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G.S.G.K.

SBharadwaj
Reg.No.:14ETMM02

LabReport

Scanningelectronmicrocopy

Objective:Tomakemicrostructuralobservationsofsampleobservedunderscanning
electronmicroscope

Equipmenthandled:HitachiS3400N

Theory :Scanning electronmicroscopyisamicroscopictechniqueusedtoenhancelinear


magnification by using electron beam as source radiation. Apart from mere observation
SEM is also used to find chemical signature of sample using EDX (Energy dispersive
Xrayspectroscopy)technique..

ThoughresolutionofSEMisstilllimitedbyAbbes
equation , it is much narrowed down as compared to optical microscopy. Thus minute
features on surface can be observed using SEM. Important feature that sets SEM stand
alone inmicroscopy techniquesisitshighdepthoffield(withhighresolution).Thisfeature
is important to analyse fracture surfaces of specimen. Important features viz. mode of
fracture,epicenter offractureandalotofinformationcanbedecipheredfromfractographs.
Apart from above listed information it isalso possible to predict qualitativelythe depth of
socollected3Dsurfaces.

Principle : Scanning electron microscope produces images of samples due to


interactionsbetween electron beamandsamplesurface.Differentkindsofinformationcan
be extracted from SEM based on interaction signal generated due to sample surface
electronguninteractions.


Themainsignalswhicharegeneratedbytheinteractionof
the electron beam and the specimens bulk are secondary electrons (SE) and
backscattered electrons(BSE) and furthermoreX rays.They come from an interaction
volume in the specimen which differs in diameter according to different energies of the
electronbeam (typically between200 eV and30keV).TheSEcomefromasmalllayeron
the surface and yield the best resolution, which can be realized with a scanningelectron
microscope. The well known topographical contrast delivers micrographs which
resemble
on
conventional
light
optical
images.

The BSE come from deeper regions of the investigated material thus giving a lower
resolution. The typical compositional contrast gives materialspecific information since
the signal isbrighterforregionsofahighermiddleatomicnumberoftheinvestigatedarea.
As a byproduct of the image giving signals Xrays are produced. They result from
ionization processes of inner shells ofthe atom leading to electromagnetic radiation. The
characteristic Xrays giveinformation about the chemical compositionof thematerial.The
method energy dispersive Xray spectroscopy (EDS) as exemplified earlier enable
thedetectionofchemicalelementsfrominaqualitativeandevenquantitativemanner.They
differ in the energy resolution (the energy values are correlated to the line energy of a
specialchemicalelement)intheprocessingandintimeofmeasurement.

Prosandcons: Addedadvantagewithliesinfactthatnosamplepreparationisrequired
to pursue observations onSEM(formetallographic study).Samples(saymetalsamples)
can be observed as they are without any modifications as compared to conventional

optical microscopy i.e. sample need not be polished ,etched to reveal the features.
However a pointthat deserves mention isthat SEM isnotcompatiblewithnonconducting
samples. As it is the electron beam interaction that we are concerned with , a non
conducting sample could accumulate charge thereby blurring the vision. Above problem
canbecircumventedbyapplying a thincoatofconductingsampleoverthenonconducting
specimen.Acarbontapecanalsousedforthispurpose.

Observations : SEM micrographs are obtained from samples that are prepared for
metallographicobservationinopticalmicroscope.

FollowinginformationisextractedfromSEMmicrograph

1) Accelerationvoltageis15.0Kv
2) Magnificationatwhichimageiscapturedis2000x
3) SEMissetforsecondaryelectronimaging.


Above details extracted from micrograph image are of little use and of no interest.
Microstructuralinformation iswhat that isrequired.Followingmicrostructuralinformationis
inferredfromaboveSEMimage.

1) There are evidences of etch pits on sample surface, that are caused due to over
etchingofthesample.Theseareartefactsandnotdefects.
2) Therearealsosmallporesobservedinthebulkofgrain.

1) Magnificationis1000x.
2) Accelerationvoltageis15.0kv
3) Twin boundaries are seen in the micrograph. These aremechanical twinsthatare
characteristicofausteniticsteels.

1) Imaging mode is different in both micrographs. Micrograph (a) is imaged in BSE


modewhereasmicrograph(b)isimagedusingtransmittedelectrons.
2) Morphology of object under observation can bedeciphered from micrograph (a) (
oneontheleftside)
3) Center portion of micrograph (b) is dense relative to the edges as there is no
availablesignalfromthatportion.

1) This is high resolution ( scale bar reads 1 nm) image obtained perhaps through
TEM.
2) ThisimagereferstodiamondfilmgrownepitaxiallyonSiwafer.
3) Slightlatticemisfitisobservedasthereismisorientationinatomicpositions.

1)
2)
3)
4)

Epitaxiallydepositedlayeronotherisobserved.
(111)ismoreamenabletoplasticdeformationthan(200)planes.
Basedongivendatalatticeparameterisevaluatedtobe3.60angstormunits.
(111)planesareclosepackedascomparedto(200)planes.

1) Acylindricalfilmisgrownonasubstrate.
2) In micrograph (b) operated in STEM mode it can be observed that the film is
permeabletoelectronflowasopposedtometalsubstratewhichisopaque.
3) Accelerationvoltageis30kvinbothcases.
4) Fieldofviewissameinbothmicrographs.
5) Micrograph(a)isoperatedinsecondaryelectronimagingmode.
6) workingdistanceinbothcasesissame.

Conclusions:Metallographyisstudiedwithhelpofscanningelectronmicroscope
2) SEMisoperatedhandsonandimagesareobtained.
3) Aspectsrelatedtomicrostructuralanalysisarerealized.