type D inclusion, if the number of particles is greater than 49, the index can be calculated from the equation
given in annex D.
For a DS type inclusion with a diameter greater than 0,107 mm, the index can be calculated from the equation given
in annex D.
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The field rating is based of the total length L The field rating is based of the total length L
L = 0,71 + l1 + l2 + l3 L = l1 + l2 + l3 + l4
with separate indication of oversized length l4 with separate indication of oversized width (l4)
a) For inclusions or stringers oversized by length only b) For inclusions or stringers oversized by width or diameter
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ISO 4967:1998(E) © ISO
Annex C
(informative)
Typical example of results (the total number of fields showing the index, by
type of inclusion, for a given number of fields observed)
14 2 — — 1 — — — — —
15 — — — — 0,5 — — — —
16 0,5 — 1 — — 1 — — —
17 0,5 — 0,5 — — — — 0,5 1,5
18 — — — 1,5 1 — — — —
19 — 2 — 3 0,5 — 0,5 — —
20 — — 0,5 — — 0,5 — — —
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© ISO ISO 4967:1998(E)
NOTE Inclusions having a length greater than the dimension of the field, or a width or a diameter greater than indicated in
table 2 shall be rated using the standard diagrams and reported separately in the test report.
i 8,5
imoy = tot = = 0,425
N 20
b) Thick series
itot = (2 ¥ 0,5) + (1 ¥ 1) + (1 ¥ 2) = 4
4
imoy = = 0,20 with indication of 1 s
20
7
imoy = = 0,35
20
b) Thick series
9
imoy = = 0,45
20
6,5
imoy = = 0,325
20
b) Thick series
5,5
imoy = = 0,275
20
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ISO 4967:1998(E) © ISO
2
imoy = = 0,10
20
b) Thick series
itot = (2 ¥ 0,5) + (2 ¥ 1) = 3
3
imoy = = 0,15 with indication of 1 s
20
4
imoy = = 0,2
20
3,5 1000
Ci = ∑
i =0,5
f i × ni
S
where
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© ISO ISO 4967:1998(E)
Annex D
(informative)
Except for type DS, the anti-log must be taken to obtain the i.
D.2 Calculation of the inclusion measurement from the chart picture number
For group A sulfides, length in µm (L):
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ISO 4967:1998(E) © ISO
For the above linear regression equations, the R² values are all above 0,999 9.
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ISO
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ISO
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ICS 77.040.99
Descriptors: steels, iron and steel products, tests, determination of content, inclusions, non-metallic inclusions, microscopic analysis.