There are a lot of reasons behind analyzing a metal surface ranging from
process control to identification of various phases present in the structure. This
descriptive science of the structures and properties of metal surfaces done at different
magnifications is called metallography. Metallography has two major aspects:
macroexamination and microexamination. Macroexamination
is done using a
magnification of 10x or less while microexamination requires a higher magnification
(Agrawal, 1988).
Aside from the difference in magnifications employed, macroexamination differs
from microexamination in that such examination grants an overall state of the specimen
compared to microexamination which imparts characteristics at a particular section of
the specimen only (Vander Voort, 1999). Thus, macroscopic examination is utilized in
routine quality control, in failure analysis and in research studies as a prelude to
microscopic examination. Since manufacturing processes have fixed implementation of
operations, quality control uses macroscopic examination as basis for acceptance or
rejection of produced goods. For research studies, macroexamination is used to reveal
variations caused by the different manufacturing processes implemented. Often times,
however, the manufacturing process of a specimen is unknown when conducting a
failure study, hence, macroexamination is used to judge quality, to locate problem areas
for further study and to determine how the specimen was produced (Agrawal, 1988).
Macroscopic examination can be done through destructive or non-destructive
testing. Non-destructive methods include liquid penetrant testing, eddy current testing,
radiographic testing and magnetic particle testing (Mechanical-student.blogpost.com,
2012). Macroetching, contact printing, fracturing and lead exudation are part of
destructive procedures (Vander Voort, 1999).
Macroetching is the widely used metallographic procedure since more
information can be derived from this simple method. Etchants are employed in such a
method to reveal macrostrutural characteristics such as variations in structure,
variations in chemical composition, and presence of discontinuities (Appendix A)
(Agrawal, 1988). Furthermore, it is used in the study of weld structure, definition of weld
penetration, dilution of filler metal by base base metals, entrapment of flux, porosity and
cracks in weld and heat affected zones (Appendix B) (Vander Voort, 1999).
Macroetching is a six-step process: surface preparation, cutting, grinding, polishing,
etching and interpretation of results (Standard Test Method for Macroetching Metals and
Alloys, 2000).
A sample specimen should be a representative of the whole that is usually
obtained through roughing cut then a finish cut. The smooth surface is achieved by
conventional methods of grinding and polishing. In cases where a fine detail is required,
a series of metallographic papers are utilized to ground the specimen. However, it
should be noted that the degree of surface roughness permitted depends largely on the
severity of the etchant that will be used and on the examination that will be conducted.
The next step is the most important step for this metallographic procedure:
macroetching. Appropriate etchant should be chosen for the specimen being observed
to attain desired results. Swab the surface with the etchant, and when etching is
completed, rinse the specimen and blow dry. It is crucial that overetching be avoided
since it can often lead to misinterpretation. The etching process will reveal the
macrostructures which is needed on the final step: interpretation of results. Depending
on what results are to be acquired, various extent of resolution and magnification are
available (Becker & Shipley, 2002). Qualitative examination gives the overall view of the
macrostructures and the distribution and orientation of the various phases, inclusions
and segregations present. Quantitative examination deals with length and width of
various microconstituents, proportion of the various phases present and grain size of
the microconstituents (Agrawal, 1988).
Another widely used metallographic procedure is sulfur printing which is a type of
contact printing technique. It is a chemical spot test employed to identify presence and
location of sulfide inclusions which is due to the low solubility of solid sulfur in iron. For
this method, a ground specimen will suffice although a pre-etched specimen does
produce improved results in terms of image intensity. The specimen is made in contact
for 1-5 minutes with a photographic bromide paper which has already been soaked in a
2% solution sulfuric acid. Caution should be abided since longer soaking times can
cause swelling of the gelatin surface of the film, which produces poor results. Upon
removal of the paper, distinct brown stains can be observed which indicates the location
of sulphides. The brown stains, silver sulphide, is the result of the reaction between the
silver bromide and H2S gas produced when the sulphuric acid reacted with the sulphide
region. Ultimately, the paper is placed in a fixing solution for 10 minutes, washed in
running water and dried (Vander Voort, 1999).
In conclusion, macroexamination is an important aspect in the study of metals
(Standard Test Method for Macroetching Metals and Alloys, 2000). It provides the
general state of the specimen which is exceedingly helpful in quality control, in research
studies and in failure analysis. It is both a practical and efficient way to observe the
variations on the structures, chemical composition and other defects (Agrawal, 1988).
REFERENCES
Agrawal, B. (1988). Introduction to Engineering Materials (pp. 318-321). New Delhi: Tata
McGraw-Hill Education.
Becker, W., & Shipley, R. (2002). Failure analysis and prevention. Materials Park, Ohio: ASM
International.
Mechanical-student.blogspot.com,. (2012). Mechanical Engineering - Free Online Course
Materials: Macro Structure of Metals. Retrieved 5 September 2015, from
http://mechanical-student.blogspot.com/2012/02/macro-structure-of-metals.html
Standard Test Method for Macroetching Metals and Alloys. (2000) (1st ed., pp. 1-2). West
Conshohocken. Retrieved from http://img.pathfinder.gr/clubs/files_3/81393/4.pdf
Vander Voort, G. (1999). Metallography, principles and practice. Materials Park, OH: ASM
International.
APPENDIX A
MACROSTRUCTURAL CHARACTERISTICS OBSERVED
THROUGH MACROETCHING
Figure A.1. Variations in structure: Flowlines (Vander Voort, 1999).
Figure A.2. Variations in structure: Dendrites (Vander Voort, 1999).
Figure A.3. Variations in structure: Cast grain structures (Vander Voort, 1999).
Figure A.4. Variations in structure: Columnar structures (Vander Voort, 1999).
Figure A.5. Variations in structure: Grain size (Vander Voort, 1999).
Figure A.6. Variations in chemical composition: Segregation (Vander Voort, 1999).
Figure A.7. Variations in chemical composition: Coring (Vander Voort, 1999).
Figure A.8. Variations in chemical composition: Banding (Vander Voort, 1999).
Figure A.9. Discontinuities: Burst (Vander Voort, 1999).
Figure A.10. Discontinuities: Laps (Vander Voort, 1999).
Figure A.11. Discontinuities: Cracks and Flakes (Vander Voort, 1999).
Figure A.12. Discontinuities: Decarburized surface (Vander Voort, 1999).
Figure A.13. Discontinuities: Carburized surface (Vander Voort, 1999).
APPENDIX B
WELDED STRUCTURES OBSERVED
THROUGH MACROETCHING
Figure B.1. Macroetching used to reveal the influence of weld parameters on
penetration depth and shape (Becker & Shipley, 2002).
Figure B.2. Macrostructures of a beryllium weldment (Becker & Shipley, 2002).
Figure B.3. Macrostructure of a titanium flash weld (Becker & Shipley, 2002).
Figure B.4. Pulsed GMAW spot weld showing a lack of fill-in (Becker & Shipley, 2002).
Figure B.5. Weld containing voids caused by incomplete fusion (Becker & Shipley,
2002).
Figure B.6. Incomplete penetration in a butt weld joint in steel (Becker & Shipley, 2002).
APPENDIX C
SULFUR PRINTING
Figure C.1. Sulfur print intensity is influenced by the composition of the sulphide
inlcusions. Both of the sulfur-printed discs contain 0.06% sulfur but the print on the left
is very light because most of the sulfides contain considerable chromium and are low in
manganese content. The sulfides in the disc at the right contain very little chromium.
