I.

Objetive
 Acquire knowledge about the metallographic sample preparation technique.
 Prepare metallographic specimens using the appropriate techniques and
procedures to study the micrographic structure of metals.
II. theoretical framework
Metallography
is the branch of metallurgy that micro
graphically evaluates the structure of
metals and their alloys, with the purpose
of identifying the present phases, their
percentage and morphology and relating
these characteristics with the chemical-
mechanical properties of the material.
What is necessary?
Graph 1: Metallography
The metallographic preparation of the area
to be tested is of vital importance for obtaining a good quality replica that allows
reliable metallographic analysis. And for this it is necessary to eliminate all types of
abrasive residues that come from slabs or polished precedents, as well as any type
of external contaminant.
Selection and cutting
The selection is directed to obtain a sample, faithful representative of the piece, that
is to say that it has the same physical discontinuities, the same constituents, in the
same concentration and equally distributed.
To ensure this condition, the following criteria should be taken into account:
 Extract samples from the extreme and middle parts of the piece.
➢ If the piece is complex extract samples of the thick and thin parts.
➢ Of the mechanically worked (deformed) pieces, samples of the cross-section and
longitudinal sections will be extracted.
➢ In the samples with thermal treatment, samples of the periphery and central part
will be obtained.
➢ To observe segregations, samples of different parts of a piece are extracted.
➢ In a failed part, samples will be taken in the area of rupture and in the area far
from the fault
➢ In the welds, samples will be taken that include welding and neighboring areas.
Cutting the sample with a saw or disk will produce:
➢ Distortion due to the drag of the saw; soft metals problem.
➢ Structural changes due to warming; difficulty presented in the hard alloys.

Therefore, any violent mechanical action should be avoided. It is also not

convenient to use oxy-acetylene cutting. For soft metals, light alloys and
unhardened steels, the hand saw will be used.
For fragile alloys (foundries and some bronzes) the sample can be extracted by
hammer blow. For hard materials (hardened steels and non-ferrous alloys hardened
by aging) abrasive discs with cooling will be used.
Abrasive cut
It consists in the separation or sectioning of a
material using discs with specific abrasives.
Types:
• Aluminum oxide discs.
• Silicon carbide discs.
Abrasive cutting techniques:
• Choose correctly the type of disc according
to the material to be cut. Graph 2: abrasive cut
• Firmly hold the piece to the cutting table.
• When advancing the disc towards the piece, it must be slow.
• Use adequate cutting speed to the disc.
• Use coolant, if the cut is with aluminum oxide disc.
• Clean the machine.
Mounting
The test pieces are assembled or embedded in
suitable materials, first for proper handling,
and secondly to preserve them during the
subsequent stages of preparation.
Among all assembly techniques, the most
widespread is assembly in synthetic plastics.
Samples that are not sensitive to high Graph 3: mounting
pressures and temperatures, compression
mounting is recommended; which consists of compressing a plastic powder and
melting it on the specimen and letting the whole unit cool down under compression,
until solidification. Thermosetting and thermoplastic resins are used for this
method.
For samples sensitive to heat and pressure, the cold assembly is used with a liquid
resin, an activator and a hardening catalyst.
Roughing
Procedure by means of which imperfections in the surface of a metal are
eliminated, using sandpaper of abrasive paper of different sizes of grains.
Types:
Thickness: Eliminates imperfection from the cut, uses mechanical equipment with
coarse-grained sandpaper normally of 80-120.
Fine: Eliminates streaks that originate in coarse roughing, successively passing the
material through a series of sandpaper with decreasing grain 240-320-400 and 600.
Equipment:
• Mechanical band scraper.
• Manual grinding machine.
 Grinding metal parts:
• Refrigerate properly.
• Hold the piece firmly.
• The piece must move, over the entire surface of the sandpaper.
• The pressure on the sandpaper is directly proportional to the material to be
removed.
• When changing from one sandpaper to another, the sample must be sanded 90º.
• The stripes obtained in each sandpaper are used increasingly.
• At the end of the last sandpaper, the surface must be free of scratches.
Polished
It is the final part of the preparation of a
metallographic specimen and aims to
leave a completely flat surface, free of
small scratches and with a mirror shine.
Types:
 Initial or thick (green)
 Intermediate (red)
 Finish (micro-cloth or velvet).
Polishing of metal parts:
Initial or thick: Graph 4: polished
 Firmly hold the specimen by
turning it in the opposite direction to the rotation of the disc, use Green
Billiard cloth and 1-micron alumina (μ).
Intermediate:
 Use red felt and 0.3-micron alumina cloth for the second disc.
Final polishing:
 Finally, polish using a fine hair cloth (micro-cloth) and 0.05-micron
alumina.
 When passing from one cloth to another wash the sample with abundant
water, to eliminate the remains of abrasives.
 Avoid touching the polished surface with your fingers or hands.
For this purpose, a mechanical rotary disc polisher with water dispenser is used.
III. Materials and equipment
 Corrugated construction iron
 Arch of closes
 Roughing equipment
 Table screw
 Emery paper No. 80
 Water shoe No. 240, 320, 400, 600
 Plastic mold
 Microscope
 Polishing machine
 Resin
  Activator
 Catalyst
 Alcohol
 Cotton
 Alumina
IV. Procedure
STAGE 1: SELECTION AND CUT
1) On a carbon steel rod (corrugated steel rod for construction) mark a sample so
that:
DIAMETER = 2 (HEIGHT)
2) Hold the piece firmly on the table screw, so that the section to be cut is
transverse.
3) Start the cut approaching, the saw arch, on the piece, with a slight inclination
towards the operator.
4) If it is possible to pour coolant (common water), continuously, over the piece and
the saw blade, in order to avoid overheating the sample.
5) Once the cut is finished, the specimen is removed from the screw and the
appearance of the surface to be prepared is noted.
STAGE 2: GROSS GROUND
CAUTION: When grinding in the bench grinder, as a means of safety, before the
equipment is turned on and during work, the operator must be placed on the side
of the equipment (parallel to the emery stone).
1) Start the equipment.
2) Press lightly the sample on the emery stone; in order to avoid excessive heating.
Make sure that the grinding face is completely resting on the emery stone.
3) As soon as you feel a slight heating of the specimen, refrigerate it with ordinary
water or with soapy water.
4) La probeta quedará desbastada cuando la superficie presente una sola cara
uniforme.
5) Después de terminar el desbaste, eliminar los ángulos o bordes cortantes de la
probeta, redondeándolos; para evitar que en etapas posteriores rompan las lijas o el
paño.
6) Observar con el microscopio la superficie obtenida y dibujar su aspecto en la hoja
de control.
STAGE 3: ASSEMBLY
1) The sample should be clean, free of scales and sharp corners.
2) Clean the plastic mold, for cold assembly, and coat it internally with take-off
solution or floor wax.
3) Place the sample in the center and with the rough face on the bottom of the mold.
4) In a graduated beaker pour the required amount (20 ml) of resin and its respective
activator, as well as catalyst (hardener) in the following proportion:
20 ml Polyester resin.
2 drops Activator (Cobalt Naphtanate).
4 drops Hardener (Peroxide).
5) Then shake with a wooden wand until a total opacity occurs; immediately pour
the mixture into the respective mold and leave it until it hardens completely (24 hr
approx.).
6) On the control sheet note the conditions and proportions used in the assembly.
STAGE 4: FINISHING FINE
In the fine roughing equipment:
1) Place the abrasive strips, water resistant, in descending order of fineness of grain:
240, 320, 400 and 600.
2) Open the knob that provides water and regulate the flow.
3) Place the sample, with the face to be prepared on the sandpaper, holding it
laterally with two fingers and pressing from above with a third finger; sanding is
started on sandpaper 240, giving it a reciprocating movement in a single direction
(moving it away and bringing it closer to the operator for about 1/2 min.); until
obtaining a flat and uniform face of fine parallel stripes.
4) Then the surface is washed, after having finished in sandpaper 240, with a jet of
water, rinsing it with alcohol, drying it and observing it with the microscope at
100x; Write down the assessment on the control sheet.
5) Next one goes to the next, finer abrasive paper; turning the sample 90o and then
repeating the roughing motion for a time equal to twice the previous sanding (1
minute); until forming a system of parallel lines finer and perpendicular to the
previous one. Then wash, dry and observe the sample with the microscope.
6) Repeat the same cycle of operations, each time you move to the next paper, until
completing the sequence 240, 320, 400 and 600; taking into account the following
indications:
➢ At all times cool with water.
➢ Wash the specimen and hands when going from one sandpaper to another.
➢ In each sandpaper, roughly double the time of the previous sandpaper.
➢ When moving from one sandpaper to another, rotate the sample 90o.
7) Record the observations in the respective control sheet.
STAGE 5 .- POLISHED THICK AND FINE.
Preparation of the abrasive
In the mechanical polishing with alumina, the preparation of the abrasive medium
for coarse and fine polishing is carried out in the same way; they only differ in the
size of the abrasive particles, being from 1 to 5 microns for coarse polishing and 0.3
to 0.05 microns for fine polishing. The preparation is done as follows:
a) When the alumina is in the form of paste.
50 ml Alumina
1 lt Distilled water
Severe mixing
b) When the alumina is in powder form.
30 gr Alumina
1 lt Distilled water
 Severe agitation
Procedure
1) Cover the disc of the polisher with a suitable cloth: Short hair for coarse
polishing (example: silk or canvas) and long hair for fine polishing (example: pool
cloth or suede).
2) Then deposit some prepared alumina in the center of the cloth and wait for it to
settle for about 30 seconds:
Coarse polishing: Alumina from 1 to 5 microns
Fine polishing: Alumina from 0.3 to 0.05 microns
3) Turn on the polishing equipment and increase the speed to:
400 RPM for steels and foundries.
300 RPM for non-ferrous (Cu, Al, etc.)

4) Press the specimen on the cloth (soft for soft metals and more or less strong for
hard metals). At first it moves radially from the center to the periphery and vice
versa, at the end of the polishing the specimen is slowly rotated about its axis
normal to the disc. If the amount of abrasive powder on the cloth is sufficient but
the cloth is dried, it is moistened with distilled water.
This coarse or fine polishing lasts 1 to 5 minutes, on average it can be polished for 3
minutes.
5) When finished polishing, wash the test tube and hands well with running water,
wipe it with a piece of cotton to remove the adhering abrasive and moisten it with
ethyl alcohol, then dry it with a hair dryer.
The polishing ends when the total elimination of scratches on the polished surface is
observed with the microscope. Do not touch the polished specimen without
attacking or attacking with foreign objects or with your fingers.
V. Graphics

Graph 5, 6, 7: cutting the metal, putting in the mold and sanding to level.
 Grafico 8, 9, 10, 11, 12:
roughing machine, then sanding
in water, polishing. Polishing
end

VI. Results
Tablas: fierro.


Fig 1 #240 Fig.2 #320 Fig.3 #400 Fig.4 #600

VII. Conclusion

In conclusion, for the preparation of the sample should follow the procedure of the
guides to the letter as any deviation affects and spoils the sample, do not touch the
metal with your fingers because it contaminates and at the time of seeing in the
microscope it will come out wrong.

VIII. Bibliography

Mensoza J. (29 de junio, 2017). “preparación de probetas”. Recuperada de:

https://es.slideshare.net/MendozaVenturaJesus/preparacin-de-probetas-
metalogrficas
NEURTEK. (18 de enero, 2016). “pasos para una preparación de muestras”.
Recuperada de: https://www.neurtek.com/es/academia/metalografia-
preparacion-de-muestras/cuales-son-los-pasos-a-tener-en-cuenta-en-una-
preparacion-de-muestras
Rincon del quimico. (9 de marzo, 2016). “preparación de una muestra
metalográfica”. Recuperada de:
https://elrincondelquimicoblog.wordpress.com/2016/03/09/preparacion-de-
una-muestra-metalografica-y-observacion-al-microscopio/
National University Jorge Basadre Grohmann School
of Metallurgy and Materials

 Topic: Preparation of Metallographic

Samples
 Student: Manuel Arturo Quispe Sosa
 Code: 2017-103011
 Course: Metallurgical engineering
 Teacher: ing. Javier Atencio
 School: ESME
 facultad: FAIN