Data Conferma/Confirmation Date: 13 nov 2013

METALLOGRAPHIC SPECIMENS
Fiat Group MATERIAL STANDARD
Powder metallurgy
Automobiles Sampling and preparation of 50210/01
normazione metallographic specimens Page: 1/5
Date: 10/23/2009
BOGGIO RICCARDO - RICCARDO.BOGGIO@CRF.IT
ROLLI RAFFAELLA - RAFFAELLA.ROLLI@CRF.IT

TMD
PURPOSE
This Standard covers methods for sampling and preparing metallographic specimens of: sint-
ered powder metal components.

-
3Code
Ch.
Change Date Description

= Nov. '92 Edition 1 - New . (MM)

Edition
Supervisor
Author

= 07/12/05 Edition 2 - § 4.1.1 changed . (FD)

= 10/23/09 Edition 3 – Completely revised (CL)

C.R.F. - Group Materials Labs Physical Analysis & Common Testings
C.R.F. - Group Materials Labs Physical Analysis & Common Testings

DISPUTE THE ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

PARTIES WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD
CONFIDENTIAL
Supervisor department
Author Department

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50210/01 Change

1
GENERAL

NOTE: The major difference between sintered powder metal parts and machined parts is the
presence of residual porosity. Any moisture trapped in pores during specimen preparation
may be released during etching or other stages and cause stains which can conceal the
material's real microstructure.

Properties of sintered materials which are evaluated on metallographic specimens include:

—Total porosity ( on selected cross section only)
— Porosity size and configuration
— Powder particle shape in only compacted component (not sintered yet)
— Metallic inclusions
— Manganous sulfide additions to improve machinability
— Alloying element segregation (alloy uniformity)
— Grain size and the presence of different phases
— Surface coatings
— Other.

1.1
The methods which are normally used for metallographic examination of sintered materials
are described below.

Preliminary operations are as follows:

a) Sampling
b) Specimen preparation
c) Etching.

2
SAMPLING
WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISPUTE THE ONLY
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

2.1

Component dimensions permitting, sample size shall be sufficient for preparation of a

VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

specimen having an effective surface area exceeding 140 mm2. Sample shall be
representative of the material's properties or of the problem in question.

2.2
CONFIDENTIAL

Samples shall be sectioned from part by abrasive-wheel cutting *.

Material shall be cooled during cutting by directing a flow of water or oil-water emulsion over
surface.

* Resin-bonded unreinforced cutoff wheel.

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Fiat Group Automobiles Change 50210/01
2.3
The piece obtained after the cut shall be cleaned with alcohol in ultrasonic cleaning
equipment. The cleaning in an ultrasonic cleaner is important in order to eliminate swarfs
produced by the cut and the coolant retained in pores. Then the piece shall be dried under
vacuum for at least 15 minutes.
Sample shall be mounted in resin (e.g. epoxy resin) at high temperature and pressure.

2.4
For components which failed during service, sample shall include the section closest to the
fracture area, and if possible the fracture area itself.
For heat treated components, sample shall include the entire section so that the effect of
furnace atmosphere on each surface can be evaluated.
For metal powder, sample shall be thoroughly mixed before examination to ensure uniform
particle size and shape distribution.

NOTE: Examination under the scanning electron microscope (SEM) is the most widely used
method for characterizing powder particles. Where the internal structure of particles is to be
characterized as well as their surface, conventional mounting, polishing and etching tech-
niques may be used if precautions are taken to prevent particle agglomeration.

3
SPECIMEN PREPARATION
Samples are levelled, ground and polished to produce a specimen with a flat, mirror-finish
surface. Surface preparation operations shall be performed in suchaway as not to cause
thermal or mechanical distortion of metallographic structure.

3.1
Grinding

3.1.1
Grinding is generally performed on automated equipment using abrasive paper discs (220

THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISNPUTE THE
grit silicon carbide) cooled with water.
For final grinding, 500 and 1000 grit abrasive silicon carbide papers are used.
Abrasive paper grit is indicative and is shown for information only.

ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

Specimen shall be thoroughly cleaned after grinding (e.g. through ultrasonic cleaning in ethyl
alcohol).

3.2
Polishing

Polishing is also performed on automated equipment using a rotary disc, with a cloth and a
CONFIDENTIAL

suspension containing 6 µm diamond powder.

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50210/01 Change

Clean specimen thoroughly after polishing (e.g. through ultrasonic cleaning in ethyl alcohol).

3.3
Vacuum impregnation
NOTE: The metallographic specimen obtained according to the procedure described above,
is impregnated under vacuum, generally with epoxy resin, in order to prevent damage to pore
shape and edges or pore clogging during polishing.

3.3.1
Wash metallographic specimen in ethyl alcohol and dry under vacuum for at least 15 minutes
to eliminate moisture trapped in pores.

3.3.2
Carry out vacuum impregnation.

3.4
Second grinding and polishing

3.4.1
After specimen impregnation, grind and polish again using abrasive paper (500 and 1000 grit
silicon carbide).

3.5
Final polishing

3.5.1
Final polishing is carried out using rotary discs and suspensions containing 6, 3 and 1 μm
diamond powder.
WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISPUTE THE ONLY
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

3.5.2
An alkaline suspension diluted in distilled water may be used for even finer polishing.
VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

3.5.3
Wash specimens thoroughly in water and ethyl alcohol after polishing and dry in hot air.
CONFIDENTIAL

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Fiat Group Automobiles Change 50210/01
4
POLISHED SURFACE ETCHING
Specimen surface is etched in order to reveal the various structural constituents of an alloy
so that they can be identified through microscopic examination.

4.1
Etching modality

Chemical etching is performed by dropping from a dropping bottle a reactive quantity

sufficient to cover the whole sample. As soon as the metallographer judges, on his own
experience basis, that the sample has reached the right tone, stop etching by means of a
spout of ethyl alcohol and followed by a warm air blow. Etching shall be light and uniform.

After etching specimens may be conserved for a short period in a desiccator.

Etchants shall be selected on the basis of the alloy concerned and the characteristics to be
revealed.

The following table shows the most commonly used chemical etchants. For particular
etchings, refer to metallographic atlas.

Name Composition General use prescriptions

NITAL 1 to 5 ml nitric acid, For carbon steels and cast irons.
100 ml ethanol (95%) or
methanol (95%)
PICRAL 10 g picric acid, For ferritic stainless steels and martensitic stain-
100 ml ethanol (95%) or less steels.
methanol (95%)
MARBLE'S 10 g copper sulphate, For austenitic stainless steels, cast irons with
REAGENT 50 ml hydrogen chloride, austenitic matrix (Ni-resist), iron-nichel and

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WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISNPUTE THE
50 ml distilled water colbalt-base superalloys.
VILELLA'S 5 ml hydrogen chloride, For martensitic stainless steels and ferritic stain-

ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

REAGENT 1 g picric acid, less steels.
100 ml ethanol (95%) or Caution! For preparation and storage use plas-
methanol (95%) tic bottles only (polyethylene).
0.5% hydrogen fluoride For aluminum alloys.
--- (48%) in distilled waterCaution! For preparation and storage use plas-
tic bottles only (polyethylene).
KELLER'S 2 ml hydrogen fluoride For aluminum and aluminum alloys.
CONFIDENTIAL

REAGENT (48%), Caution! For preparation and storage use plas-

3 ml hydrogen chloride, tic bottles only (polyethylene).
5 ml nitric acid,
190 ml distilled water

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