Production and Evaluation of Field Metallographic Replicas: Standard Practice For
Production and Evaluation of Field Metallographic Replicas: Standard Practice For
Production and Evaluation of Field Metallographic Replicas: Standard Practice For
INTRODUCTION
Replication is a nondestructive sampling procedure which records and preserves the topography of
a metallographic specimen as a negative relief on a plastic film. The microstructural replica can be
examined using a light microscope (LM) or scanning electron microscope (SEM) for subsequent
analysis. Specimens examined in the SEM are vacuum coated with vaporized carbon or a suitable
metal to provide contrast and conductivity. The convenience of the replication process makes it
suitable for obtaining microstructures from field locations for subsequent examination and analysis in
a laboratory. The proper preparation of the test surface and of the replica itself is of paramount
importance and must receive careful attention. Because of the diversity of metallographic equipment
available and the wide range of environments in which replication is conducted, the preparation of
replicas of high quality should be viewed as a skilled process for which there exists a variety of
techniques that achieve satisfactory results.
This practice presents some guidelines on the preparation of metallic surfaces and production of
replicas and guidelines on evaluation of replica quality. It does not attempt to limit the variations in
technique developed by skilled metallographers, each of which may produce acceptable replicas.
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NOTE 1—It is recommended that the purchaser of a field replication tester. A replica may also be made on the decarburized surface, if it serves
service specify that each replicator demonstrate proficiency by providing the purpose of the investigation.
field prepared replica metallography and direct LM and SEM comparison
to laboratory prepared samples of an identical material by grade and 6.4 Do not remove any precipitates, carbides, nonmetallic
service exposure. inclusions such as oxides and sulfides during the polishing or
etching operations.
5. Evaluation Methods
6.5 Etching procedures for surface metallographic examina-
5.1 A suitable replica should accurately reproduce all the tion should be performed in accordance with Practice E407.
microstructural features present on the surface that was repli-
6.6 The quality of the surface preparation should be con-
cated.
trolled by the use of a portable field microscope.
5.2 No visible loss of resolution is permitted over the
6.7 To prevent possible contamination of any components,
normal range of magnifications on the LM as shown in Figs.
the etched area should be prepared carefully and thoroughly
1-3.
washed after replication.
5.3 The resolution of the structural detail in the replica
should exceed 0.1 µm to permit SEM examination at high 7. Replication Technique
magnifications (up to 5000×). See Figs. 4-6.
7.1 In general, a replicated area of 12 by 18 mm (0.5 by 0.75
6. Metal Surface Preparation in.) is satisfactory.
6.1 If magnetic particle testing was previously used on the 7.2 A replica is produced by one of the two methods
work-piece, demagnetize the piece before beginning surface described below. All methods produce acceptable replicas.
preparation. 7.2.1 A replica may be produced by wetting one side of a
sheet of plastic film with a suitable solvent, such as acetone or
6.2 Surface preparation may be accomplished using manual,
methyl acetate, and applying the wetted side of the film to the
mechanical, or electrolytic polishing methods.
prepared metal surface.
NOTE 2—Electrolytic preparation always carries the risk of pitting, and 7.2.2 Alternatively, a replica may be produced by wetting
of enlarging existing voids such as creep cavities and porosity. the prepared metallic surface with a suitable solvent, such as
6.3 Prepare the surface to be replicated using the methods acetone or methyl acetate, and applying the strip of plastic film
suggested in Methods E3 modified for field use, as appropriate, (usually cellulose acetate) to the wet surface. The film is
in such a way as to obtain a surface free of deformation, pressed against the surface for several seconds to ensure
scratches, polishing defects, etch pits, and other artifacts which adherance.
may obscure the true microstructural features. 7.2.3 Apply a rubber-based replicating compound to the
NOTE 3—The presence of decarburization can be detected with a prepared metal surface. Cover with the material’s carrier paper,
portable hardness tester during the grinding steps. Further grinding to then use a roller to spread the compound into a uniformly thin
reach a surface free of decarburization can be monitored with the hardness layer under the paper.
FIG. 1 Example of Replica Microstructure at 100× LM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
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FIG. 2 Example of Replica Microstructure at 400× LM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
FIG. 3 Example of Replica Microstructure at 1000× LM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
7.3 The replica shall be prepared as soon as possible after to the slide before transferring the replica on the tape surface.
specimen preparation of the original surface is completed, to Using the rounded end of a glass rod to apply the replica on the
minimize transfer of post-preparation oxidation and contami- tape is usually beneficial in reducing air bubbles and ensuring
nation to the replicating film. a flat replica. Some metallographers prefer to coat the back side
7.4 After the film has dried, remove the replica and perma- of the replica with an opaque substance such as black paint or
nently mount on a rigid slide to facilitate analysis of the replica ink prior to applying tape to improve the contrast when the
and to protect it from damage during subsequent transport and replica is subsequently examined.
storage. The mounting may be accomplished using a double- 7.5 Place identification on the slide, and store it in a durable
sided adhesive tape, either applied to the back side of the dried slide container for safe, contamination-free transfer to the
replica film while it remains on the prepared surface or applied examination laboratory.
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FIG. 4 Example of Replica Microstructure at 1000× SEM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
FIG. 5 Example of Replica Microstructure at 2000× SEM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
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FIG. 6 Example of Replica Microstructure at 5000× SEM. Material: See Specification A335/A335M, Grade P22. Etchant: 2 % Nital
contrast in the replicated microstructure when examined in the replica. In addition, neither precipitates, such as primary and
LM and to prevent charging of the film when examined in the secondary carbides and carbonitrides, nor nonmetallic
SEM. Documentation of the structural features of interest inclusions, such as oxides and sulfides, shall be dislodged
should then be made at the appropriate magnifications with the during polishing or etching regardless of their size.
LM or SEM.
10. Documentation
9. Replica Surface
10.1 Photomicrographic documentation of microstructural
NOTE 4—Examples of replicated microstructures, (Specification A335/
A335M steel, Grade P22 shown, with 2 % Nital etch. This material features shall be obtainable over the normal range of magnifi-
exhibits a wide range of microstructures, not all of which are shown here.) cation: 50 to 1000X LM and 500 to 5000X SEM.
9.1 High quality replicas must meet the criteria listed in 10.2 Each replica be adequately identified. Minimum iden-
Section 5. tification should include the job or other identification number,
9.2 No folds or permanent deformation shall be allowed to the name, the presence and characteristics of any coating
develop in the replica film during processing. applied to either side of the replica, and the name of the
preparer.
9.3 Microstructural features should be clearly developed
over an area of at least 6 mm (0.25 in.) in diameter. 10.3 A statement shall be made on the conformance or
non-conformance of the replica to this practice.
9.4 Replicas taken at weldments should accurately record
the base metal, weld metal, and heat-affected-zone microstruc- 10.4 Replicas shall remain attached to their carrier slides,
ture along the fusion line for a distance of at least 13 mm (0.5 and shall be stored in dust-free biological slide cases, with
in.). proper indexing to permit retrieval where required for record.
9.5 All microstructural features shall be accurately rendered 11. Precision and Bias
and photographic documentation shall be obtainable over the
11.1 It is not possible to specify the precision or bias of this
range of magnifications normally used for replica evaluation:
practice because no quantitative results are produced.
50 to 1000X for LM and 500 to 5000X for SEM.
However, all quantitative results produced through the exami-
9.6 All grain boundaries, grain boundary precipitates, nation of replicas can be influenced by the replication process.
cracks and cavities should be easily identified.
9.7 Precipitates and inclusions contained in the material that 12. Keywords
are greater than 0.1 µm should be accurately recorded on the 12.1 replica; replication
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