BAHAN LABORATORIUM

metalografi

Objektif

Untuk mempelajari karakteristik struktural atau konstitusi logam atau paduan dalam kaitannya dengan nya
sifat fisik dan mekanik.

pengantar

Ada dua metode pemeriksaan metalografi:

I) Makroskopi
2) Mikroskop
Dalam Makroskopi pemeriksaan karakteristik struktural atau karakteristik kimia
dari logam atau paduan dilakukan dengan mata telanjang atau dengan bantuan mikroskop berdaya rendah atau
teropong, biasanya di bawah l0x.
Dalam pemeriksaan yang sama mikroskop dilakukan dengan spesimen logam siap, mempekerjakan
perbesaran dengan mikroskop optik dari 100x sampai setinggi 2000x.

persiapan spesimen

1. Grinding

Sepotong kecil dari spesimen dipotong oleh logam-pemotongan-saw. Setelah memotong operasi, Gerinda di
the edges of the specimen should be carefully removed by a fine file or coarse grinding paper.
The silicon carbide grinding papers are held flat in a unit containing water facility for
lubrication purpose. Each unit contains four grades of papers, starting with grade 400 (coarse)
and finishing with grade 1200 (fine). Grinding of the work piece is done by starting with the
coarse papers and then continuing with the fine papers. In each stage, grinding is done by
rubbing the specimen backwards and forwards on the grinding paper in one direction only,
until the surface is completely ground, that is, until only grinding marks due to this particular
paper can be seen to cover the whole surface.
The specimen is washed thoroughly to remove coarse silicon carbide particles before
proceeding to a finer paper.
The direction of grinding is changed from paper to paper, so that the removal of previous
grinding marks is easily observed. The extra time spent on each paper should be increased as
the finer papers are used. At the end of the grinding sequence, the specimen is washed
thoroughly and dried. Now, the specimen is ready for polishing.

2. Polishing

The polishing is done on rotating wheels covered by a special cloth. Alumina is employed as
polishing agent. The 1-micron size is commonly used, but the total polishing time shortened
by starting on the 7 or 3 micron grade.
The pad should be kept well supplied with lubricant. The specimen should be held firmly in
contact with the polishing wheel, but excessive pressure should be avoided. During polishing
the specimen should be rotated or moved around the wheel so as to give an even polish. The
specimen should be thoroughly cleaned and dried between each wheel.
MATERIALS LABORATORY

3. Etching

Before etching, it is essential to ensure that the polished surface is grease and smear free.
If the final polishing has involved the use of magnesia ( in the form of an aqueous paste of
fine magnesia) or alumina (in the form of an aqueous suspension of fine alumina), then
thorough washing followed by drying off with acetone or alcohol will give a suitable surface,
although it must not be fingered afterwards.

Etching is generally done by swabbing. Etching times will vary from specimen to
specimen, however, a good general, procedure is to observe the surface during etching, and to
remove the specimen when evidence of the grains first appears. Microscopical examination
will then reveal whether the degree of etching is sufficient. Further etching can then follow to
strengthen up the details as required.
After each etching, the specimen should be thoroughly washed in running water, followed
by drying off with acetone or alcohol.
* As a guide the following etchants are commonly used:
Alcoholic Ferric Chloride - copper alloys
Mixed Acids - aluminum alloys
Nital (ethyl alcohol+ 2% HN03) - iron and steel
Dilute HCI - zinc alloys

A. MICROSCOPICAL EXAMINATION

The microstructural study of a material can provide information regarding the morphology
and distribution of constituent phases as well as the nature and pattern of certain crystal
imperfections. Optical metallography is a basic tool of material scientists, since the equipment
is relatively inexpensive and the images can be obtained and interpreted easily. Distribution
and morphology of the phases can be studied and, if their properties are known, a quantitative
analysis of the micrographs provides some information about the bulk properties of the
specimen. A limited study of line and surface informations is also possible with the optical
microscope.
In order to obtain reproducible results, with good contrast in the image, the specimen
surface is polished and subsequently etched with appropriate reagents before microscopic
examination. In a polished specimen, the etching not only delineates grain boundaries, but
also allows the different phases to be distinguished by differences in brightness, shape, and
color of the grain. Differences in contrast may result from differences in light absorption
karakteristik dari fase. Hasil etsa dalam serangan preferensial atau mewarnai preferensial
permukaan. Serangan preferensial korosi elektrokimia; itu juga diketahui bahwa
bahan yang berbeda menimbulkan korosi pada tingkat yang berbeda. batas butir sering anodik untuk bulk
logam di bagian dalam gandum dan begitu juga terukir pergi istimewa dan digambarkan.
Pewarnaan diproduksi oleh deposisi produk etch solid pada permukaan spesimen. Ini adalah
dibentuk oleh reaksi kimia antara ETSA dan spesimen. Di bawah menguntungkan
kondisi penggunaan ETSA yang tepat memungkinkan identifikasi konstituen. Kegagalan
analisis tergantung banyak pada pemeriksaan metalografi.
BAHAN LABORATORIUM

Pemeriksaan struktur mikro dapat memberikan informasi kuantitatif tentang berikut

parameter:
1) Ukuran butir spesimen
2) The amount of interfacial area per unit volume
3) The dimensions of constituent phases
4) The amount and distribution of phases.

Magnifications up to 1000x can be obtained with a resolution of 2 µ. For grain size

measurements, the grains along a line, circle, or within a known area are counted. It would be
useful to obtain an average value of grain diameter from a microstructural section. In linear
intercept method, the grains intercepted by a theoretical line on the specimen surface are
counted (Fig. 1). The number of grain boundaries intersected per unit length of a test line (n L)
can be noted. The average grain size is indicated by the inverse of n L , corrected for the
magnification, M, of the micrograph. In general, then, the average grain diameter, d, is given
by
d= C/n L . M
where C is some constant greater than 1 ( Typically, a value of C=1.5 is adequate).

Fig.1 Linear intercept method for grain size determination

Experimental

Specimens are going to be polished and etched as explained above. With an unmounted
specimen, even if it is almost level, it is best to fix it on a glass or metal slide by means of a
piece of plasticine. The prepared surface is made level by means of a suitable levelling device.
The correct procedure is to start with low power examination in order to obtain an overall
picture, and then successively higher magnifications are used to resolve the fine details. In
focusing, the stage is gradually moved towards the objective and when the image appears,
focusing is completed with the fine adjustment.
It is almost good practice to examine specimens first in the polished condition, as certain
features, such as the presence of inclusions, cracks, porosity, and sometimes even the different
phases, are revealed. This is followed by an examination in the etched condition.
Do not examine one or two fields only. It should always be remembered that the structure
of a given specimen exists in three dimensions, whereas the prepared surface represents a
two-dimensional picture in the plane of the micro-section. This fact should be taken into
account in the interpretation of the geometry of any particular configuration.

Results
The investigation result of the optical microscopy is going to be recorded as follows:
1. Examine each specimen and sketch typical microstructure
2. Estimate the carbon content of the steels.
3. Calculate the average grain diameter of the micrograph, using linear intercept method.
MATERIALS LABORATORY

B. MACROSCOPIC EXAMINATION OF METALS

Objective
To examine the nature of inhomogenities and flow lines in a metal by unaided eye or with the
aid of a low-powered microscope or magnifying glass.

Introduction
Metallurgical data obtained by a chemical and metallographic analysis of a metal or an alloy
are usually not representative of the entire piece. These data represent the characteristics of
the metal only at the particular section of the piece. The general distribution and variation in
size of nonmetallic inclusions; the uniformity of structure; the location and extent of
segregation; the presence of fabricating defects, such as seams or hammer bursts; and residual
ingot defects, such as pipe can not be examined by microscopy.
The nature of inhomogenities in a metal, and the extent to which they exist therein, are best
determined by macroetching a representative piece and subsequently examining the
conditions thereby revealed with the unaided eye or with the aid of a low-powered
microscope or magnifying glass. Such an examination is referred to as a macroscopic, or
macro, examination. The magnification employed is usually not over 10x.

Macroetching sections may reveal conditions in the metal that are related to one or
more of the following heterogeneous circumstances:
1. Crystalline heterogeneity, the presence and extent of which depend upon the
manner of solidification and the crystalline growth of the metal or alloy.
2. Chemical heterogeneity, owing to impurities in the metal or alloy and to localized
segregation of certain chemical constituents. Such segregation may be intentional (the
pengenalan karbon ke permukaan baja selama proses kasus karburasi), atau
mungkin tidak disengaja dan tidak diinginkan, misalnya, pemisahan belerang atau
fosfor yang begitu sering ditemukan pada baja cor.
3. heterogenitas Teknik, yang timbul dari dingin-kerja atau proses yang memperkenalkan permanen
menekankan ke dalam logam. heterogenitas tersebut jarang terjadi pada logam cor, namun kehadirannya
sangat penting dalam logam cold-rolled, penempaan, dll

Percobaan

Tiga percobaan akan dilakukan:

1. Sulphur Percetakan:
Kotoran mungkin ada di produk baja. Sangat diharapkan bahwa jumlah mereka harus minimal dan
homogen didistribusikan dalam produk. Kotoran ini menurunkan mekanik
sifat-sifat baja, terutama kandungan sulfur dalam baja membuatnya rapuh.
Belerang mungkin ada kimia dalam baja di salah satu dari dua bentuk, baik sebagai sulfida mangan atau sebagai
besi sulfida. pencetakan sulfur mendeteksi dan secara permanen mencatat distribusi sulfur dalam
baja.
Permukaan bunga yang harus diuji untuk distribusi sulfur harus cukup halus
dan bebas dari benda asing seperti kotoran dan lemak. Grinding permukaan pada kertas, nomor
400-1200 dan mencuci menyeluruh berikutnya umumnya akan menghasilkan permukaan yang memuaskan
untuk tujuan.
BAHAN LABORATORIUM

kertas bromide fotografi direndam dalam larutan 2% asam sulfat untuk

sekitar 3 atau 4 menit. Makalah ini dihapus dari larutan asam dan dibiarkan mengalir
bebas dari kelebihan solusi. Sisi emulsi kertas kemudian ditempatkan dalam kontak langsung dengan
the prepared specimen surface and allowed to remain in contact under moderately applied
pressure for 1 or 2 min. Care must be taken that all entrapped air bubbles between the paper
and the specimen surface are eliminated.
The reaction of the sulphuric acid with the sulphide regions of the steel produces hydrogen
sulphide gas, which reacts with the silver bromide in the paper emulsion, forming a
characteristic brown to gray-black deposit of silver sulphide. These reactions may be
expressed as follows:

FeS + H2SO4 ~ FeS04 + H2S

or
MnS + H2SO4 ~ MnS04 + H2S
H2S + 2 AgBr ~ Ag2S + 2 HBr

When the reaction has proceeded for approximately the recommended length of time, the
photographic paper is removed from the surface of the specimen, rinsed in clear running
water, and then fixed permanently by placing it in a photographic fixing solution for about 15
min. When fixation is completed, the print is again washed in running water for
approximately 30 min. and subsequently dried in the usual manner.
The examination of properly prepared sulphur print will disclose quite clearly, because of the
presence of darkly colored areas of silver sulphide, the precise location of sulphur inclusions
on the prepared surface of the metal. A grouping or gathering of such silver sulphide areas
indicates the presence of sulphur segregation, whereas a random dispersion of the spots
denotes a more uniform, distribution of the sulphur inclusions.

2. Flow lines:

It is sometimes desirable to determine whether or not a finished piece has been forged, cut, or
cast into shape and to note, in the event that it was forged, the direction of metal flow. Flow
lines as revealed by macroetching in forgings are a natural consequence of applied mechanical
working. If the flow pattern shows highly selective etching characteristics, it is likely that the
material may be defective and may contain an excessive amount of inclusions and segregated
areas.
A macroetched forged-material shows a directional flow pattern consisting of streaks and
striations. The orientation of this pattern with respect to the plane of the prepared surface
indicates the direction of metal flow during deformation. The flow lines are made visible
because the elongated inclusions of impurities, such as oxides, sulphides and other elongated
heterogeneous areas are selectively attacked by the etching reagent.

3. Welded sections:

It is often desirable, and frequently necessary, to determine the soundness of a welded joint
and to observe macroscopically over a cross section of the weldment the various zones
wherein structural changes have occurred. This is accomplished by macroetching the prepared
surface with the usual hydrocWoric acid solution, or in some cases with a milder reagent such
as 2 or 3 % nital (ethyl alcohol + 2% HN03).
In ferritic welds, the specimen of interest is prepared in a manner described for metallographic
specimens and finally alternately polished and etched in saturated picral to remove disturbed
MATERIALS LABORATORY

metal. The prepared surface is then etched for 10 to 20 sec. in 5% nital, after which the
surface is thoroughly washed and lightly rubbed on a metallographic polishing cloth until the
columnar grains in the weld metal show distinctly. This procedure is repeated several times to
lessen the light reflectivity characteristics of the surface and to produce some relief of the
macrostructure. The specimen of interest is then etched by immersion for about 2 min. in
saturated picral, followed by thorough washing in cold running water and swabbing with a
tuft of cotton to remove the loosely adhering reaction products formed on the surface. The
specimen is finally rinsed in alcohol and dried in a stream of warm air.

Specimens

1. Sulphur printing: a piece of rail material

2. Flow lines: done without a specimen, shown on blackboard
3.Welded sections: finding the location of weld section of a welded-material

Procedure

1. Sulphur printing: follow the instructions in the introduction section.

2. Flow lines:
3. Welded section: follow the instructions in the introduction section (for grinding the
penggunaan spesimen nomor 240-400 kertas grinding gosok permukaan spesimen menggunakan
kapas seberkas oleh 9g FeCl 3 + 6 cm3 HCl + 100 solusi cm3 H2O sampai bagian las
muncul).

hasil

1. Menggambar skematis inklusi sulfur dalam bahan rel (Spesimen 1).

2. Apakah inklusi sulfur didistribusikan homegeneously atau sebagai titik terpisah di
bahan? Diskusikan efek mereka pada sifat mekanik material.

3 Apa yang menyebabkan garis aliran muncul. Apakah garis aliran eksis dalam bahan dicor?
Mengapa?
4. Apa garis aliran menunjukkan dalam hal sifat mekanik material?
5. Menggambar skematis dilas-bagian dari spesimen 3.
6. Apa yang Anda mengetahui dengan memeriksa dilas-bagian itu? Dapatkah Anda berbicara tentang las
kualitas, penampilan dan bahan dilas, dll? Dengan memeriksa bagian las, berhubungan ini
mengakibatkan sifat mekanik material.

Referensi

1. Kehl, GL, Prinsip-prinsip Praktek Laboratorium Metalografi, 3rd Ed., 1949.

2. Güleç, Ş., Malzeme Ders Notlan, Makina Fakültesi, SAYA Tu.
3. Imperial College of Science dan Teknologi, Departemen Metalurgi dan
Material Science, Tahun ke-2 Bahan Laboratorium Catatan untuk Teknik dan Aeronautical
Insinyur.
4. ASTM Standar dan Standar ASM (mereka ada di perpustakaan kami, silakan berkonsultasi
dengan pustakawan).