Struktur Mikro dan Persiapannya

Asep Ridwan Setiawan

 <0.2 nm 0.2-10 nm 1-1000 mm >1 mm
1 nm = 4x10-8 in
HRTEM, STEM Optical Naked Eye
Microscope
AFM
SEM,TEM,
XRD
Struktur Material
 Struktur Makro (>100 micron)
Struktur material yg bisa diamati dengan mata, seperti : porositas,
struktur lasan,pengecoran, forging (flow lines).
 Struktur Mikro (0.1-100 micron)
Struktur material yg hanya bisa diamati dengan mikroskop, seperti
: fasa, ukuran butir, cacat-cacat, presipitat
 Struktur Nano (1-100 nm)
Struktur material pada level atomik/sub atomik seperti : struktur
DNA, CNT, dsb
Definisi
 Struktur = berhubungan dengan
susunan dari komponen-komponen
dalam suatu material.
 Struktur Mikro = susunan
geometris dari butir-butir dan
beberapa fasa yang ada dalam suatu
material.
 Batas butir adalah antarmuka
(interface) antara 2 butir dalam
material polikristal dimana kristal
tersebut acak/tidak beraturan
karena perubahan drastis arah
kristalografik nya
Tujuan Materialografi
 The goal of materialographic preparation is to obtain the true
microstructure or “The True Structure,” meaning an
undisturbed material surface, which can be analyzed in an
optical light microscope or an SEM.
 The basic problem for a metallographer preparing a
specimen is that the preparation process itself modifies the
specimen surface and, theoretically, a “true structure”
completely without artifacts can never be obtained.
 Consequently, a preparation process should be used that
creates the smallest amount of artifacts, making it possible, in
practice, to analyze a microstructure in a satisfactory way.
Pemilihan metoda penyiapan sampel
 The preparation process will always influence the prepared
surface, creating artifacts.
 Artifacts are defined as false structural details introduced
during the preparation.
 Microcracks, comet tails, pitting, contamination, and lapping
tracks are all caused by the preparation process.
 The choice of preparation :
 Mechanical polishing
 Electrolytic polishing
 Chemical polishing
 Chemical-mechanical polishing.
Sampel / Spesimen Materialografi
 Ideal specimen size is 12–40 mm, square or cylindrical, with
a height of 12–30 mm.
 Exception : welds, where larger specimens have to be
prepared.
 The “sample” can be defined as the piece of material in its
“raw” state, as taken from the original material work piece.
As soon as the “sample” is treated prepared and described, it
turns into a “specimen” .
Sample Preparation Process
Sample Preparation Process
1. Sample selection
 Sample preparation= makan waktu, biaya dan perhatian lebih
karena material yg dianalisa biasanya tidak homogen.
 Faktor-faktor yg harus dipertimbangkan
 Jumlah : tergantung ukuran sampel, kerumitan, kondisi servis
 Lokasi : Lokasi kritis, dan lokasi yg blm terganggu
 Orientasi : tergantung dari proses pembuatan, bentuk dan fitur
yang mau diteliti
2. Sectioning
 To obtain a specimen, some kind of sectioning from the basic
material work piece is necessary.
 If this sectioning could take place without disturbing the specimen
surface, the specimen could be examined without further work.
 unfortunately all the known sectioning methods will leave some
kind of irregularities on the surface.
 Cutting must not significantly alter the bulk structure. Some
damage will usually occur at the cut surface, but the extent of the
damage can be minimized. The depth of the damage varies with
the technique used and the material being cut.
 Methods: shear, band saw, abrasive cutoff saw, and high- or low-
speed diamond saws
3. Mounting
Mounting is needed for a number of reasons:
 The specimen is small and is difficult to handle.
 The specimen has an awkward shape and mounting is necessary to
secure the preparation of the correct surface.
 Edge retention and flatness of the specimen is important for a correct
examination.
 The specimen is brittle or has cracks or pores, and the mounting
impregnation will stabilize the surface. Also the specimen could be a
powder material or in a shape not fit for preparation.
 A standard specimen size is required when using semiautomatic
or automatic preparation equipment. In general, most mounts
are round with diameters of 1, 1 ¼, or 1 ½ in. Mount height is usually
½ to ¼ in.
Dasar-dasar pemilihan mounting
material
 Dimension
 The material and technique employed must not damage the
specimen.
 Inherent resistance of the mounting material to the solvents
and etchants to be used.
 For microprobe, SEM examination, or electropolishing, a
conductive mount is desirable
Kriteria untuk mounting yg baik
 To obtain a good mount the following criteria should be
fulfilled:
1. No gap between specimen and mount material.
2. Rate of removal wear resistance of mounting material should
correspond to that of the specimen material.
3. No air bubbles in the mounting material or along the edge of
the specimen.
4. The mounting material should be resistant to common
etchants.
5. The mounting material should not pick up abrasive grains
during the preparation
3. Mounting
 Mounting methods : mechanical clamping, adhesive mounting, hot
compression, and cold castable mounting in a mounting plastic
resin.
 Hot compression mounting or hot mounting indicates that the
specimen is placed with an amount of resin in a cylinder in a
mounting press and heated under pressure for a specified period
of time. The resin polymerizes around the specimen, and after
cooling, a mount can be ejected from the press. (+ / -)
 Cold mounting typically takes place at room temperature but
often the temperature during the curing will reach 30–130°C
peak temperature. During cold mounting, the specimen is
normally placed in a mold mounting cup and a mixture of a resin
and a hardener is poured into the mold. After 5 min to 20 h the
plastic will cure, and a mount can be taken from the mold. (+ / -)
4. Grinding
 Grinding is done using rotating discs covered with silicon
carbide paper and water.
 There are a number of grades of paper, with 180, 240, 400, 1200,
grains of silicon carbide per square inch. 180 grade therefore
represents the coarsest particles and this is the grade to begin the
grinding operation. Always use light pressure applied at the centre of the
sample.
 Wash the sample in water and move to the next grade, orienting the
scratches from the previous grade normal to the rotation direction. This
makes it easy to see when the coarser scratches have all been
removed.
 After the final grinding operation on 1200 paper, wash the sample
in water followed by alcohol and dry it before moving to the
polishers.
 Plane Grinding = untuk meratakan sampel
 Fine grinding is the process used for establishing a specimen
surface suited for the first polishing step.
 Faktor yg hrs diperhatikan dalam grinding:
1. Material removal : rake angle, grain shape/contact point,
force, fluids
2. Deformasi : ulet atau getas.
 Grinding abrasives : aluminium oxide, silicon carbide,
diamond, boron nitride
Equipment
 Minitom: Small, automatic precision cut-off machine for
sectioning all materialographic and ceramic specimens.
 Metason: Ultrasonic Cleaning: For effective ultrasonic
cleaning of metallographic, ceramic, and mineralogical
specimens
 LaboPress-3 :Semi-automatic mounting press for hot
mounting of all materials.

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Equipment
 LaboPol (grinding and polishing machine):Machines for
grinding, lapping and polishing for 200 or 230 mm discs.
 LaboForce :Specimen movers for semi-automatic preparation of
materialographic specimens on LaboPol grinding and polishing
machines.
 LectroPol-5: :Automatic, microprocessor controlled electrolytic
polishing and etching of metallographic specimens
Bersambung…
Latihan
 Describe the steps involved in the preparation of a
metallographic sample:
 Sectioning (cutting)
 Plastic coating of the samples
 Mounting
 Grinding
 Why should the specimen be roughly washed after each stage
during either grinding or polishing?
 Why is fine grinding performed wet?