Metallographic

preparation of powder
metallurgy parts Application
Next to casting, mechanical forming
and machining, powder metallurgy
lurgy for the high volume production of
small, intricately shaped, and/or very
Notes
(P/M) technology is an important precise parts such as gears and links.
method of manufacturing metal parts.
Undesirable characteristics of ingot- In addition, the process offers the
based metals can be greatly reduced, potential to produce a wide variety
and desired properties of metals which of alloys with different material
would normally not alloy easily can be properties such as high tem-
achieved by combining different metal perature toughness and hard-
powders or mixtures of metal and non ness. High speed cutting tool
metal powders. bits from sintered tungsten
carbide powder are an example of
The process of making powders, com- the variety of different properties which
pacting them into useful shapes and can be achieved with the powder metal-
then sintering them is costly, but the lurgical process.
finished parts have some specific ad-
vantages over wrought or cast parts. As the density of the compacted and
sintered part influences its key proper-
The main advantages are: ties of strength, ductility and hardness,
- the possibility to make fine grained a specific porosity is critical. For pro-
homogenous structures cess control, metallography is used to
- the ability to form complicated check porosity, non-metallic inclusions
shapes with close dimensional and cross-contamination. In research
tolerances and failure analysis, metallography is a
- and the ability to produce parts with major tool used to develop new prod-
a superior surface finish. ucts and improve manufacturing pro-
cesses. In addition to chemical analysis,
Costly machining processes are thus quality control also includes physical
reduced or eliminated and consequently methods for checking density, dimen-
there is less scrap loss compared to sional changes, flow rate etc.
other forming methods. It is therefore
most economical to use powder metal- less
stain
P/M
m e ntal tched
eri e
Exp , colour
l
Difficulties during metallographic preparation Solution: stee

Grinding and polishing: Sufficiently long polishing

To reveal the structure with the correct and representative porosity.

Fig.1: Porosity of a P/M steel sample after a Fig. 2: Same sample as Fig.1 after 8 min. Different powder metallurgy steel components
4 min. polish with 3 µm diamond polish with 3 µm diamond
Production of Synchronising hub

powder metallurgy
parts

Manufacturing process of iron and steel powders

Production produce pure iron powder. It is used for al- A good powder mix not only has the ability to
To achieve the desired structure and near net loying and low density applications, such as produce the required properties of a specific
shape of a powder metal part, stringent pro- bearings. alloy, but also needs to facilitate handling,
cess control of the following production steps compacting and sintering.
is required: In the atomizing process molten metal of For instance, the easy flow of powder and its
the desired alloy flows through a nozzle and capability to mix evenly with other powders
- Making the powder is struck by high pressure water or gas jet. is important for an even powder distribution
- Mixing the powder with additions such as Small droplets are formed which solidify into before pressing, and ensures uniform proper-
lubricant, carbon and/or alloying elements particles. Atomized powders result in higher ties of the finished part.
- Compacting the powder in carbide dies densities than mechanically crushed pow-
- Sintering at high temperature (1100- ders, therefore all steel powders are produced For the production of components the mixed
1200°C) in a protective atmosphere by atomizing. powders are first compacted under high pres-
sure in a carbide die. At this stage the part
Chemical and atomisation methods are the Copper powder is made by atomizing or elec- has the geometrical features of the finished
two most common methods for powder pro- trolytic methods. Tungsten carbide powder component, but not its strength and is called
duction. The chemical method converts metal is produced by adding controlled amounts of the “green” part. In order to develop the
from ore oxides directly to metal powder at carbon to the tungsten powder and carburis- mechanical and physical properties of the
a temperature below the melting point. For ing it at 1400 - 2650°C material, metallurgical bonding has to take
example, iron powder is made through direct place through sintering at high temperature
reduction from iron ore into sponge iron. The Powder production and mixing is a highly in a sintering furnace. The bonding occurs
sponge iron is then mechanically crushed to specialized and complex process which pro- through diffusion between adjacent particles.
powder, which is further refined through duces custom made powder mixes designed To avoid oxidation, which would impair the
annealing under reducing atmosphere to to satisfy the needs of a specific application. inter-particle bonding, the sintering process
is conducted in a protective atmosphere.

The bonding increases the density, and

pressed and sintered powder metal parts
generally contain between 5 and 25% residual
porosity. Depending on the application some
parts may need an additional hot isostatic
pressing for better dimensional accuracy, or
surface finish or impregnation with oil. Final
treatments, such as surface hardening, plat-
ing or coating can be applied.

Sponge iron powder, SEM Atomized iron powder, SEM

 Difficulties in the
metallographic
preparation of
powder metallurgy
parts
Fig. 3:
Sintered tungsten carbide
(WC/Co), etched with
Murakami’s reagent.
1500 x

The sintering of cemented carbides is carried The main challenge during the preparation is
out in a vacuum sintering process. to show the true porosity after grinding and
The carbide powder is mixed with 3-25 w% polishing. Depending on the hardness of the
cobalt and small amounts of titanium and material this can be more or less successful.
tantalum carbides are added to inhibit grain During the grinding of soft metals, abraded
growth. This mixture is pressed and sintered. metal is pushed into the pores, which then
At 1280 – 1350°C the liquefaction of cobalt has to be removed by polishing.
takes place and results in the formation of a Samples from parts in which hard and soft
eutectic-like phase of WC/Co. Densification materials are mixed are prone to show pro-
begins at lower temperatures and reaches a nounced relief. The preparation of green parts
theoretical 100% shortly after the liquefaction needs particular care and patience as they are
has occurred. During liquefaction the part very fragile.
shrinks up to 40% in volume. Fig. 4: Carbide distribution in conventionally
produced steel
Recommendations for the
Applications
Components made by powder metallurgy are
preparation of powder
mainly used for the following applications: metallurgy parts
Cutting
- Mechanical and structural parts, mainly iron For sectioning a powder metallurgy com-
based, but also from copper, brass, bronze ponent of a specific metal or alloy one can
and aluminium. The largest user of P/M parts select an appropriate cut-off wheel using the
is the automotive industry. Component sup- recommended charts and guidelines. For
pliers make connecting rods, synchronizing mixed materials it is recommended to use a
hubs, chain sprockets, cams and gears. cut-off wheel suitable for cutting the material
- Refractory metals which, due to their high which constitutes the major part. For sintered
melting points, are difficult to produce by carbides a resin bonded diamond cut-off
melting and casting. Fig. 5: Carbide distribution in powder wheel is recommended (e.g. B0DXX). Green
metallurgically produced steel
parts need to be mounted in cold mounting
- Porous material in which controlled poro- resin (see section “Mounting”) before cutting,
sity serves a specific purpose, for instance so that they are not crushed by clamping.
self lubricating bearings.
Mounting
- Composite materials that do not form al-
In order to assure good adhesion of the
loys, for instance copper/tungsten for electri-
mounting resin to the sample material it is
cal contacts, cemented carbide cutting tools
essential to degrease the sample thoroughly
(Fig. 3), materials for brake linings and
with acetone, toluene or Isopar C* before
clutch facings, diamond cutting tools, or
mounting (Use proper safety precautions
metal matrix composites.
when handling solvents!).
- Special high-duty alloys, such as nickel
and cobalt based super alloys for jet engine Sintered parts can be mounted with a resin
parts, and high speed tool steels, which have suitables to the mechanical properties of the
an even distribution of carbides and have sample material: For hot compression mount-
isotropic qualities (Figs. 4 and 5). ed either phenolic resin (MultiFast) or resins
containing harder filler material (DuroFast,
In addition, different powders and powder LevoFast). For a cold mounting acryllic resins
mixtures for thermal spray coatings are pro- with filler (DuroCit-3 or LevoCit) can be used.
duced and are also subject to metallographic For more information see www.struers.com
quality control. Green parts need to be re-impregnated after
sectioning under vacuum with a cold mount-
ing epoxy resin (CaldoFix-2, EpoFix,
SpeciFix-40).
Powders can be mounted by mixing a small
amount (about 1/2 teaspoon) of powder with
a slow curing epoxy resin and pouring it into
a mounting cup. During the approx.12 hours
curing process the particles will form a layer
by settling at the bottom of the cup.

*Available from Exxon

 Preparation method for Grinding
P/M bronze

Step PG
FG

Foil/Paper MD-Largo

Type SiC Diamond

Fig. 6: Abrasive
Size #320 9 μm
Surface of P/M steel
after fine grinding
on MD-Allegro Suspension/ Water DiaPro
Lubricant Allegro/Largo 9

rpm 300 150

Force [N]/ 35 25
specimen

Time (min) As needed 4

Polishing

Fig. 7: Same sample as in Fig. 6 showing Fig. 9: Larger magnification of surface from Fig. 7, Step DP OP
insufficient polish showing metal “lids” covering pores

Surface MD-Mol MD-Chem

of diamond polishing to remove the metal
pushed into the pores during grinding and
Type Diamond Silica
reveal the correct porosity. For soft metals the Abrasive
final polishing time should not be prolonged Size 3 µm 0.04 µm
unnecessarily, as this leads to rounding of
Suspension/ DiaPro Mol R3 OP-S NonDry
the pore edges. Starting with 500# or 800#, Lubricant
green parts are ground manually on silicon
carbide Foil/Paper to 4000#. The surface is rpm 150 150
re-impregnated as needed. Polishing can be
done on a semi-automatic polishing machine
Force [N]/ 25 25
Fig. 8: Same sample as in Fig 7 after longer polish for individual samples. specimen
showing correct porosity
In order to establish the exact polishing time
Time (min) 4 1
for specific alloys and parts, it is recom-
Hard metal powders can be hot compression
mended to check the structure during polish-
mounted by mixing with one measuring spoon Table 1: Preparation method for 6 samples of P/M bronze, mounted,
ing every two minutes with the microscope, 30 mm dia., using the semi-automatic Tegramin, 300 mm dia.
of the fine grained mounting resin DuroFast.
and only proceed to the next polishing step
As an alternative to DiaPro polycrystalline diamond suspension P,
when all residual metal has been removed 9 µm, 3 µm and 1 µm can be used together with red and green or blue
The mixture is then poured into the cylinder
from the pores. lubricant.
of the mounting press and is topped with
phenolic resin.

Grinding and polishing

The grinding and polishing procedure for
powder metals follows the same rules which
are applied to prepare ingot based samples of
the same material.
Plane grinding high volumes of samples
of materials >150 HV can be carried out on
an aluminium oxide grinding stone or
a diamond grinding disc (MD-Piano).
Materials <150 HV can be plane ground on Fig.10: Water stains from cleaning can lead to Fig.11: P/M bronze, unetched, containing 500x
silicon carbide Foil/Paper. misinterpretation of structure graphite (grey), and α-δ eutectoid (blue)

For fine grinding with diamond the fine grind- Cleaning and drying
ing disc MD-Allegro is suitable for materials After polishing it is essential to clean the sam-
>150 HV and MD-Largo for materials <150 ple with a water/detergent mixture to remove
HV. This is followed by a thorough diamond remnants of the polishing suspension and
polish with 3 µm and a brief final polish with lubricant from the pores. The sample is then
1 µm or with oxide polishing suspensions. rinsed with water, followed by a thorough
As one of the major goals of preparing a rinse with isopropanol and dried with a
powder metallurgical sample is to show the warm stream of air, holding the sample at an
true porosity, it is important that the diamond angle. Do not blow the stream of air directly
polishing step is carried out long enough to
achieve this goal (see Figs. 6-9). For large or Fig.12: Same as Fig.11, etched with 500x
soft samples it can take up to 10-15 minutes iron-III-chloride, showing grain structure
of bronze
Grinding Preparation method Preparation method Grinding
for P/M steel for sintered carbides

Step PG FG Step PG FG

Surface Foil/Paper MD-Allegro Surface MD-Piano MD-Allegro

Type SiC Diamond Type Diamond Diamond

Abrasive Abrasive
Size #220 9 μm Size #220 9 μm

Suspension/ Water DiaPro Suspension/ Water DiaPro

Lubricant Allegro/Largo 9 Lubricant Allegro/Largo 9

To reveal the structure, the common chemical

rpm 300 150 rpm 300 150
etching solutions for metals and their alloys,
that are recommended in the literature, can
Force [N]/ 35 30 be used. The following procedure is recom- Force [N]/ 30 30
specimen specimen
mended for etching: wet the surface with
isopropanol, immerse sample face up into
Time (min) As needed 5 etchant and slightly agitate. When the ap- Time (min) As needed 4
propriate etching time has elapsed, take the
Polishing sample out of the etchant and rinse either Polishing
with isopropanol or water depending on the
Step DP 1 DP 2 etchant (see below) and dry with a stream Step DP OP
of warm air. Interpretation and photographic
documentation should take place immediately
Surface MD-Mol* MD-Nap after drying. Surface MD-Dac MD-Chem*

Type Diamond Diamond Etching time depends on the alloy and it needs Type Diamond Silica
Abrasive Abrasive
Size 3 μm 1 μm some experience for the correct timing. Etch- Size 3 μm 0.04 μm
ing too short will not give sufficient contrast
Suspension/ DiaPro DiaPro of the different phases. If the sample is over- Suspension/
DiaPro Dac 3 OP-U NonDry
Lubricant Mol B 3 Nap B 1 Lubricant
etched, it is difficult to distinguish the various
phases (see Figs.15-17). When working with
rpm 150 150 rpm 150 150
unfamiliar material it is recommended to etch
shorter rather then longer and to check the
Force [N]/ 30 20 result with the microscope first. More etching Force [N]/ 30 20
specimen specimen
can be carried out if necessary, but if the sam-
ple is overetched, it needs to be repolished.
Time (min) 6-8 0.5 - 1 Following are some of the common etchants. Time (min) 4 1
Follow standard safety precautions when
Table 2: Preparation method for 6 P/M steel samples, mixing and working with chemical reagents! Tabel 3: Preparation method for 6 samples of sintered carbides,
mounted, 30 mm dia., using the semi-automatic Tegramin, mounted, 30 mm dia., using the semi-automatic Tegramin, 300 mm dia.
300 mm dia.
As an alternative to DiaPro polycrystalline diamond suspension P, 9 µm,
As an alternative to DiaPro polycrystalline diamond Copper and copper alloys: 3 µm and 1 µm can be used together with green/blue lubricant.
suspension P, 9 µm, 3 µm and 1 µm can be used together
with green or blue lubricant.
1. 100 ml water *Optional step

*Alternatively MD-Dac/DiaPro Dac 3 can also be used.

20 ml hydrochloric acid
5 g Iron-III-chloride
from the top onto the sample surface as it 10-20 sec
forces the liquids out of the pores, which Rinse with water followed by isopropanol
will leave stains on the surface (Fig.10). It is 2. 100 ml water
important to use a high quality alcohol for 10 g ammonium persulfate. Use fresh only!
rinsing to keep staining to a minimum. Rinse with water followed by isopropanol
Steel:
Etching
It is recommended to examine the unetched 1. 1-3% Nital for iron-carbon alloys, iron-
sample first to check the density, shape and carbon-copper alloys and pre-alloyed
size of the pores, oxidation and inclusions, iron-molybdenum:
sintering necks and free graphite (see Figs.11 100 ml ethanol Fig.13: P/M steel with 0.5%C, diffusion alloyed with Ni, Cu and
and 12). It is important to know the theo- 1-3 ml nitric acid Mo. Etched in picral, showing areas of fine pearlite surrounded
retical density in order to compare it to the 10-60 sec depending on carbon content. by ferrite, martensite, bainite and Ni-rich austenite.

porosity. Rinse with isopropanol (Fig.14)

After this initial inspection it is recommended 2. Picral to develop difference between
to etch the sample immediately to avoid dry- martensite and austenite:
ing stains, which form when cleaning and 100 ml ethanol
drying liquids are gradually released by the 4 g picric acid
pores. For very dense sintered carbides this 10-60 sec. depending on carbon content.
is not as important as for any powder metal Rinse with water followed by isopropanol
with a certain amount of porosity. (Fig.13)

Fig.14: P/M steel with 0.8% C, pre alloyed with 1.5% Mo.
Etched with nital, showing dense bainite
 Struers ApS
Pederstrupvej 84
DK-2750 Ballerup, Denmark
Phone +45 44 600 800
Fax +45 44 600 801
[email protected]
www.struers.com
Fig.15: Etched too short
3. For contrast between pearlite, bainite
and martensite: AUSTRALIA & NEW ZEALAND
Struers Australia
NETHERLANDS
Struers GmbH Nederland
200 ml ethanol 27 Mayneview Street Zomerdijk 34 A
Milton QLD 4064 3143 CT Maassluis
4 g picric acid Australia Telefoon +31 (10) 599 7209
Phone +61 7 3512 9600 Fax +31 (10) 5997201
1-2 ml nitric acid Fax +61 7 3369 8200 [email protected]
20-100 sec, depending on carbon content [email protected]
NORWAY
and alloying elements. BELGIUM (Wallonie) Struers ApS, Norge
Struers S.A.S. Sjøskogenveien 44C
Rinse with water followed by isopropanol 370, rue du Marché Rollay 1407 Vinterbro
F- 94507 Champigny Telefon +47 970 94 285
sur Marne Cedex [email protected]
Stainless steels: Téléphone +33 1 5509 1430
Vilella’s reagent: Télécopie +33 1 5509 1449
[email protected]
AUSTRIA
Struers GmbH
45 ml glycerol Fig.16: Etched too long, over etched Zweigniederlassung Österreich
BELGIUM (Flanders) Betriebsgebiet Puch Nord 8
15 ml nitric acid Struers GmbH Nederland 5412 Puch
Zomerdijk 34 A Telefon +43 6245 70567
30 ml hydrochloric acid 3143 CT Maassluis Fax +43 6245 70567-78
30 sec to 5 min Telefoon +31 (10) 599 7209
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Rinse thoroughly with water followed by [email protected] POLAND

Struers Sp. z o.o.
isopropanol CANADA Oddział w Polsce
Struers Ltd. ul. Jasnogórska 44
7275 West Credit Avenue 31-358 Kraków
Sintered tungsten carbides: Mississauga, Ontario L5N 5M9 Phone +48 12 661 20 60
Murakami‘s reagent Phone +1 905-814-8855
Fax +1 905-814-1440
Fax +48 12 626 01 46
[email protected]
100 ml water [email protected]
ROMANIA
10 g potassium or sodium hydroxide CHINA Struers GmbH, Sucursala
Struers Ltd. Bucuresti
10 g potassium ferricyanide No. 1696 Zhang Heng Road Str. Preciziei nr. 6R
Zhang Jiang Hi-Tech Park 062203 sector 6, Bucuresti
Etching by immersion or swab etch Shanghai 201203, P.R. China Phone +40 (31) 101 9548
Fig.17: Correct etching
Rinse thoroughly with water followed Phone +86 (21) 6035 3900
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Author SWITZERLAND
CZECH REPUBLIC & SLOVAKIA Struers GmbH
Elisabeth Weidmann, Birgitte Nielsen, Struers GmbH Organizační složka Zweigniederlassung Schweiz
Summary Struers A/S, Copenhagen, Denmark vědeckotechnický park Weissenbrunnenstraße 41
Powder metallurgy is a method of produc- Judy Arner, Struers, Inc., Westlake, OH, USA Přílepská 1920, CH-8903 Birmensdorf
CZ-252 63 Roztoky u Prahy Telefon +41 44 777 63 07
ing parts from metals which normally would Acknowledgements
Phone +420 233 312 625 Fax +41 44 777 63 09
Fax +420 233 312 640 [email protected]
not alloy easily, or from mixtures of metals We wish to thank Höganäs AB, SE 26383 Höganäs, [email protected]
[email protected] SINGAPORE
and non-metals, taking advantage of their Sweden, for the co-operation and supplying information Struers Singapore
and material for reproduction: all photos of P/M GERMANY 627A Aljunied Road,
combined properties. Although the powder Struers GmbH #07-08 BizTech Centre
components, diagram and SEM photos on page 2, Figs.
metallurgical process is costly, it has the 1, 2, 6, 7, 8, 9, 10, and 13 - 17. Special thanks go to
Carl-Friedrich-Benz-Straße 5
D- 47877 Willich
Singapore 389842
Phone +65 6299 2268
advantage of economically producing large M. Carlsson who generously shared her professional Telefon +49 (0) 2154 486-0 Fax +65 6299 2661
experience with us. Fax +49 (0) 2154 486-222 [email protected]
amounts of small and intricately shaped parts [email protected]
Figs. 4 and 5 courtesy Böhler Edelstahl GmbH, SPAIN
with homogenous structures. The density of Kapfenberg, Austria FRANCE Struers España
compacted and sintered parts affects their Struers S.A.S.
370, rue du Marché Rollay
Camino Cerro de los Gamos 1
Building 1 - Pozuelo de Alarcón
Bibliography
strength, ductility and hardness. Therefore Höganäs Handbook for sintered components, 6.
F-94507 Champigny CP 28224 Madrid
sur Marne Cedex Teléfono +34 917 901 204
metallographic control of porosity is an inte- Metallography, Höganäs AB, 1999 Téléphone +33 1 5509 1430 Fax +34 917 901 112
Télécopie +33 1 5509 1449 [email protected]
gral part of quality control. Höganäs iron and steel powders for sintered [email protected]
During metallographic grinding, metal is components, Höganäs AB, 1998 FINLAND
Structure 24, Metallographic examination of P/M HUNGARY Struers ApS, Suomi
pushed into the pores and if the subsequent stainless steel matrix composites, N. Frees, Institute for
Struers GmbH
Magyarországi Fióktelepe
Hietalahdenranta 13
00180 Helsinki
polishing steps are not carried out properly, Product Development, Technical University, Lyngby, 2040 Budaörs Puhelin +358 (0)207 919 430
Szabadság utca 117 Faksi +358 (0)207 919 431
residual metal “lids” covering the pores will Denmark, 1991 Phone +36 2380 6090 [email protected]
Metallographic etching, G. Petzow, ASM, Metals Park, Fax +36 2380 6091
obstruct the evaluation of the correct poros- Email: [email protected] SWEDEN
Ohio, 1978
ity. Thorough grinding and polishing with IRELAND
Struers Sverige
Box 20038
diamond, and microscopic checks between Struers Ltd. 161 02 Bromma
Unit 11 Evolution@ AMP Telefon +46 (0)8 447 53 90
polishing steps, assure a true representation Whittle Way, Catcliffe Telefax +46 (0)8 447 53 99
Rotherham S60 5BL [email protected]
of the structure. The given procedures for Tel. +44 0845 604 6664
automatic preparation and the chemical etch- Fax +44 0845 604 6651
[email protected]
UNITED KINGDOM
Struers Ltd.
ants have been used successfully in day to Unit 11 Evolution @ AMP
ITALY Whittle Way, Catcliffe
day practical laboratory application and give Struers Italia Rotherham S60 5BL
Via Monte Grappa 80/4 Tel. +44 0845 604 6664
reproducible results. 20020 Arese (MI) Fax +44 0845 604 6651
Tel. +39-02/38236281 [email protected]
Fax +39-02/38236274
[email protected] USA
Struers Inc.
JAPAN 24766 Detroit Road
Marumoto Struers K.K Westlake, OH 44145-1598
P/M steel with copper infiltration Takanawa Muse Bldg. 1F Phone +1 440 871 0071
3-14-13 Higashi-Gotanda, Fax +1 440 871 8188
Shinagawa [email protected]
Tokyo
141-0022 Japan
Phone +81 3 5488 6207
Fax +81 3 5488 6237
[email protected] 28.02.2019 / 62140805