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Metallographic

preparation of High Alloy


Tool Steels Application
Steels can broadly be classied a high standard of clean-
Notes
into three categories based on chemi- liness. Such properties
cal composition: can only be achieved by
- Carbon steels carefully controlling all
- Low alloy steels with small amounts stages of steelmaking,
of alloying elements and subsequent forging/
- High alloy steels with >6% alloying rolling and heat treatment
elements processes.
Cold work tool steel.
In addition to carbon, high alloy steels The main demands Tool for punching
contain large amounts of alloying on the metallography
elements such as chromium, nickel, departments of steel
vanadium, tungsten and molybde- producers of high quality
num. Wear resistance, toughness, alloyed tool steels are the
strength and hardness are the most following:
important characteristics of tool steel, - To handle high sample
and the alloying elements mentioned volumes efciently,
improve and optimize these me- - To use, if possible, one
chanical properties, and, if added in standard procedure for
sufcient amounts, provide specic all steel qualities,
properties such as corrosion and heat - And to deliver well
resistance, retention of hardness at polished surfaces
high temperatures, and retention of with undamaged car-
strength at low temperatures etc. bides and inclusions.
This is particularly impor-
The increasing demands of ad- tant for evaluating struc-
vanced production technologies and tures with carbides and
economic pressures in all industries inclusions of ultra clean
require steel manufacturers to con- steel.
stantly improve the quality of high
Plastic mould steel etched with 1000x, DIC
performance tool steel alloys for spe- The metallographic sample evalu- 5% Picral, revealing some singular
cial and demanding applications. For ation includes distribution and size of needles and plates at high
example, steels for making punches, carbides, detection of decarburiza- magnication in an otherwise
amorphous martensite
dies or cutting tools require very spe- tion of hardened and then tempered
cic properties such as high strength steels, detection of micro-segrega-
and hardness combined with tough- tions and inclusion ratings.
ness. In addition, these steels require

Difculties during metallographic preparation Solution:


Cutting: Grinding and polishing: Handling - Selecting the correct cut-off wheel
Efcient cutting without overheating. large sample volumes. Very ne car- - Using automatic grinding and
bides and inclusions can be pulled polishing equipment
out of the soft matrix; large carbides - Sufcient diamond polishing to
can be cracked during plane grinding. polish past the mechanical damage
of grinding

Fig.1: Thermal damage due to faulty


cutting conditions

Fig. 2: Fractured primary carbides 200x


Fig. 3:
Production and Melting Electric Arc
Production Flow Production ow
for high alloy tool
application
Furnace
steels

Rening Vacuum
Induction
Furnace

Ladle Vacuum Vacuum


Furnace Degas- Treatment
sing

The production process of high al- Casting Ingot Continuous


Casting Casting
loy steels is a sophisticated process of
melting and remelting. A mixture of iron
and well sorted scrap is rst melted in
an electric arc furnace, and cast into Remelting Vacuum
Induction
an ingot form, or continuously cast into Melting
Protective Electro- Vacuum
bloom or billet. For many applications Gas slag Arc Furnace
Electroslag Remel-
these primary products can be further Remelting ting
processed into bar, rod or plate form.
For steels with higher quality demands,
the primary product can be used as
Hot forming Hot Hot Rolling
feedstock for a secondary steelmaking Forging
process. This secondary process can
be a double or even triple remelt by
vacuum induction melting plus vacuum
arc remelting, or electroslag remelting, Heat
treatment
which can also be done under pressure and
and protective gases. machining

The main purpose of this secondary


process is to reduce impurities such as Cold work tool steel: 1.6-2% carbon, Plastic mould steel: 0.3% carbon,
oxides, sulphides and silicates so that 5-12% chromium, for punching, stamp- 12-17% chromium, for molding plastic
with successive remelts the degree of ing, deep drawing, thread rolling tools, parts for the automotive, medical and
cleanliness increases and homogenous shear blades. consumer goods industry.
ingots with excellent mechanical and Properties: high toughness, high com- Properties: Can be polished to high sur-
physical properties are produced. pressive strength and wear resistance, face nish, exceptional toughness and
The high cost of these energy intensive good nitrideability. hardness, good corrosion resistance.
remelting techniques is reected in the
price of high temperature and corrosion Hot work tool steel: 0.38% carbon, For tool making the steel is used in the
resistant martensitic and hot work tool 5% chromium, 1.5-3% molybdenum as tempered condition. After the tool
steels for special applications. and 0.5% vanadium, for pressure die is machined it is surface hardened by
casting tools. nitriding or induction hardening. The
The range of high alloy steels is very Properties: high hot strength, tough- conditions under which tools have to
wide and some products are even tailor- ness and wear resistance, high thermal operate are varied and sometimes ex-
made for especially demanding applica- fatigue and shock resistance. treme. Therefore, the variations in alloys
tions. Following are some examples of for tool steels are wery wide in order to
high alloy tool steels and their applica- High speed tool steels: 0.75-1.3% accommodate the best possible selec-
tions, with the approximate content of carbon, 4.5% chromium, 2% vanadium, tion for specic difcult and demanding
main alloying elements: 6-18% tungsten, 4-9% molybdenum, tool applications.
for taps, turning and milling tools.
Properties: retention of hardness and
toughness at elevated temperature.
High speed
cutting tool

Hot work tool steel. Tool for moulding plastic


Tool for pressure
die cast
Difculties in the
preparation of high
alloy tool steels

As heat treatability of tool steels is a Recommendations for high alloy steels


quality criterion, thermal inuence dur- are best processed
ing cutting has to be avoided in order to the preparation of high on fully automatic
give a true representation of the actual alloyed steels grinding and po-
structure. When cutting larger sections lishing machines,
and failure analysis samples this prepa- Cutting which guarantee a
ration step has to be carried out with The majority of samples are usually fast and efcient workow and reprodu-
great care. sectioned by rough mechanical means cible results. As tool steels are hard,
from slabs and blooming mill material ne grinding with diamond is more ef-
The main difculty of grinding and into standard sizes. Critical cuts for heat cient and economical than grinding with
polishing high alloyed tool steels is the treatment samples or failure analysis silicon carbide paper. Sometimes a nal
retention of carbides and non metallic are always carried oxide polish after the diamond polishing
inclusions. In cold working tool steels out with a metallo- step can be useful for contrasting and
primary carbides are very large and graphic cut-off ma- identifying carbides.
fracture easily during grinding. In the chine. High alloy tool
fully annealed conditions, secondary steels are extremely Following are suggestions for prepara-
carbides are very ne and can easily sensitive to thermal tion methods with fully automatic grin-
be pulled out from the softer matrix. damage. Therefore ding and polishing equipment, and
(See Fig. 2 front page, micrograph with special care must be semi-automatic equipment respectively.
cracked carbides). taken to select the
Processing large sample volumes of dif- appropriate cut-off wheels and secure These methods are based on experi-
ferent high alloy tool steels during vari- sufcient cooling for cutting. ence and offer excellent reproducible
ous stages of the production can be a Soft aluminium oxide or resin bonded results. Small changes may have to be
challenge, which requires a very efcient cubic boron nitride cut-off wheels are made to accommodate specic require-
organisation of the workow, automatic recommended. ments or personal preferences.
equipment and standard procedures.
Mounting
Depending on the size and volume of
the samples and the information that is
needed from them, the specimens can
be unmounted, hot or cold mounted.
Surface treated samples that need
good edge retention should be hot
compression mounted using bre-rein-
forced resins (IsoFast, DuroFast). Sam-
ples that do not require edge retention
can be left unmounted if their dimen-
sions are suited for sample holders. For
standardizing sample sizes, which can
be an advantage when handling large
volumes, cold mounting in rectangular
silicon or polypropylene mold cups (Uni-
Form) is recommended. It is important
that the cold mounting resin has little
shrinkage to avoid contamination due to
gaps between sample and resin.

Grinding and polishing


The main requirements on the prepara-
tion of high alloy tool steels are a true
representation of form, amount and size
of carbides, and the retention of non-
metallic inclusions in an undeformed
matrix. Large volumes of samples of
Grinding Grinding

Step PG FG Step PG FG

Surface Stone 150# MD-Allegro Surface MD-Piano 220 MD-Allegro

DiaPro
Suspension 9 m Suspension
Allegro/Largo

Lubricant Water Blue Lubricant Water

rpm 1450 150 rpm 300 150

Force [N] 300 300 Force [N] 210 210

Time As needed 9 min. Time As needed 7 min.

Polishing Polishing

Step DP 1 DP 2 Step DP 1 DP 2 OP 1*

Surface MD-Dac MD-Nap Surface MD-Dac MD-Nap MD-Chem

Suspension 6 m 1 m Suspension DiaPro Dac DiaPro Nap B OP-AA

Lubricant Blue Blue rpm 150 150 150

rpm 150 150 Force [N] 210 150 90

Force [N] 300 150 Time 6 min. 1 min. 1 min.

Remark: DiaPro diamond suspensions can be substituted with *Optional


Time 6 min. 4 min. DP-Diamond suspension P as follows: For FG with 9m,
DP 1 with 3 m, DP 2 with 1m.

Table 1: Preparation method for high alloy tool steel on large Table 2: Preparation method for high alloy tool steel on table models
automatic equipment semi-automatic equipment

The preparation data in Table 1 are for


6 samples, 65x30 mm, unmounted or Etching and structure interpretation
cold mounted, using Struers MAPS or
AbraPlan/AbraPol. Etching the white primary carbides stand out.
Usually samples of tool steel are rst ex- For ne globular pearlite a brief sub-
For smaller sizes and numbers of amined unetched to identify inclusions mersion into picric acid followed by 2%
samples semi-automatic grinding and and carbide size and formation. Nital gives a good contrast and avoids
polishing equipment will give also good, For revealing the structure, either Nital staining.
reproducible results. or picric acid in various concentrations
is used. For instance, to show the car- For mixing and working with etching
The data in Table 2 are for 6 samples, bide distribution in cold work steel a solutions standard safety precautions
30 mm mounted, clamped into a sam- 10% Nital colors the matrix dark while have to be observed.
ple holder, using Struers TegraPol-31/
TegraForce-3 with TegraDoser-5.

Fig. 4: Cold work tool steel etched 100x Fig. 5: Hot work tool steel etched 500x
with 10% Nital, primary carbides with Picral and Nital, globular pearlite
stand out white
High speed tool steel after nal heat treatment, very Plastic mould steel is a corrosion resist- Fig. 9: Plastic mould steel, etched in 100x
ne structured martensite with chromium carbides ant tool steel which before heat treating 5% Picral, amorphous martensite with
strings of primary carbides
shows an amorphous martensite with
Nital: strings of carbides (Fig. 9). After anneal-
100 ml ethanol ing it shows nely dispersed carbides
2-10 ml nitric acid (Caution do not (Fig.10).
exceed 10% solution, explosive!) The even distribution of carbides in tool
steel can be improved by powder met-
Picric acid etching solution: allurgical process. Through a powder
100 ml ethanol making process and subsequent hot
1-5 ml hydrochloric acid isostatic pressing, a homogenous, seg-
1-4 g picric acid regation free steel is made, which is es-
pecially suitable for unconventional tool
Structure interpretation geometries that would be expensive to Fig.10: Plastic mould steel after 500x
Generally high alloyed steels have the make by mechanical means (Figs.11 annealing shows very ne carbides
same structural phases as regular iron- and 12).
carbon alloys: ferrite, pearlite, martensite
and austenite, but the solid solution can
absorb a certain amount of alloying ele-
ments. Carbon forms complex carbides
with some alloying elements such as
chromium, tungsten and vanadium. In
addition, the solubility of carbon in iron
changes: Adding alloying elements such
as silicon, chromium, tungsten, mo-
lybdenum and vanadium increases the
alpha area of the iron-iron carbon dia-
gram, while adding nickel and manga- Fig. 6: Cold work tool steel after initial hot 200x
nese will enlarge the gamma area. These forming, slightly contrasted by a short nal oxide
polish, showing large primary carbides in a ferritic-
characteristics inuence the time-tem- pearlitic matrix
perature transformation which is speci-
cally important for the heat treatment of
tool steels.

The primary structure of cold work tool


steel is a ledeburite. Its coarse structure
is transformed through hot rolling or
forging into a ferritic-pearlitic matrix with
large primary carbides (Fig. 6). A subse-
quent full annealing shapes the second-
ary ne carbides (Fig. 7). Fig. 7: Fully heat treated cold work tool 200x Fig.11: Carbide distribution in
steel showing very nely dispersed secondary conventionally produced steel
Hot work tool steels in the fully heat carbides and small white primary carbides
treated condition show ideally a tem-
pered martensitic matrix containing very
ne globular pearlite (Fig. 5). Here it is
important that segregations from the pri-
mary structure are as much as possible
evened out through heat treatment as
uneven chemical composition can lead
to corrosion problems (Fig. 8).

Fig. 8: Hot work tool steel 100x Fig.12: Carbide distribution in powder
showing segregations metallurgically produced steel
Struers A/S
Pederstrupvej 84
DK-2750 Ballerup, Denmark
Phone +45 44 600 800
Fax +45 44 600 801
struers@struers.dk
www.struers.com

Summary Application DEUTSCHLAND


Notes Struers GmbH
An ever larger portion of high alloy tool Karl-Arnold-Strasse 13 B
Metallographic preparation of D- 47877 Willich
steels are today made to t custom- High Alloy Tool Steels Telefon +49/(0) 21 54/4 86-0
ers applications. This requires the e-mail: verkauf.struers@struers.de
Elisabeth Weidmann, Anne Guesnier, STERREICH
production of very clean material with Struers GmbH
Struers A/S, Copenhagen
very specic mechanical, physical and Judy Arner, Struers Inc, Westlake, Ohio, USA
Zweigniederlassung sterreich
Ginzkeyplatz 10
metallurgical properties. Metallographic Bill Taylor, Struers, Ltd., Glasgow, UK A-5020 Salzburg
inspection from the initial casting and Telefon (0662) 625711
e-mail: stefan.lintschinger@struers.de
rst forming stages, to the nal semi- Bibliography
Schumann, VEB Deutscher Verlag fr SCHWEIZ
nished, heat treated product, is an es- Grundstofndustrie, Leipzig 1968
Struers GmbH
Zweigniederlassung Schweiz
sential tool for controlling manufacturing Dohmke Verlag W. Giradet, Essen, 1977 Weissenbrunnenstrasse 41
Metals Handbook, Desk Edition, ASM, Metals Park, CH-8903 Birmensdorf
and heat treatment processes. Telefon (01) 77763-07
Ohio, 44073, 1985 e-mail: rudolf.weber@struers.de
Color Metallography, E. Beraha, B. Shpigler, ASM,
The main challenges regarding metal- THE NETHERLANDS
Metals Park, Ohio, 44073, 1977 Struers GmbH Nederland
lographic preparation are managing the Metallographic etching, G. Petzow, ASM, Metals Park, Electraweg 5
Ohio, 44073, 1978 NL-3144 CB Maassluis
large sample volume, and producing Tel.: +31 (0) 10 599 72 09
consistently excellent surface nishes. e-mail: glen.van.vugt@struers.de
Acknowledgements
CZECH REPUBLIC
As size, form and distribution of car- We wish to thank Bhler Edelstahl GmbH, Kapfenberg, Struers GmbH
bides and inclusion are the main quality Austria, for generously supplying information, sample Ocel sk 799
material, and the permission to reproduce drawing CZ-190 00 Praha 9
indicators of tool steel, it is essential Tel. 02 / 84 818 227
and photos on page 2 and 3, Figs. 6, 11 and 12 on page e-mail: david.cernicky@struers.de
that they are retained during prepara- 5, photo of punching tool on page 1 and of stamping
POLAND
tion. Automatic grinding and polishing, tool on page 6. Special thanks to J. Hofsttter and A. Struers Sp. z o.o.
using diamond for ne grinding and Dreindl for their co-operation. Oddzia w Polsce
ul. Lirowa 27
polishing, gives good and reproducible PL-02-387 Warszawa
Tel.: 022/824 52 80
results. Using one preparation method For further details on the mentioned Struers e-mail: grzegorz.uszynski@struers.de
applicable for all the various types of equipment, accessories and consumables please HUNGARY
tools steels makes the handling easy see www.struers.com or contact your local Struers GmbH
Struers representative. Magyarorszgi ktelep
and efcient. Pusks Tivadar u. 4
H-2040 Budars
Phone (23) 428-742
Fax (23) 428-741
e-mail: zoltan.kiss@struers.de
FRANCE
Struers S.A.S.
370, rue du March Rollay
F- 94507 Champigny
sur Marne Cedex
Tlphone +33 1 55 09 14 30/31
e-mail: struers@struers.fr
BELGIQUE
Struers S.A.S.
370, rue du March Rollay
F- 94507 Champigny
sur Marne Cedex
Tlphone +32 43 70 93 18
e-mail: struers@struers.fr
JAPAN
Marumoto Struers K.K.
Takara 3rd Building
18-6, Higashi Ueno 1-chome
Taito-ku, Tokyo 110-0015,
Phone: +81 3 5688-2914
e-mail: struers@struers.co.jp
SINGAPORE
Struers A/S
10 Eunos Road 8, #12-06 North Lobby
Singapore Post Centre
Singapore 408600
Phone +65 6299 2268
e-mail: struers.sg@struers.dk
UNITED KINGDOM
Struers Ltd.
Erskine Ferry Road, Old Kilpatrick
Glasgow, G60 5EU
Phone 01 389 877 222
e-mail: info@struers.co.uk
USA and Canada
Struers Inc.
24766 Detroit Road
Westlake, OH 44145-1598
Phone (888) 787-8377
e-mail: info@struers.com

09.04 / 62140204
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