E04 2012

A General Introduction
to EN 10247
Dipl.-Ing. Damian Moll, AG der Dillinger Httenwerke
Nov 14 2012
NMI Workshop, ATLANTA
Product Segments
Earth moving equipment
Engineering
Offshore
Shipbuilding
Steel construction
Pressure vessel and boiler construction
Linepipe
Structural tubulars
Mould and die steels
Safety engineering
Specialist stockists
Dipl.-Ing. Damian Moll
Steel service centres

Job rolling
Semi products
All steels correspond to national and
international standards
Nov 14 2012
New York Times Building, USA
Nov 14 2012
Height:
Storeys:
Plate thickness:
DH-delivery:
Steel grades:
319 m
52
up to 203 mm
about 3,900 t
ASTM A572-42
ASTM A572-50
ASTM A572-K
Shanghai World Financial Center, China

Total area:
Height:
Storeys:
Plate thickness:
DH-delivery:
Steel grades:
24,000 m
492 m
101
up to 100 mm
about 23,000 t
ASTM A572-50, DI-MC 460
Nov 14 2012
Nov 14 2012
Total length:
Height:
DH-delivery:
Steel grades:
Viaduc de Millau, France
2,460 m
343 m
43,000 t
S355K2G3; S355N/NL; S460 QL1;
DI-MC 460
5
Queen Mary 2
Length:
Width:
Height:
Top speed:
Passengers:
Crew members:
345 m
41 m
72 m
30 knots
2,800
1,300
DH-delivery: 21,261 t
Steel grades:
LR-A up to E
LR-AH36 up to LR-DH36
DIMARINE 36
Nov 14 2012
Transcaucasian pipeline
Pathway:
from Baku (Azerbaijan) via Tbilisi

(Georgia) to Ceyhan (Turkey)
Length:
1,768 km
Diameter:
34 and 42
Plate thickness: 16.2 to 25.8 mm
DH-delivery: 63,000 t
Steel grade: 5L-X65 sour pH3&4
Nov 14 2012
Survey
Intro
Steel cleanliness
Scope of the new standard
Basic regulations, definitions and terms
Test method
Evaluation methods
Comparison to existing standards
Brief look at the future development
1.
2.
3.
4.
5.
6.
7.
8.
Nov 14 2012
Intro
metallographic specimen
microscope
chart
The same test method and similar evaluation methods as other standards
Standard for manual or automatic assessment
Developed for manual assessment but automatic assessment is possible

Conversion
Converting the results of other standards into EN 10247 is not possible

First standard with single inclusion oriented assessment
In other standards field oriented assessment

Nov 14 2012
What is good cleanliness?
Parameters of steel production processes
Inclusion parameters
melting
shape
casting
size
forming
number of inclusions
de-oxidization
distribution
steel composition
composition
Inclusions have mostly a negative influence on material properties and are

undesirable in steel
Nov 14 2012
10
Statement of the content of nonmetallic inclusions which occur as sulfides

and oxides in steel
What is optimal cleanliness?

Optimal cleanliness
Application
Inclusion parameters
Component parameters
Shape
Type of component
Size
Dimensions
Number of inclusions
Distribution
Composition
Nov 14 2012
Stress situation
11
What is optimal cleanliness?
Zugspannung
tensile stress
neutral fiber
Druckspannung
compression stress
Nov 14 2012
12
Scope of the standard
Size of particles:
3 m < length < 1410 m
2 m < width
3 m < diameter
elongated
inclusions lie parallel to each other and to the main direction

of deformation
The standard does not apply to free cutting steels

Minimum of 5-fold deformation degree of the specimens is
recommended
Nov 14 2012
13
Basic determinations and definitions
Inclusion
L, d > 3 m
w > 2 m
L, d
1.00 < L/w <1.30
Elongated
1 inclusion
Round
1 inclusion
Single particles
Nov 14 2012
14
Basic determinations and definitions

Inclusion
e < 40 m und t < 10 m
L, d > 3 m
For all particles: e < 40 m and t < 10 m
w1
w > 2 m
t
L
L1
e
L, d
L2
w2
w
w1>w2
w
round
1 inclusion
elongated
1 inclusion
single particles
2 elongated particles
1 inclusion L x w1
2 round particles
2 inclusions L1 and L2
4 elongated particles
1 striger
3 round particles
1 stringer
1 inclusion L x w
1 inclusion L x w
three or more particles
two particles
w5 = w2 + t2 + w3
w5 > w4> w1> w2> w3
w1
e < 40 m
t < 10 m
e < 0 m
t < 10 m
w1 w2
t
w2
w1 > w2
e L
w = w1 + t + w2
t
15 round perticles
2 stringers
1 inclusion L x w1
two stringers
Nov 14 2012
e2 < 0 m
0 < e1, e3, < 40 m
e1
w1
e2
t1,t2,t3, < 10 m
w2
t1
e3
w3
t2
15 round particles
2 stringers
1 inclusion L x w
two stringers overlaped
w1 > w2
e
w5
w4
28 round particles
4 stringers
1 inclusion L x w5
t3
agglomeration of stringers
15
Test method
Investigation of the metallographic specimens under the light microscope
(at least 6 specimens)
measurement area covers at least 200 mm
classification of the observed inclusions in the microscope through
a comparison with the chart. As a rule magnification 100 : 1
DIN 50602
NF A 04-106
SS 11 11 16
Nov 14 2012
ASTM E45
ISO 4967
16
Test method
inclusions will be evaluated according to their shape (morphology):

, , ,
Additionally, lengths and widths will be considered
assessment with the determination of size or of size and distribution
elongated, scattered
single inclusion
elongated, aligned
inclusion
globular, aligned
inclusion
globular, scattered
single inclusion
Nov 14 2012
17
Type of inclusion
observed inclusion
Test method
classification of inclusion: 7.3
Nov 14 2012
18
Test method
width
length
Nov 14 2012
19
Test method
width
Table 2
Nov 14 2012
length
20
Assessment methods
Worst-inclusion method Method P

length/diameter, area
Worst-field method Method M

number, length/diameter, area
Average-field method Method K
Nov 14 2012
number and length/diameter per mm2, number and area per mm2
21
Assessment methods
Method P, Worst-inclusion method
Start point
Nov 14 2012
22
Assessment methods
Method M, Worst-field method
Start point
Nov 14 2012
23
Assessment methods
Method K, Average-field method
Start point
19 x
Nov 14 2012
24
Assessment methods
Standard methods:
Worst-inclusion method
with parameter length method PL and diameter method Pd
Average-field method
with parameters number and length per mm2 method Kn, KL

and number and diameter per mm2 method Kn, Kd
Nov 14 2012
25
Assessment methods
EN 10247 Standard methods:
Worst-inclusion method
Nominal values
< 88
< 176
< 176
< 88
Actual values
Average values PL, Pd [m]
59
110
154
44
PL, Pd [m]
Nominal values
Actual values
Average values
Nov 14 2012
Kn
KL,Kd
[n/mm]
[m/mm]
<2
< 20
Kn
KL,Kd
[n/mm]
[m/mm]
1.4
12
Average-field method
26
Comparability with the former standards
Direct conversion of the determined values impossible

Different image charts and criteria of assessment
Classification of individual inclusions in the new standard
Possibility of the comparison through reclassification of the raw data
Possibility of the inclusion description in relation to the old and the
existing standards
Nov 14 2012
27
Comparability with the former standards

Type of
inclusion
Color
Standard
EN 10247
ASTM E45
DIN 50602
Type of
inclusion
NF 04-106
SS 111116
Sulfide
grey
EA
SS
elongated
Oxide
black
EC
OS
elongated
Oxide
black
EB
OA
globular, aligned
Oxide
grey/black
EAD
Sulfide/Oxide
color
EF
e.g. Nitride
OG
ED
Nov 14 2012
globular, single
black
28
Summary
the same test method and similar assessment methods

easier and clearer classification of inclusions
better method of comparison of the results (physical dimensions)
reduction of the number of applied standards in practice
upgrading of the microscopes necessary (eyepiece graticule or image
analysis)
greater need of communication between customer and supplier
Nov 14 2012
29
Important changes planned
changing the ratio L/w from 1.3 to 3
name of inclusions
new assessment rules for mixed inclusions
changes to Table 2
changes in the forms

Nov 14 2012
30
Thank you
for you
attention
Nov 14 2012
31
Automated Image Segmentation in the

Metallographic Area with Focus on Nonmetallic
Inclusions
Jrgen Phringer1, Dr. Jati Kastanja2
1 voestalpine Stahl GmbH, Linz
2 Carl Zeiss Microscopy GmbH
Stahl GmbH
www.voestalpine.com
A fully equipped Image Analysis Laboratory
Schusterkugel historic
magnifying device
folding rule - for distance
measuring
mesh determine particle size
Clipper and a scale to cut out
structures and phase fractions
And Most Important:
Stahl GmbH
|
door plate (quantitative microscopy)
Introduction
Accurate thresholding is essential for any

subsequent step in automated image
analysis
Due to this fact a high potential risk of

erroneous use and unknown measurement
bias.
Problem solved with automatic grey level

segmentation
Stahl GmbH
3
16.11.2012
So simple?
There are many methods a little lesser than sand on the beach
Otsu procedure
IsoData
Mean value
Two peaks
Image segmentation, partioning the image into
Edge pixels
Iterative
selection
homogeneous
regions, is a challenging task
Min. Error*Robust Analysis of Feature Spaces: Color Image Segmentation Dorin Comaniciu MIT
Fuzz (entropy)
Fuzz (Yager)
Triangulation procedure
..
Unfortunately, no universal method
Stahl GmbH
4
16.11.2012
Small trip through metallographic tasks
SiAl alloy
Cu alloy
grey cast iron
Stainless
Steel alloysteel
Stahl GmbH
5
16.11.2012
To do list
How to detect inclusions?
Separation of particles and background (matrix)
How ?
Fix this and many tasks (phase fraction,) are solved!
particles consist of grey (sulfide) and dark (oxide) fractions - separation
How ?
Automated inclusion detection ready to measure!
Stahl GmbH
6
16.11.2012
matrix
fiction perfect world - reality
The perfect background
uniform
single grey value
no digital noise
situation: easy
solution : non
SiFi - not in this universe!
Stahl GmbH
7
16.11.2012
matrix
background
slight inhomogeneity
slight noise
Grey values are

normally distributed
situation : medium
solution : Gaussian fit
Only in a perfect world!
Stahl GmbH
8
16.11.2012
matrix
Grey values are nearly
normal distributed
and there is more!
situation : difficult
solution : several possible
algorithms
Welcome in our world!
Stahl GmbH
9
16.11.2012
Step 1 separation of particles and

background
polished metallic samples

matrix appears approximately
normal distributed
everything outside of the normal
distribution is object
two methods
Triangulation (weak peek)

IsoData
object
background
b0
Stahl GmbH
10
16.11.2012
Background separation - example

Phasefraction:
method Median
15,02 %
method Triangulation
19,87 %
Stahl GmbH
|
NMI assignment
* Free cutting steel usually no topic on NMI rating according to ASTM E45, EN10247,
Stahl GmbH
12
16.11.2012
step 1: background separation
Stahl GmbH
13
16.11.2012
step 2: separation oxide / sulfide

algorithm Otsu or IsoData
Otsu
IsoData
255
t
i * P0 (i ) i * P0 (i)
1
t
t * i 0t
i 255
2
P0 (i)
P0 (i )
i t
i 0
Otsu's threshold clustering algorithm searches for the

threshold that minimizes the intra-class variance, defined
as a weighted sum of variances of the two classes.
N. Otsu, "A threshold selection method from grey level histograms", IEEE Trans.
System Man and Cybernetics, Vol. 9,1979
Stahl GmbH
|
The procedure divides the image into object and

background by taking an initial threshold, then the
averages of the pixels at or below the threshold and pixels
above are computed. The averages of those two values
are computed, the threshold is incremented and the
process is repeated until the threshold is larger than the
composite average.
Ridler, TW & Calvard, S (1978), "Picture thresholding using an iterative selection method",
IEEE Transactions on Systems, Man and Cybernetics 8: 630-632
step 2: separation oxide / sulfide
Stahl GmbH
15
16.11.2012
Proof
Stahl GmbH
16
16.11.2012
microscopic image
grey Mn-sulfide
black (tip) Pb-oxide
Proof
Stahl GmbH
17
16.11.2012
segmented image
Step 1 matrix elimination
No steel matrix is present in
image
Step 2 oxide / sulfide identification
blue representing Sulfides
red representing Oxides
Use for complex inclusions
Stahl GmbH
18
16.11.2012
segmented image
Step 1 matrix elimination
No steel matrix is present in
image
Step 2 oxide / sulfide identification
Complex inclusions
Magenta dominant sulfide
Cyan dominant oxide
Summary
No trival task
Several segmentation algorithm possible
Presented algorithm (ISO-Data, Otso and Triangulation)
Solve standard applications like Phase fraction,

Solve identification of NMI particles
User bias eliminated with automated segmentation!
Stahl GmbH
19
16.11.2012
Thank you
Stahl GmbH
20
16.11.2012
Das Forum fr
Metallurgie und Werkstofftechnik
The Austrian Society

for Metallurgy and Materials
Automated SEM/ EDX Partikelanalyses to Determinate NonMetallic Inclusions in Steel Samples Round Robin Tests Aiming
at Studying the Comparability of Results From Different
Measurement Systems
Goals:
Phase 1
Finding measuring differences in the data of the four measurement
systems
Presentation and explanation of differences in results
Phase 2 => Decision to phase 1

Performing a further measuring run with adjusted gray scale settings
ASMET The Austrian Society for Metallurgy and Materials
Inclusions in Steel Samples Round Robin Test

Participants and combination of devices:
Participants of the round

robin test
Type of REM
Type of EDXSoftware
voestalpine
Stahl Donawitz
FEI XL40
EDAX
voestalpine
Stahl Linz
ASPEX Instruments
Gresham Scientific
Bhler Edelstahl
JEOL 6490 HV
INCA
MUL
Chair for Metallurgy
FEI Quanta 200 MK2
INCA
Inclusions in Steel Samples Round Robin Test Phase 1

Sample Choice and Sample Preparation Phase 1:
Sample A
Sample B
Sample C
The samples have then been
conductively mounted, ground
and polished to 1m. After
that, the measuring positions
have been defined by means
of hardness indentations

Choice of Parameters for Phase 1:
The choice of the following parameters has been made based on criteria resembling real
day to day working conditions of the participants.
Accelerating voltage:
Measurement time per inclusion:
Partikel scan:
Measurement surface marked area:
Partikel detection:
Pixel size:
15kV
3s
core 100%
~80mm
1m
~ 0,45m
Identification of inclusion starting from a minimum of 4 pixels

Element ID
No data exclusion
In case of problems affecting the comparability of the measurement the cycle is to be
started anew.

Evaluation Phase 1:
Sum of all inclusions of different samples normalized to 25 mm
The substantially lower quantity of detected particles with round robin test participant
T2 can be attributed to a deviation of the measurement parameter of the pixel size (~
1m).

Evaluation Phase 1:
Number of inclusions over circle equivalent diameter (CED) normalized to 25mm

Evaluation Phase 1:
Inclusion area over inclusion type (roughly classified) for the sum of detected particles

Evaluation Phase 1:
Example of a ternary system Al-Ca-S of sample B for the sum of detected inclusions

Evaluation Phase 1:
Conclusion Phase 1
Uniform choice of measurement parameters (see pixel size T2) is crucial
Good agreement of the inclusion area of the oxide particles
EDX-measured values are similar for all participants (ternary system)
Differences in the number of particels and of the inclusion area of the sulfides class
Particle detection represents the biggest problem and is the

main cause for the differences Phase 2

Sample Choice and Sample Preparation Phase 2:
Probe A
Probe B
Probe D
The samples have then been
conductively mounted, ground
and polished to 1m. After that,
the measuring positions have
been defined by means of
hardness indentations

Choice of Parameters for Phase 2:
Here, the parameters have been taken over from phase 1 ( the surface area has been
reduced to about 25mm) and a gray value definition has been added.
EDAX
INCA
220
190
190
40
220
0 bis 255
40
0 bis 255

Evaluation Phase 2:
Sum of all inclusions of different samples normalized to 25 mm
During the analysis of sample D of participant T2, construction works have been
carried out on the premises. At times, these caused significant ground motions. That
is why clear deviations of these results can be attributed to an environmental impact.

Evaluation Phase 2:
Number of inclusions over circle equivalent diameter (CED) normalized to 25mm

Auswertung Phase 2:
Influence of matrix units of sample D

Evaluation Phase 2:
Conclusion Phase 2
Attention to environmental influences
The gray value calibration leads to a clearly improved agreement of the results
of the particle detection
To minimize the deviations with particles <2m the parameter of the pixle size
of ~0,45m has to be considerably reduced
In order to allow for a classification, the influence of the matrix concentration is

to be considered when evaluating the chemical composition
Ringversuch REM/EDX-Partikelanalyse
Thank you
The Measurement of Inclusions and

Stringers in Hot Worked and Cold Worked
Nitinol Products
Frank Sczerzenie and Clarence Belden
SAES Smart Materials, New Hartford, New York, USA
frank_sczerzenie@saes-group.com, 315-266-2026 extension 202
clarence_belden@saes-group.com 315-266-2026
making innovation happen, together
Outline
Materials
Procedure
Maximum inclusion definition
Stringer definition
Metallographic difficulties for E1245
Results for coil and wire
Observations coil and wire
Results for bar
Observations for bar
Conclusions and future work
Production Materials
1. Hot rolled 6.3 mm diameter x coil:
Standard VIM VAR, 355 mm x 1700 Kg ingot.

Process Improvement VIM VAR, 406 mm x 1450 Kg ingot.
2. Cold drawn 2.16 mm diameter wire:

Process Improvement VIM VAR, 406 mm x 1450 Kg ingot.
3. Hot rolled 50.8 mm round cornered square (RCS) pre-rolled bar
4. Hot rolled 32 mm round bar
Procedures
Inclusion Evaluation:
Reference: Sczerzenie et al. The Measurement of Total Inclusion
Content in Nickel-Titanium Alloys, Journal of Materials
Engineering and Performance: Volume 21, Issue 12 (2012), Page
2578-2586.
Beyond ASTM F2063-05 requirements.
Counted carbides and oxides separately.
Histograms for all inclusions at 0.1 m and larger.
Percentile versus area fraction for all fields of view.
Counted void as part of adjacent carbide or oxide.
12 or more samples for each material.
REDOX - Material:
Proprietary changes in melting and hot working aimed at reducing
the formation of intermetallic oxides Ti4Ni2O(N,C)x.
Schematic of Coil Sample and Metallographic

Scanning Technique
Inclusion count catalogued with respect to

center, mid-radius and edge locations in hot
worked product.
A Stringer in Cold Drawn 2.2 mm Diameter

Wire
Carbide
Oxide
Void
Need a quantitative
definition of a stringer
20 m
Definition of Maximum Inclusion Dimension
The maximum
inclusion dimension
shall be the
maximum length of
all contiguous
particles and voids
including particle
separated by voids.
Stringer Definition
ASTM E 45-05 Standard test Methods for Determining the Inclusion
Content of Steel:
An individual inclusion that is highly elongated in the deformation
direction or three or more Type B [alumina type] or C [silicate type]
inclusions aligned in a plane parallel to the hot working axis and offset
by no more than 15 m with a separation of less than 40 m between
any two nearest neighbor inclusions.
SAES for NiTi Alloy:
An individual inclusion that is highly elongated in the deformation
direction or two or more inclusions aligned in a plane parallel to the hot
working axis and offset by no more than 1 m, with separation of less
than 5 m (0.000195 in.) between any two nearest neighbor inclusions.
Metallographic Difficulties for Automated

Analysis
In the
optical
microscope
with white
light,
intermetallic
oxide are low
contrast to
the matrix.
Inclusions in Hot Rolled Coil
Maximum inclusion m
Average area fraction
Maximum area fraction
Standard SE
Coil
24.53
0.653%
1.23%
Process
Reduction by
Improvement Process
Coil
Improvement
19.23
21.6%
0.493%
24.5%
0.91%
26.0%
Carbides per field

Carbide maximum
Carbide maximum area fraction
102
18.15
1.06%
94
19.23
0.91%
7.8%
-6.0%
14.2%
Oxides per field

Oxide maximum
Oxide maximum area fraction
5
24.53
0.65%
1
11.95
0.19%
80.0%
51.3%
70.8%
Distribution of Inclusions in Standard Coil
Distribution of Inclusions in REDOX Coil
Area Fraction of Inclusions in Standard Coil
Area Fraction of Inclusions in REDOX Coil
Inclusions in Standard and REDOX 2.2 mm

Diameter Wire
Maximum inclusion m
Average area fraction
Maximum area fraction
Process
Reduction by
Standard
Improvement Process
SE Wire
Wire
Improvement
43.62
27.84
36.2%
0.68%
0.60%
11.8%
1.45%
1.07%
26.2%
Carbides per field

Carbide maximum m
Carbide maximum area fraction
144
19.94
0.81%
137
26.40
0.97%
4.9%
-32.4%
-19.8%
Oxides per field

Oxide maximum m
Oxide maximum area fraction
7.1
43.62
0.91%
2.3
27.84
0.31%
67.6%
36.2%
65.9%
Distribution of Inclusions in Standard Wire
Distribution of Inclusions in REDOX Wire
Area Fraction of Inclusions in Standard Wire
Area Fraction of Inclusions in REDOX Wire
Stringers in Standard Coil
Stringers in REDOX Coil
Stringer Length Distribution in

Standard and REDOX Coil, Normalized
Stringers in Standard and REDOX 2.2 mm

Diameter Wire
Standard SE
Wire
Stringers per field
18.7
Average stringer length m
7
99th percentile stringer length m
44
Maximum stringer length m
76.36
Process
Reduction by
Improvement Process
Wire
Improvement
17.8
4.8%
7
0.0%
36
18.2%
60.83
20.3%
Stringer Length Distribution in Standard Wire
Stringer Length Distribution in REDOX

Wire
Stringer Length Distributions in

Standard and REDOX Wires,
Normalized
Observations on Coil and Wire

REDOX reduced the maximum size (36%) and the
maximum area fraction (26%) of inclusions. This was
due to a reduction in number (80%) and size (71%) of
intermetallic oxides in hot rolled coil.
Stringer length distributions were very similar in
Standard Process and REDOX hot rolled coil. REDOX
gave a 12% reduction in the maximum stringer length.
Stringer length distributions were very similar in
Standard Process and REDOX cold drawn wire. REDOX
gave a 20% reduction in the maximum stringer length.
27
Observations on Coil and Wire
Cold drawing increases inclusion area fraction in

Standard Process wire (17.9%) and REDOX wire(17.6%)
compared to coil.
Cold drawing increases maximum stringer length in
standard process wire (111%) and REDOX wire (90%)
compared to coil.
Void formation may have a significant effect on these
statistics.
28
Standard 2 Inch RCS Carbide and Oxide Size

Distributions
29
Standard 1.27 Inch Diameter Bar Carbide

and Oxide Size Distributions
30
Standard 1.27 Inch Bar versus RCS, Carbide

Size Distribution, Normalized
31
Standard 1.27 Inch Bar versus RCS, Oxide Size

Distribution, Normalized
32
Standard 2 Inch RCS Bar Stringer Length

Distribution
33
Stringer Length Distribution in Standard 1.27

Inch Diameter Bar
34
Stringer Length Distribution in Standard RCS

and 1.27 Inch Bar, Normalized
35
Observations on Hot Rolled Bar

Carbide and intermetallic oxide size distributions were
not changed in hot rolling Standard material from 2 inch
RCS to 1.27 inch diameter bar.
Stringer length distributions and maximum stringer
length were not changed in hot rolling Standard material
from 2 inch RCS to 1.27 inch diameter bar.
Void formation is a less significant factor in inclusion
area and stringer formation in hot rolling.
36
Conclusions
1. This work demonstrated a method for the analysis of
the total inclusion content of VIM-VAR NiTi alloys.
2. Definitions for maximum inclusion dimension and for
stringers have been applied quantitatively to one
superelastic NiTi alloy.
3. Particle size distributions of both carbides and oxides
are not normal. These distributions are skewed toward
positive values with relatively few larger particles
approaching the maximum particle size.
4. The statistics of normal distributions and the calculation
of a six sigma 99.9999% confidence interval for
maximum inclusion size or area fraction do not apply to
inclusions in superelastic VIM-VAR NiTi alloys..
Conclusions, continued
5. Consider applying improved statistical tools such as
extreme value statistics to determine inclusion limits in
the ASTM Standards.
6. Both carbides and oxides form stringers.
7. There is no correlation of increased oxide formation to
the radial position of the sample in the ingot, or coil.
8. REDOX material resulted in a reduction of maximum
inclusion size and area fraction in hot rolled coil and
cold drawn wire. Maximum stringer length was slightly
reduced.
9. The reduction in maximum area and size of inclusions
in REDOX coil and wire was the result of reducing the
number, size and area fraction of intermetallic oxides.
Conclusions, continued
10. Hot rolling tends to stabilize the carbide and oxide size
distributions. More work is needed to determine the
effect of process parameters and product size.
11. Hot rolling tends to stabilize the stringer size
distribution.
12. Inclusion area fraction is below 1.5% in all As = -15oC
alloy products .
13. Inclusion size and area fraction limits are presently a
matter of engineering judgment.
14. More work needs to be done to reduce both the carbide
and oxide content of VIM-VAR NiTi alloys.
Thanks for your attention
w w w. s a e s g e t t e r s . c o m
w w w . m e m r y. c o m
Introduction to Stereology and

Quantitative Metallography
ASTM E 1245
George F. Vander Voort

Consultant Struers Inc.
ASTM E 1245
A Stereological Procedure to Characterize
Discrete Second-Phase Particles
Uses field and feature-specific measurements.
While the measurements employ stereological
parameters, they may be made on only one plane,
for example, the longitudinal. If the threedimensional values are desired, then additional test
planes must be assessed.
ASTM E 1245
Measure or calculate:
Area Fraction, usually in %
Number per mm2, NA
Average Length in m
Average Area in m2
Mean Free Path in m
Number of Interceptions/mm, NL
Volume Fraction A Measure of

the Concentration of a Second
Phase Constituent
V
VV =
VT
But, there is no simple way to directly measure
the volume per unit volume of a constituent!
Point Fraction Point Counting

ASTM E 562
Superimpose a grid composed of points over
the microstructure. In practice, points are hard
to see, so we use crosses or intersecting vertical
and horizontal test lines. The intersection is the
point. The point must be in the constituent to
be a hit. If it is a tangent hit, count it as
one-half. Calculate PP by:
P
PP =
PT
Number Per Unit Area, NA

The number of particles per unit area,
NA, is a measure of the quantity of
particles, that is the number density.
NA is related to the number per unit
volume, NV, which can only be
determined by serial sectioning. It is
determined by:
N
NA =
AT
The average particle length and average

particle area are calculated based upon
individual particle measurements.
Mean Edge-to-Edge Spacing,

The mean edge-to-edge spacing between
particles, known as the mean free path, is a
good structure-sensitive parameter. is
calculated from:
1 - AA

NL
Interceptions Per Unit Length, NL

NL is a measure of the number of
interceptions with phase or grain
boundaries per unit length of test line. It
is calculated from:
N
NL =
LT
N is the number of interceptions and LT is the
true line length (line length/magnification)
Results of an Experiment to Measure All

Inclusions in VIM/ESR Alloy 718 on
Three Parallel Test Planes
ASTM E 1245
Area fractions of inclusions on three parallel planes, same

specimens, of Alloy 718.
ASTM E 1245
Number per sq. mm of inclusions on three parallel planes, same

specimens, for Alloy 718.
ASTM E 1245
Average area of inclusions on three parallel planes, same

specimens, for Alloy 718
ASTM E 1245
Mean free path of the inclusions on three parallel planes, same

specimens, for Alloy 718.
Results of an experiment where an ascast strand of 303 resulfurized stainless

steel was sampled at 12 adjacent midradius locations and the sulfide
inclusions were measured by E 1245.
ASTM E 1245
Sulfide area fractions on 12 specimens taken along an as-cast strand of 303

stainless steel, at the mid-radius location.
ASTM E 1245
Sulfide number per sq. mm taken at 12 locations along an as-cast

strand of 303 stainless steel at the mid-radius location.
ASTM E 1245
Average area of sulfides taken at 12 locations along an as-cast strand of 303

stainless steel, at the mid-radius location.
ASTM E 1245
Mean free path for sulfides at 12 locations along an as-cast strand of

303 stainless steel, at the mid-radius location.
Results of an Experiment to Measure

Sulfide Inclusions in 1 Diameter Bars
from Bottom-Poured Ingots of 303
Stainless Steel
Six ingots were poured. Three were supposed to
have been rolled to billets, reconditioned and
then re-rolled to 1 diameter bar, while the other
three were supposed to have been rolled from
ingot to bar without conditioning using interstand re-heating
About a year after the project began, 106

1 diameter bars were delivered to the
R&D Center but without any ingot
codes!
The best we could do at that point was
cut a piece from each bar, split it
longitudinally, and measure the sulfides.
ASTM E 1245
Distribution of area fractions of the sulfides for 106 bars of wrought 303
stainless steel, at the mid-radius location, longitudinal plane.
ASTM E 1245
Distribution of number per sq. mm of sulfides for 106 bars of wrought 303
ASTM E 1245
Distribution of average area of sulfides for 106 bars of wrought 303

ASTM E 1245
Plot of sulfide length vs. area measurements for each of 106 wrought
bar specimens in wrought 303 stainless steel.
Study of Oxides in 52100 Bearing Steel

Made by Different Melting Practices
Heats 1, 2 and 3 EF, LT, VD, BP
Heat 4 EF, LT, VD, CC
Heats 5A and 5B EF, LT, BP (not Degassed)
Heat 6 EF/ESR
Heat 7 Production Size VIM/VAR
Heats 8 and 9 Lab Size VIM/VAR
Oxides in 52100 Bearing Steel

Electric Furnace Ladle-Treated, Bottom-Poured Steel,
Vacuumed Degassed (Heats 1-3) vs. Heat 5A, Not Degassed
Heat
VV
(%)
NA
(mm-2)
L
(m)
A
(m2)
MFP
(m)
EF1
0.0039
2.0
7.2
28.5
173147
EF2
0.0038
1.6
8.1
37.6
119992
EF3
0.0051
2.5
7.2
28.7
92186
EF 5A
0.0109
7.0
6.8
27.6
41812
1 vs 5A
99%
90%
NSS
NSS
90%
2 vs 5A
99%
95%
NSS
NSS
99%
3 vs 5A
98%
90%
NSS
NSS
99%
Oxide volume fraction and number were greater and spacing between
inclusions was less in the non-degassed heat. No size differences.

Electric Furnace Ladle-Treated, Bottom-Poured Steel,
Vacuumed Degassed (Heats 1-3) vs. Heat 5B, Not Degassed
Oxide volume fraction, number and length were greater and spacing
between inclusions was less in the non-degassed heat.

Electric Furnace, Ladle-Treated, Vacuum-Degassed and
Continuously Cast (Heat 4) vs Electric Furnace, Ladle-Treaded and
Bottom-Poured (Heats 5A and B)
Oxide volume fraction and number were greater, and spacing was less, for the
non-degassed heats.

Electric Furnace, Ladle-Treated, Vacuum-Degassed and
Continuously Cast (Heat 4) vs the Production Size VIM/VAR
(Heat 7)
Oxide volume fraction and number are lower and they are spaced farther
apart in the production VIM/VAR heat

Electric Furnace, Ladle-Treated, Vacuum-Degassed, BottomPoured (Heats 1-3) vs Laboratory Size VIM/VAR Heat 8
Oxides in the lab VIM/VAR heat (8 not 9) are lower in amount and
number, smaller in size and farther apart than in the electric furnace,
ladle-treated, vacuum-degassed, bottom-poured heats.

Non-Degassed Electric Furnace, Ladle-Treated, Bottom-Poured
Heats 5A and B vs Production VIM/VAR Heat 7
Oxides in the production VIM/VAR heat are lower in volume fraction and
number and spaced much farther apart

Non-Degassed, Electric Furnace, Ladle-Treated, Bottom-Poured
Heats 5A and B vs the Lab VIM/VAR Heat 8
Oxide volume fraction and number are lower , size smaller, and
spacing greater in the lab VIM/VAR heat 8

Production VIM/VAR Heat 7 vs Lab VIM/VAR Heat 8
Oxide volume fraction, length and area are slightly smaller in the lab
VIM/VAR heat than in the production heat
Oxides in 52100 Bearing Steel: Conclusions

Oxide volume fraction and number are reduced by
vacuum degassing electric furnace heats
Oxide volume fractions and number are further reduced
by double vacuum melting
Oxides in small (500 Lb) lab VIM/VAR heats are lower in

volume fraction and smaller in size than in larger (20,000
Lb) production heats
In general, the oxide size was unaffected by differences in
melting practice
Spacing between oxides followed the reduction in volume
fraction and number/unit area
Results of an E 1245 Experiment to

Characterize Sulfides in 303 Stainless Steel
A 100 lb (45.5 kg) Lab ingot of 303 SS was made for
the experiment.
An as-cast disk was cut from the bottom of the
ingot before hot forging.
The balance of the ingot was heated to 1260 C,
held 1 h, and forged to three cross-sectional sizes:
54 mm2, 47.5 mm2 and 35 x 25 mm (72, 78 and 91%
reductions.
Effect of Hot Reduction on NA of Sulfides

Number of Sulfides/sq. mm
3000
2500
2000
1500
1000
500
0
0
20
40
60
80
100
% Hot Reduction
Hot Forged 100 Lb Lab Ingot of 303 Stainless Steel
Effect of Hot Reduction on Avg. L of Sulfides
Average Sulfide Length, um
5
4
3
2
1
0
0
20
40
60
80
% Hot Reduction
100
Effect of Hot Reduction on Avg. A of Sulfides
Average Sulfide Area, sq. um
14
12
10
8
6
4
2
0
0
20
40
60
80
100
% Hot Reduction
Effect of Hot Reduction on of Sulfides

180
Mean Free Path, um
160
140
120
100
80
60
40
20
0
0
20
40
60
80
% Hot Reduction
100
Effect of Homogenization on of As-Cast Sulfides

184
Mean Free Path, um
182
1302 C
180
178
176
174
172
1260 C
170
168
166
0
10
15
20
Time, hours
25
Affect of Homogenization at 1260 C

on Sulfide Mean Free Path
190
Mean Free Path, m
180
As Cast
170
72% Reduction
160
150
140
78% Reduction
130
120
110
100
0
10
15
20
Homogenization Time, hours
25

on Sulfide Mean Free Path
200
Mean Free Path, m
190
As Cast
180
72% Reduction
170
160
78% Reduction
150
140
130
120
110
100
0
10
15
20
25
Average Sulfide Length, m

on Sulfide Length
6
5
78% Reduction
4
3
2
As Cast
72% Reduction
0
0
10
15
20
25
Average Sulfide Length, m

on Sulfide Length
6
5
78% Reduction
3
2
As Cast
72% Reduction
0
0
10
15
20
25
Results from an Experiment to Measure

All inclusions in VIM M50 Bearing Steel
Remelted Using Three Methods: EBR,
VAR and ESR
All 3 VIM ingots were from the same heat

with 31 ppm O and 0.004% S.
After remelting, the oxygen was 6.4, 6.7
and 20.1 ppm while the sulfur was 0.0015,
0.002 and 0.0012% for EBR, VAR and
ESR, respectively.
Tests were performed on 6 x 6 inch billets

but there were fine voids associated with the
carbides (a common problem with M50 and
similar highly alloyed steels).
Billets were forged to 1 inch square bars.
Six specimens were evaluated from the top,
middle and bottom for each remelt type (18
per type).
Inclusion Area Fraction (%) at the Top,

Middle and Bottom Ingot Locations
0.012
Area Fraction, %
0.01
0.008
VIM/EBR
0.006
VIM/VAR
VIM/ESR
0.004
0.002
0
Top
Middle
Bottom
VIM M50 Bearing Steel Bar (1 sq.) Remelted Using EBR, VAR and ESR
NA at the Top, Middle and Bottom Ingot

Locations
180
160
Number/sq. mm
140
120
100
VIM/EBR
80
VIM/VAR
60
VIM/ESR
40
20
0
Top
Middle
Bottom
VIM M50 Bearing Steel Bar (1 sq.) Remelted Using EBR, VAR and ESR
Avg. Inclusion Length at the Top, Middle and

Bottom Ingot Locations
1.4
Average Length, m
1.2
1
0.8
VIM/EBR
VIM/VAR
0.6
VIM/ESR
0.4
0.2
0
Top
Middle
Bottom
VIM M50 Bearing Steel Bar (1 Sq.) Remelted Using EBR, VAR and ESR
Avg. Inclusion Area at the Top, Middle and

Average Area, sq. m
2.5
1.5
VIM/EBR
VIM/VAR
VIM/ESR
0.5
0
Top
Middle
Bottom
Mean Free Path at the Top, Middle and

90000
Mean Free Path, m
80000
70000
60000
50000
VIM/EBR
40000
VIM/VAR
30000
VIM/ESR
20000
10000
0
1
Statistical Analysis of the Bar Data by

Remelt Practice
Type
A A, %
NA, mm-2
Avg. L, m
Avg. A, m2
, m
VIM/EBR
0.0038
71.8
0.80
0.72
44324
VIM/VAR
0.0084
117.5
0.96
0.94
14198
VIM/ESR
0.0077
54.6
1.26
1.64
17286
Level of Significance (Student t Test)

Comparison
AA
NA
EBR versus VAR
99%
80%
95%
80%
95%
EBR versus ESR
99%
nss
99%
99%
95%
VAR versus ESR
nss
95%
99%
99%
nss
nss = differences were not statistically significant
Specimens and Images for Round

Robin (11 Participants)
MnS in 416 (#1)
MnS in 1215 (B5 - #2)
MnS in modified 416 (#3)
MnS in 1215 (B2 - #4)
Sigma in 329 (#5)
Delta Ferrite in 304 (#6)
Delta Ferrite in 15-7PH (#7)
Al2O3 in Al (#8 and 9)
Examples of Images Captured and Stored
1215 B2 (#4)
1215 B5 (#2)
25 fields from each of two specimens of 1215 free-machining steel taken

from the same bar, transverse plane showing sulfides. Captured with
100x objective. Should yield very similar results.
416 Stainless Steel (#1)
CTC 5F (Mod. 416) Stainless Steel (#3)
25 fields from each of specimens of enhanced-machining stainless steels,

transverse planes showing sulfides. Captured with 100x objective. Aim sulfur
levels are approx. 0.35 and 0.5% for 416 and 5F. Hence, 5F should have a
slightly higher content of sulfides.
As-Cast 304 Stainless Steel (#6)
329 Stainless Steel (#5)
15 fields of 304 stainless steel (captured with a 50x objective) and 25 fields
(captured with a 100x objective) were very difficult subjects. The 304 contains
manganese sulfides and delta ferrite, which can be detected, while the 329 was
etched with Murakamis to reveal sigma phase. Note the fine particles at the
delta ferrite austenite interface. Both were difficult images.
15-7PH Stainless Steel (#7)
15 fields of 15-7PH stainless steel were captured with a 50x

objective. Delta ferrite was colored using 20% NaOH
electrolytically, longitudinal plane.
Al Al2O3 Composite A6 (#9)
Al Al2O3 Composite C3 (#8)
10 fields in each of two specimens of an Al-Al2O3 composite, cut from the

same component, were captured with a 20x objective. Results should be
quite similar for both specimens.
Images of a ruled test scale were

captured when each series of
specimen images were captured.
These were used for image analysis
calibration.
This was a first-order round

robin, that is, only the most basic
instructions were provided, e.g.,
nature of images, what should be
detected, and what should be
measured. The user must make all
other decisions.
Number per Unit Area, NA

Counting requires corrections for
particles that intersect the frame
border. Touching particles must be
separated to obtain an accurate
count. No specific methods were
defined.
Average Area and Length

Small particles cannot be accurately
measured, e.g., when they are
comprised of 5 or fewer pixels. No
instructions were given regarding
deletion of small particles.
Calculation of Mean and

Standard Deviation
Individual area and length data can be
handled in two ways, and this will affect the
mean and standard deviation. If all of the
individual data are summed and X and s
are calculated, the s value will be larger
than if field averages of area and length are
averaged. This difference affected the
precision evaluations.
Area Fraction Measurements

Specimen
Mean
2.177
2.386
2.105
2.351
2.386
2.964
18.31
24.76
23.85
0.209
0.341
0.376
0.182
0.490
0.376
1.049
2.218
2.473
95 %
CL
0.161
0.244
0.253
0.152
0.351
0.253
0.705
1.490
1.660
%RA
7.4
10.2
12.0
6.5
14.7
8.5
3.9
6.0
7.0
Number/mm2 Measurements
Specimen
46774 84954 28843 18502 21062 6301 47837
1770
1881
11689 17619
3700
4926
5992
1149
4608
381
368
95% CL
7852
12603
2646
3524
4286
822
3296
273
263
% RA
16.8
14.8
9.2
19.0
20.4
13.0
6.9
15.4
14.0
Mean
S
Average Area, m2, Measurements

Specimen
Mean
0.47
0.29
0.78
1.45
1.23
5.2
3.91
138.5
134.5
0.127 0.073 0.121 0.439
0.154
1.238
0.333
27.4
23.54
95% CL 0.085 0.057 0.112 0.367
0.129
1.035
0.256
21.06
18.1
10.5
19.9
6.5
15.2
13.5
% RA
18.2
20.0
14.3
25.3
Average Length, m, Measurements

Specimen
Mean
0.78
0.60
1.0
1.34
1.14
2.73
2.59
14.37
14.0
0.07
0.059 0.066 0.121
0.086
0.848
0.521
4.113
3.812
95% CL 0.058 0.049 0.057 0.112
0.072
0.074
0.40
3.16
2.93
6.3
28.7
15.5
22.0
20.9
% RA
7.5
8.1
5.7
8.4
Mean Free Path, m, Measurements

Specimen
33.66 19.97 42.03
44.5
53.98
61.57
8.42
27.06
27.91
6.75
2.31
5.73
4.04
15.84
3.08
0.49
3.24
3.08
95% CL
4.54
1.82
4.1
3.11
12.18
2.37
0.41
2.32
2.20
% RA
13.5
9.1
9.7
7.0
22.6
3.8
4.9
8.6
7.9
Mean
Average % RA, All Measurements

Specimen
Avg.
% RA
12.68 12.44 10.18
13.24
14.9
14.78
7.53
13.44 12.66
Student t values in test of significance of

differences between means
Comparison
AA
NA
MFP
B5 vs B2
(1215)
1.73
5.99
4.08
6.52
6.36
1 vs 3
(416 vs 5F)
1.95
5.57
4.88
8.18
1.17
C3 vs A6
(Al-Al2O3)
0.91
0.7
0.37
0.22
0.63
Not statistically significant Differences significant at 90% CL

Differences significant at 95% CL or better
Comparison of Similar Specimens

B5 vs B2 (both 1215, same heat): B5 sulfides had a slightly greater
area fraction, much lower NA, greater area and length and further
apart compared to B2
5F vs 416 (5F has about 0.5 % S while 416 has about 0.35 % S):
sulfide volume fraction is greater in 5F (weak statistic difference),
NA is much lower, they are larger in size but the MFP difference
was not significant
C3 vs A6 composites: no statistical difference between specimens

cut from same part.
Specimens 5 and 6 had the highest % RA.

The particles in 5 were sigma phase and
detection of the sigma was difficult as the
contrast was poorer than for the other
specimens.
Specimen 6 was delta ferrite, of low

volume fraction, but with good contrast.
However, only 15 fields were evaluated
while 25 were evaluated in specimens 1 to
5. This impaired the %RA for specimen 6.
Specimen 7 had the best (lowest)

%RA. It contained over 18% delta
ferrite and 15 fields, as for specimen
6, were evaluated. The higher
volume fraction gave a better %RA
for 15 fields.
Average % RA for All Specimens

Measurement
AA
NA
MFP
Avg. % RA
8.47
14.39
15.93
13.68
9.68
The best % RA was obtained for the

area fraction, AA, measurements, a 0dimensional measurement.
The %RA for length measurements, a
1-dimensional measurement, was better
than for the area, a 2-dimensional
measurement.
% RA for the NA data may be high

due to variations in how small
particles were counted, in how edge
corrections were (or were not) made,
and in how touching particles were
handled.
%RA for the MFP is misleading as 3

labs had erroneous results and the
writer contacted them to get theeir
data corrected.
Point Counting Inclusions
Point counting of inclusions is tedious and imprecise. This work used 100
fields measured with a 100-point grid, but the 95% confidence limits are
poor, typical for volume fractions below 2%.
Lineal Analysis of Inclusions
A Hurlbut counter was used (one hour per specimen) to measure the lineal
fraction of inclusions. Again, the precision of the measurements is poor.
Image Analysis Inclusion Measurement
Image analysis measurement of the inclusions using 1080 fields (grouped in 12 sets
of 90) gave better precision in less time than the manual measurements.
Inclusions measured by image analysis using different magnifications (field

sizes) shows the influence of the number of fields on the mean value.
The relative accuracy of the inclusion volume fractions improved with

increasing number of fields measured and is poorest for the highest
magnification (small field size increases field-to-field variability).
The relative accuracy of the inclusion area fractions improved (decreased) as

the area measured increased.
The range for the inclusion area fraction measurements increases with
magnification (decreasing field size). It is relatively constant with increasing
number of fields measured.

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A General Introduction

NMI Workshop, ATLANTA

Steel service centres

NMI Workshop, ATLANTA

New York Times Building, USA

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

Shanghai World Financial Center, China

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

Viaduc de Millau, France

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

from Baku (Azerbaijan) via Tbilisi

NMI Workshop, ATLANTA

NMI Workshop, ATLANTA

Developed for manual assessment but automatic assessment is possible

Converting the results of other standards into EN 10247 is not possible

In other standards field oriented assessment

NMI Workshop, ATLANTA

What is good cleanliness?

Parameters of steel production processes

Inclusions have mostly a negative influence on material properties and are

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

Statement of the content of nonmetallic inclusions which occur as sulfides

What is optimal cleanliness?

NMI Workshop, ATLANTA

What is optimal cleanliness?

NMI Workshop, ATLANTA

Scope of the standard

inclusions lie parallel to each other and to the main direction

Dipl.-Ing. Damian Moll

The standard does not apply to free cutting steels

NMI Workshop, ATLANTA

Basic determinations and definitions

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

Basic determinations and definitions

For all particles: e < 40 m and t < 10 m

three or more particles

two stringers overlaped

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

inclusions will be evaluated according to their shape (morphology):

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

Dipl.-Ing. Damian Moll

classification of inclusion: 7.3

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll

NMI Workshop, ATLANTA

Worst-inclusion method Method P

Worst-field method Method M

Average-field method Method K

NMI Workshop, ATLANTA

Dipl.-Ing. Damian Moll