GUIDELINE FOR MACRO and MICRO ETCHING METALLIC

MATERIALS - PROCESSES AND REAGENTS

1. Scope

This document is an in-house guideline for both MICRO and MACRO Etching metallic material
samples.

2. General
The surfaces to be etched should be smoothed by filing, machining, or grinding on
metallographic papers. With different alloys and tempers, the etching period will vary from a few
seconds to several minutes, and should be continued until the desired contrast is obtained. As a
protection from the fumes liberated during the etching process, this work should be done under a
hood. After etching, the specimens should be thoroughly rinsed and then dried with a blast of
warm air. Coating the surface with a thin clear lacquer will preserve the appearance.

3. Purpose

The AWS Structural Steel and Bridge Welding Codes, AWS D1.1 and D1.5, respectfully,
specifies that MacroEtching of weld samples is required for procedure and welder qualifications,
yet does not provide details on how to complete these tests. This guideline fills the void that
exists between the codes and practical applications of them with respect to "MacroEtching."

4. Procedure
4.1 Specimen Surfaces preparation

Care must be taken to prevent overheating the specimen during polishing. Excessive pressure
during polishing will form deep scratches and will increase the depth of disturbed metal on the
surface of the specimen.

4.1.1 Rough polishing

This operation can be performed by means of different type sand paper. For rough polishing, a
adhesive sand paper should be used as a covering for the rotating polishing wheels. During
rough polishing the specimen is moved in a clockwise direction around the polishing wheel to
insure equal metal removal from the entire surface by not allowing prolonged polishing in any
one direction.

4.1.2 Fine Polishing

Fine polishing is often done using a water coolant and silicon carbide abrasive paper mounted on
a rotating disc. The two-wheel unit in the laboratory can be equipped with rough polishing wheel
and a final polishing wheel. Wheel speed for final polishing has to be set at a second position
(about 1150 rpm). A small stream of water is directed at the center of the rotating wheel.

4.1.3 Final Polishing

Final polishing is very similar to that used for rough polishing. Aluminum oxide is the most
popular final polishing abrasive for ferrous and non-ferrous materials. It is also possible to use
chromium oxides for soft materials.

The abrasive particles used in final polishing are generally carried on a napped or short pile cloth
such as billiard cloth or "microcloth." Most polishing cloths can be obtained cut to size and
coated with an adhesive backing. The adhesive back eliminates the need for mechanical
clamping.

CAUTION!
Be sure that you supply the rotating wheel with continuous flowing water. This step is taken to
insure cool surface during polishing.

4.2 Etching of specimens

Temperature - 160 to 180 °F.

Polished metal specimens usually show no structural characteristics. Etching of the metal surface
is done to make visible the crystalline structure of the metal and to produce optical contrast
between the various constituents. Etching is done by exposing the cleaned and polished
specimen surface to suitable etching solution such as those described in Table 1. These etching
reagents are powerful, hazard and must be handled with care.

CAUTION!
Do not forget: etchants are composed of organic and inorganic acids, alkalis or other complex
substances.

If the specimen is not sufficiently etched after the first application the etching process may be
repeated.

If the specimen is overetched it must be repolished prior to re-etching. Immediately following

the etching the specimen should be washed in warm water to stop the etching, then immersed in
alcohol and finally dried in a blast of warm air. Rapid drying is important to prevent water spots.
Etching reveals structural characteristics by preferential etching. That means that some areas
such as grain boundaries are more highly stressed than other areas and are more subject to
chemical etching.

4.3 For Ferrous Metals

Etching solutions suitable for carbon and low alloy steels, together with directions for their use,
are suggested as follows.

CAUTION: Always pour the acid into the water. Nitric acid causes bad stains and severe burns.

The solution may be used at room temperature and applied to the surface to be etched with a
glass stirring rod. The specimens may also be placed in a boiling solution of the acid, but the
work should be done in a well-ventilated room. The etching process should be continued for a
sufficient period of time to reveal all lack of soundness that might exist at the cross-sectional
surfaces of the weld.

Table 1

Carbon and Low-Alloy Steel Etchants

ETCHANT COMPOSITION TIME CHARACTERISTICS REVEALED

Nital § 1-5% 5-30 minutes Macroscopic examination - Carburization
Nitric and decarburization, hardness
Acid penetration, cracks, segregation, weldd
§ 95%-99% examination.- Average ground or
Methanol polished surface.

Microscopic Examination - Develops

ferrite grain boundaries in low-carbon
steel; produces maximum contrast
between pearlite and a cementite or
ferrite network; develop grain boundaries
in 4% silicon steel; develops ferrite
boundaries in structures consisting of
martensite and ferrite; etches chromium-
bearing low-alloy steels resistant to
action of picral. Darkens pearlite.
Polished surface.
Picral § 4 gram 3 - 5 hours Carbon and Low-Alloy Steels.
Picric Acid
§ 100 ml Macroscopic examination - Carbon
Methanol Segregation
 Microscopic Examination - Reveal s
maximum detail in pearlite, untempered
and tempered martensite, and bainite;
reveals undissolved carbide particles in
martensite; differentiates ferrite,
martensite, and massive carbide by
coloration; differentiates bainite and fine
pearlite; reveals carbide particles in grain
boundaries of low-carbon steel and
wrought iron - Polished surface.
Iodine 15 to 60 Macroscopic Examination - works better
Tincture, minutes with steel is 180 to 200 °F. Slow but
USP available from Pharmacy
Iodine and § 1 part of 30 to 60 The solution should be used at room
Potassium powdered minutes temperature, and brushed on the surface
Iodide iodine to be etched until there is a clear
(solid definition or outline of the weld.
form),
§ 2 parts of
powdered
potassium
iodide,
§ 10 parts of
water, all
by weight.
Hydrochloric § 1 part HCL 15 to 60 Macroscopic Examination - Segregation,
Acid Hydrochlor minutes porosity, hardness penetration, cracks,
ic Acid inclusions, dendrites, flow lines, soft
(Muriatic spots, structures, weld examination. - Sa-
Acid) cut, machined or average ground surface.
§ 1 part Use at or near Boiling Point of Acid
Distilled Solution.
Water
Ammonium § 1 part of Applied by vigorously rubbing the
Persulfate ammonium surface to be etched with a piece of
persulfate cotton saturated with the solution. The
§ 9 parts of etching process should be continued until
water, by there is a clear definition of the structure
weight in the weld.

5. Acceptance

For acceptable qualification, the test specimen, when inspected visually, shall conform to the
following requirements:
Fillet Welds. Fillet welds shall have the following:
 1. No cracks
2. Thorough fusion between adjacent layers of weld metals and between weld metal and
base metal
3. Weld profiles conforming to intended detail, but with none of the variations prohibited in
AWS D1.5 3.6
4. No undercut exceeding 1 mm.
5. Fusion to the root of the joint but not necessarily beyond.
6. Leg sizes equal to or greater than the specified leg size.

6. Principal Etch Observations to be Recorded

Identification Description Location

to use on
Photograph
A Cracks
B Seams or Laps
C Decarburization
D Pinhole
E Segregations
a Pipe
b Porosity
c Bursts
d Segregations
 Flakes or Cooling Cracks
 Dendritic Pattern
 Ingot Pattern
 Grain Boundaries
Surface or Subsurface
Surface or Subsurface
Surface or Subsurface
Surface or Subsurface
Surface or Subsurface
Center or Central Area
Center or Central Area
Center or Central Area
Center or Central Area
General
General
General
General

7. Reporting Requirements

A digital photograph shall be taken of the macro/micro etched specimen for inclusion in any
report or PQR. Indications on the photograph shall be marked as listed above.