JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014 www.mejournal.

org
doi:10.14355/me.2014.0301.03

DeformationStructureInducedby
IndentationinGaAsandSiSingleCrystals
Y.B.Xu1,Z.C.Li2,Y.Q.Wu3
ShenyangNationalLaboratoryforMaterialsScience,InstituteofMetalResearch,ChineseAcademyofSciences,
Shenyang110016,China
2SchoolofMaterialsScienceandEngineering,CentralSouthUniversity,Changsha410083,China
3AmesLaboratory,IowaStateUniversity,Ames,IA50011,USA
1

ybxu@imr.ac.cn;2zhchli@csu.edu.cn;3yqwu@ameslab.gov

Abstract
Investigations conducted by the authors into the plasticity,
damage, phase transformation and fracture induced by
microindentationarecriticallyreviewed.Thematerialsused
in this study are Si and GaAs single crystals. The principal
findingsarethefollowing:(a)Microindentationmayinduce
a transition from crystalline to nanocrystalline and
amorphousstructure.Thereisacriticalstressforoccurrence
of the transition. The shear stress, rather than hydrostatic
stress is proposed to be attributed to this transition. (b) The
atomicscale structures ahead of the cracktip are extended
and successfully screened by a highresolution electron
microscope (HREM) using both plane view and
crosssectional view. It is found that the crack tip is not
atomically sharp, dislocations produced during indentation
lead to the crystal lattice distortion and even to a transition
fromcrystallinelatticetodisorderedstructureresultinginan
amorphousbandwithawidthof12nmaheadofthecrack
tip. The crack propagates along the amorphous band rather
thansequentialruptureofcohesivebonds.(c)Theresultsof
fast Fourier transformation and corresponding inversefast
Fourier transformation fringe images from different lattice
planes reveal that deformation around the cracktip is
anisotropic. The lattice fringes along ( 111 ) plane are not
changed and the atom arrangement on this plane is still
essentially ordered, and serious lattice distortion occurs on
the planes of (001) and ( 11 1 ). (d) Insitu observations by
HREM show that there is a critical current density for the
crystalline nucleation in amorphous area stimulated by an
electronbeam,andthecrystallinenucleationisnotrelatedto
theirradiationinducedtemperaturerise.
Keywords
Microindentation, HREM; Amorphization, Cracktip Structure,
Crystallization, Fast Fourier Transformation and Inversefast
FourierTransformation

Introduction
Mechanical damage, including deformation, phase
transformation,andmicrofractureinducedbycontact
stress in the semiconductor materials is an important

topic of both technological and fundamentalinterests.

The influence of the mechanical damage on the
properties of the semiconductors is crucial in the
design and fabrication of nanoscale microelectonic
and optoelectronic devices. In this case, micro and
nanoindentations have been widelyused as the most
common and the simplest technique both to assess
mechanical properties and induce mechanical
deformation damage. The entire brittle materials such
assiliconandgalliumarsenidehavebeenshowntobe
a various kinds mechanical damages including slip,
twin and phase transformation as well as cracking at
ambient temperature. The phase transformation
induced by indentation has been reported by using
transmission electron microscopy (TEM) and high
resolution electron microscope (HREM) in Si. In
contrast with Si, however, there is no evidence of the
phase transformation induced by indentation to be
observed in GaAs, where slip and twinning had been
suggestedtobeamajordeformationmode.
A number of studies of the entirely semiconductors
appear to be characteristic discontinuities on the
indentation loaddisplacement curves, which is called
popin. It is proposed that this kind of event is
caused by the generation of discrete dislocation loops
or the phase transformation under contact stress.
Although the mode of deformation induced by
indentationhasbeenextensivelyinvestigatedinSiand
Ge, but there has been little report on the
microstructure evolution induced during indentation
incompoundsemiconductors,especially,inGaAs.
In this article, we will give a review of the
microstructural aspects of the damage and fracture
generated under the contact loading at ambient
temperature, and even the electronbeaminduced
crystallization in amorphous semiconductor resulting
from researches carried out by the authors over the
past 20 years. The emphasis is placed on the direct

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www.mejournal.org JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014

of 0.049 N at ambient temperature. The sample was

oriented in such a way that the diagonals of the
indentation impression were aligned along <110>
directions in the (001) plane. A crosssectional sample
waspreparedinasandwichedway.Thespecimenwas
ionbeam thinned. In order to obtain electron
transparent sections in the whole indented region,
further lowangle ionbeam thinning of very short
duration(3~5min)wascarriedoutduringintervalsof
HREM observations, allowing the whole amorphized
region (from topside to bottom) near the interface to
beobservedclearlybyHREM(JEOL2000EXII,Japan).

observations, carried out by TEM and HREM, of the

microstructure evolution, including deformation,
phasetransformation, and in particular deformation
behavior ahead of the cracktip in silicon and gallium
arsenidesinglecrystals.
Materials and Experimental Procedures
The <110> oriented Si and GaAs single crystals were
selected for the studies. The Si has a diamondtype
lattice structure as shown in Fig. 1a, and GaAs has a
sphaleritetypelatticestructure,whichissimilartothe
diamond lattice structure as shown in Fig. 1b. The
difference between the Si lattice structure and the
GaAslatticestructureisfouratomslocatedatthe<1/4
1/4 1/4>. In the GaAs, these four atoms are Gaatoms
and the rest are Asatoms. Both of them are typical
brittlematerialsatambienttemperature.

For planeview samples, 3 mm diameter discs with

(110) orientation surface were ultrasonically cut,
mechanically ground and polished to a thickness of
about300m.Vickersindentationswereconductedon
the polished surface by using a Vickers
supermicroindenter (CHX1000, Shanghai) with
differentloads,0.0049N,0.049N,0.098Nand0.147N,
respectively, in air at ambient temperature. The
diagonalofindenterisselectedtoparalleltoacertain
direction as shown in Fig. 2. In order to increase
success rate for TEM observation of the indentations,
400 impresses were generally made in the surface for
planviewed samples. The indented specimens were
mechanically thinned to approximately 80 m and
dimpled to a thickness of about 20 m from the side
oppositeindentations.Thedimpledsidewasionbeam
thinned to perforation. Finally, a further 5 min
thinning was performed on both sides with ionbeam
thinning to remove the materials deposited on the
surface. The structures were characterized by TEM
(JEM2000FXII,Japan)andHREM(JEM2010,Japan).

FIG.2ILLUSTRATIONOFSPECIMENFORINDENTATIONTEST

FIG.3SCHEMATICDIAGRAMOFTHESANDWICHMETHOD
FORCROSSSECTIONALOBSERVATION

As discussed in the studied results, amorphous phase

can be induced in both Si and GaAs crystals under
indentation, the related electronbeam induced
crystallizationinGaAswithamorphousphaseinduced
by indentation was insitu investigated to study the
nucleationandgrowthprocessesbyusingaJEM2010
HREM operating at 200 kV. The current densities of
the electron beam were selected to be 93, 74 and 50
pA/cm2,respectively.
Results and Discussion
DeformationStructuresInducedbyIndentation
1)

Fig. 4a shows a planeviewed brightfield

observationofanindentationonthe(110)Sisurface.
A great deal of tangled dislocations distribute
around the periphery of the indentation. The
dislocationsarebendedintocontoursandendedin
thesameplaceasshowninadarkfieldinFig.4b.It
can be seen that the indented region is

FIG.1ILLUSTRATIONOFCRYSTALLINESTRUCTURESFOR
CRYSTALS,(a)Si,(b)GaAs

For the crosssectional view, sandwich method was

usedas shown in Fig. 3. A platelike specimen (about
0.5 mm thickness) of [001] singlecrystal silicon was
selected.Vickersindentationswereformedwithaload

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DeformationDislocations

JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014 www.mejournal.org

characterized by a devoid of crystallographic

contrast.Aselectedareaelectrondiffraction(SAED)
takenfromtheindentedregionconsistsofdiffused
rings (insert in Fig. 4a), indicating that a transition
from crystal lattice to amorphous structure occurs.
This kind of result is confirmed further by HREM
observationsthatwillbediscussedlater.

Fig. 6 shows a planeviewed TEM brightfield

micrographofanindentationproducedwithaload
of 0.049 N in GaAs single crystal at room
temperature. It is shown clearly that tangled
dislocation distribution around the vicinity of the
indentation is inhomogeneous, and appears to be
the fourfold symmetry of the rosette, consisting of
fourset long arms, and fourset short arm
dislocations. This observation is similar to the
earliestfindingbyWarrenetal.asshowninFig.7.
Meanwhile, Bourhis and Patriarche have studied
the nanoindentation structures achieved at room
temperatureon(001)GaAswitheithernorptype
doping,andfoundthatGaAswithndopedshows
partial dislocations in the form of both long and
shortrosettearmsasshowninFig.8.

FIG.4PLANEVIEWOBSERVATIONSOFANINDENTATIONON
(110)Si,(a)BRIGHTFIELDIMAGE,(b)DARKFIELDIMAGE
TAKENFROMTHEPERIPHERYOFTHEINDENTATION

Fig. 5 is a crosssectional brightfield image taken

from the edge of an indenter marked by A. It is
interesting to note that an amorphous region,
shaped as an inversed triangle, which is absent
fromthecrystallinelattice.Thiswillbediscussedin
detaillater.Undertheindentation,somegroupsof
dislocations, marked by B, C, D and E, can be
observed. It is reasonable to propose that the
dislocations belong to different kinds of
characteristics.Itisclearthatthedistributionofthe
dislocationsaroundtheindenterisinhomogeneous
and they have different natures. This is confirmed
furtherbytheobservationinGaAs.

FIG.7FOURFOLDSYMMETRYROSETTEPATTERNAROUND
{001}SURFACEINDENTATIONS,(a)INTRINSICGe,(b)GaAs

FIG.5CROSSSECTIONALTEMIMAGETAKENFROMA
REGIONNEARBYANINDENTATIONON(001)Si

Fig.9showstheschematicdiagramsofthepossible
slipgeometryina(110)GaAscrystallinethinfilm.
Itcanbeseenthattherearesixpossibleslipplanes.
Four of the slip planes, ( 1 1 ), ( 1 1 ), ( 1 1)
and (1 1 1), are shown in Fig. 9a, and other two,
( 1 1 1) and ( 1 1 1 ), are shown in Fig. 9b. The
analysis of dislocations which are shown in Fig. 6,
reveals that the short rosettearm dislocations are
parallel to the direction [ 1 12] or [1 1 2], and they

FIG.6DEFORMEDSTRUCTUREINDUCEDBYAN
INDENTATIONWITHALOADOF0.049N

FIG.8TEMPLANEVIEWOFANINDENTATIONINGaAs
UNDERVARIOUSCONTRASTCONDITIONS

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glideontheplanesof( 1 1 ),( 1 1 ),( 1 1)and

(1 1 1)in(110)GaAscrystallinethinfilm.

with the dislocation line directions of [ 112 ] and

[ 1 12 ], consisting of the short rosette arm
dislocations, are proposed to be the type
dislocations.
The characteristic of thedislocations shown in Fig.
11 were analyzed under different diffraction
conditions as shown in Fig. 12. By using a
diffraction condition of g=[ 1 1 1 ], only the
dislocations along [ 1 10 ] direction were detectable
as shown in Fig. 12a. When g is [ 004 ], only the
dislocations along [ 1 12 ] were visible (see in Fig.
12b).Fig.12cwasimagedusingg=[ 1 13 ],itcanbe
seen that only the dislocations along [ 1 12 ] were
visible and those along [110] were slightly
detectable. When g=[ 220 ], the dislocations were
not detectable besides those along [ 1 10 ] direction
as shown in Fig. 12d. According to gb=0, the
Burgersvectorscanbedeterminedtobeof1/2[110]
for shortrosette arm dislocations and 1/2[ 1 10 ] for
longrosette arm dislocations. The former is a
mixed type dislocation and the later is purescrew
one. The related results are listed in Table 1. The
distribution of dislocations induced by an
indentationinsiliconsingleismuchsimilartothat
inGaAs.

FIG.9SCHEMATICDIAGRAMOFTHEPOSSIBLESLIP
GEOMETRYIN(110)GaAsCRYSTALLINETHINFILM

Fig.10showsTEMobservationsoftwofieldsnear
an indentation, showing the longrosette arm
dislocations. It consists of the high dense
dislocationstructurenearthecenterofindentation.
The halfloop shape of the dislocations and long
and straight dislocations along [ 1 10 ] direction
glide on ( 1 1 1) or ( 1 1 1 ) plane as shown in Fig.
9b. This observation is similar to theearliest study
of Warren et al., who attributed to the different
nobilitiesofanddislocations,andwasverified
furtherbyBourhisandPatriarche.

FIG.11THREESETDISLOCATIONSTRUCTURETAKENFROMA
CORNEROFANINDENTATIONANDTHERELATEDSAED

FIG.10TEMIMAGESOFTHELONGROSETTEARM
DISLOCATIONSAROUNDANINDENTATION

Inordertodeterminetherosettedislocationnature,
thediffractioncontrastanalysishasbeenmadeinto
oneofthefieldsobservedatpresentstudy.Fig.11
shows a brightfield TEM image taken from one
corner of the indentation and the related SAED
pattern. It is found that these dislocations glide
alongthreesetsofdirectionsof[ 1 1 0],[ 1 1 2 ]and
[1 1 2 ], respectively, during indentation induced
deformation.Thedislocationswhichareparallelto
[1 1 0] direction glide along ( 1 11 ) or ( 1 1 1 ) plane.
They are referenced to be type dislocation. The
othertwosetsofdislocationslyingontheplanesof
( 11 1 . 1 1 1 .), ( 111 ) and ( 1 11 ), as shown in Fig. 9,

16

FIG.12DISLOCATIONANALYSISBYVARIOUSDIFFRACTION
CONDITIONS,(a)g=[ 1 1 1] ,(b)g=[ 004 ],(c)g=[ 1 13] ,(d)g=[ 220]

JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014 www.mejournal.org

TABLE1DIFFRACTIONCONTRACTANALYSISOFTHELONGANDSHORTROSETTEARMDISLOCATIONS

b(1/2)

visibleornot

Fig.No.

[110]

[1 1 0]

[101]

[10 1 ]

[011]

[01 1 ]

[1 1 0]

[1 1 2 ]

[ 1 1 2 ]

12a

[1 1 1 ]

visible

missing

missing

12b

[004]

missing

visible

missing

12c

[1 1 3 ]

missing

visible

missing

12d

[2 2 0]

visible

missing

missing

TABLE2CONTRASTANALYSISOFSTACKINGFAULTSASSHOWNINFIG.14

b(1/2)

Figure
number

14a

11 1

[110]

[ 1 10]

[101]

[ 10 1]

1/3

Visibleornot

[011]

[ 01 1]

Ld*

Trl**

SFF***

2/3

1/3

visible

visible

visible

14b

111

2/3

1/3

1/3

2/3

missing

missing

visible

14c

220

2/3

1/3

1/3

1/3

2/3

1/3

visible

missing

missing

14d

113

1/3

2/3

1/3

missing

visible

missing

*Leadingdislocations,**Trailingdislocations,***Stackfaultfringes

2)

StackingFaults

As shown in Fig. 13, twokind of morphologies of

the stacking faults had been observed in GaAs
inducedbyindentationwithalargeloadof0.147N.
Fig. 13a is a planeviewed TEM brightfield image
of one kind of stacking fault. It is seen clearly that
the trace of the stacking fault is parallel to [ 220 ]
and theyarein( 1 1 1 ) or ( 1 11 ) planes.Diffraction
contrastanalysisofthepartialdislocationsbyusing
differentdiffractionconditionsareshowninFig.14
and the results are listed in Table 2. When the
g=[ 11 1 ]isusedtoimaging,thestackingfaultsand
partial dislocations at both ends of the stacking
faults were visible (Fig. 14a). The stacking fault
fringes were visible, and the partial dislocations at
the end of the stacking faults disappeared when
g=[ 111 ] was used to image (Fig. 14b). However,
wheng=[ 220 ]and[ 113 ]wereusedtoimage(Figs.
14candd),onlyleading(Fig.14c)andtrailing(Fig.
14d)dislocationsarevisiblerespectively.Therefore,
the Burgers vectors of the partial dislocations can
be determine to be 1/6[ 1 12 ] and 1/6[ 12 1 ],
respectively.

Fig. 13b shows another type of stacking faults

occurred in GaAs crystal during indentation.
Contrast analysis shows that this kind of stacking
faults are composed of the partial dislocations
which are parallel to each other and have the
Burgersvectorsof1/6[ 1 12 ].

FIG.13STACKINGFAULTSOBSERVEDNEARAN
INDENTATIONINDUCEDWITHALOADOF0.147NINGaAs

FIG.14CONTRASTANALYSISOFASERIESOFPARTIAL
DISLOCATIONSINSTACKINGFAULTS,(a)g=[ 11 1] ,(b)g=[ 111 ],
(c)g=[ 220 ],and(d)g=[ 113 ]

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3)

Many of those studies focused on the phase

transformation in Si and Ge, but there has been
little report on the pressure induced phase
transitioninGaAs.

DeformationTwins

In addition to the dislocations and stacking faults

formed during indentation, and twinning is also
one of the important modes of deformation. As
shown in Fig. 6, twofoldsymmetry deformation
bandsdistributearoundtheindentation.AnSAED
as shown in Fig. 15a were taken from the region
markedbyacircleinFig.6.Thetypicaldiffraction
spotsreflectingtwinningcanbeseenobviously,the
diffractionspotslocateatthepositionsof1/3{111}
of that from the GaAs crystal. The analysis shows
thatthetwinningplaneis{111}anditsdirectionis
<112>. These indicate that the twofoldsymmetry
deformation bands have a typical twining
characteristic. The twins distributing around the
indentation looks like a rhomboid as shown
schematicallyinFig.15b.

Fig.17showsaTEMinvestigationofanindentation
inducedwithaloadof0.0049NinGaAs.Fig.17ais
aTEMbrightfieldimageofanindentationregion.
Different diffraction contrasts, which can be
reducedtogreyandbrightcontrasts,canbeseenin
the indentation region. The related contrast
distribution in the indentation region is illustrated
intheschematicdiagraminFig.17b.SAEDstaken
fromtheareasasindicatedbyAandCinFig.17b
areshowninFig.17candFig.17d,respectively.Itis
found that the 4 zones along diagonals as marked
by A in Fig. 17b have the similar contrast that
changes while tilting the sample in TEM. The
electron diffraction from these areas reveals
polycrystalline characteristic with diffraction
speckles as shown in Fig. 17c, implying that a
transition from single crystal to polycrystal or
microcrystal has occurred during indenting. A
further detail can be obtained from the HREM
observation as displayed in Fig. 18, where many
nanograins (marked by n) with a size of about 10
nm can be observed. These nanograins, among
which is amorphous structure, have different
crystalline orientations. However, the SAED taken
fromotherareasasmarkedbyBandCinFig.17b
are slightly elongated speckles, indicating that
these zones are deformed slightly although they
still keep single crystalline nature. Fig. 19 shows a
HREM image taken from the indentation center,
many dislocations (marked by D) and stacking
faults(denotedbySF)canbedetected.

FIG.15SAEDANALYSISOFTWINSAROUNDTHE
INDENTATION,(a)SAEDPATTERNTAKENFROMTHEAREA
MARKEDBYACYCLEINFIG.6,(b)SCHEMATICDIAGRAMFOR
THETWINDISTRIBUTIONAROUNDINDENTATION

Fig. 16a presents a typical HREM image of the

twins. It can be found that each piece of twins is
consisted ofmultimicrotwins, and the twin plane
is a stacking fault plane. This is seen more clearly
from Fig. 16b, where two stacking faults in the
original location of the twins are shown. This
implies that the formation of the twin is related to
theproductionofstackingfaultclosely.

FIG.16HREMIMAGESOFTWINS(a),ANDTWINING
INITIATIONREGION(b)

IndentationinducedPhaseTransition
1)

FIG.17PLANEVIEWEDTEMINVESTIGATIONOFAN
INDENTATIONINDUCEDWITH0.0049N,(a)BRIGHTFIELD
IMAGEOFTHEINDENTATION,(b)SCHEMATICDIAGRAMOF
THECONTRASTDISTRIBUTIONINTHEINDENTATION
REGION,(c)SAEDTAKENFROMTHEAREASASMARKEDBYA
IN(b),(d)SAEDTAKENFROMTHEAREASASMARKEDBYCIN
(b)

SingleCrystaltoPolycrystalTransition

A great number of investigations have been made

sincethefirstobservationofhighpressureinduced
phase transition by Minomura and Drickamer.

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amorphous structure occurred under the

indentation. This is a surprising finding and is, to
the authors knowledge, the first observation of a
crystalline lattice to amorphous transition in GaAs
singlecrystalunderindentation.Itisalsonoted,as
shown in Fig. 21, that there are many
disordered/amorphous clusters (marked by *) with
12 nm in size, and nanograins (denoted by nano)
with different orientations and dislocations (by D)
distributing along the interface between the
amorphous and crystalline lattice zones. It is
reasonable to propose that the crystalline to
amorphoustransitionmaygothroughacrystalline
lattice deformation and distortion, rather than
latticeabruptcollapse.

FIG.18HREMIMAGETAKENFROMAREGIONINTHE
INDENTATIONASINDICATEDBYAINFIG.17B

FIG.19HREMIMAGETAKENFROMINDENTATIONCENTER,
SHOWINGDISLOCATIONSMARKEDBYDANDSTACKING
FAULTSDENOTEDBYSF

2)

IndenterinducedAmorphization

FIG.21HREMIMAGEOFTHEINTERFACEREGIONBETWEEN
CRYSTALLINEANDAMORPHOUSPARTSINA0.049NLOAD
INDUCEDINDENTATION

Itissurprisingtonotethatdeformationbehaviorin
silicon induced by indentation is much similar to
those in GaAs single crystal. Fig. 22 is a typical
TEM observation of an indenter made on (110)
silicon single crystal. As the same that seen in Fig.
20, the diffusion diffraction rings taken from the
center of the indenter, shown inserted in Fig. 22,
indicate that the amorphization took place as that
inGaAs.ThiscanalsobefurtherverifiedbyHREM
observationasshowninFig.23,wheretworegions
theamorphousregionatthelowerpartaremarked
by aSi and the crystalline one at upper part is
markedbycSi.

FIG.20BRIGHTFIELDTEMIMAGETAKENFROMAN
INDENTATIONINDUCEDWITHALOADOF0.049N,THE
INSERTISASAEDFROMTHEINDENTATIONCENTER

It is interesting to find that a transition from

crystalline lattice to amorphous structure occurred
during indentation with the load of 0.049 N in
GaAs. Fig. 20 shows a planeviewed brightfield
TEM image and related SAED (see insert) of an
indentation. The SAED consists of two diffusion
rings. The SAED analysis reveals that the rings in
the SAED are from the (111) and (220) or (113)
crystalline planes and belong to the one from
amorphous GaAs. This is confirmed further by
HREM observation as shown in Fig. 21, where a
completely disordered lattice area marked by
amorphouszonecanbeseenobviously,indicating
that a transition from crystalline lattice to

FIG.22PLANEVIEWTEMIMAGEOFANINDENTEDREGION
ON(110)SiSURFACE,ANDTHEINSERTSAEDISTAKENFROM
THEINDENTATIONCENTER

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FIG.24MICROSTRUCTURESOFANINDENTATIONSUBJECTED
ANNEALINGAT500C/60MINOBSERVEDBY,(a)TEM,(b)
HREM

FIG.23HREMIMAGETAKENFROMANINDENTATION
CENTERINSiSINGLECRYSTAL,SHOWINGTHE
PHASETRANSFORMATIONTAKENPLACEFROM
CRYSTALLINELATTICETOAMORPHOUSSTRUCTURE

ElectronbeaminducedCrystallization
1)

In contrast with the crystalline region, the

disorderedlatticeandamorphousregionisastrong
evidence for the occurrence of the transition from
crystalline to amorphous in silicon. From uneven
interface between the two regions of c/a Si, and a
great deal of defects such as microtwins, clusters
with lattice disorder marked by the arrows,
indicating again that this kind of transition goes
through middle severe lattice deformation stage,
ratherthancrystallinelatticesuddencollapse.

InsituObservation

Theseveralmechanismsforelectronbeaminduced
crystallization have been proposed by some
researchers and are involved: elastic collision
driven
recrystallization,
plasticinteraction
promoted defect motion and electron beam
induced induced recrystallization. Jeni et al have
considered that crystallization is a plastic or
ionizationprocesswhichisacutandrecombination
oftheatomicbonds.Narayanhasproposedthatthe
mattermigrationoccurredatinterfacebetweenthe
crystalline and amorphous as the crystallization.
However, there have been fewer insitu
observations of the nucleation and growth of
recrystallization induced by electronbeam,
especially,inamorphousGaAs.

In order to verify the amorphous matter

underneath the indenter produced by the
indentation rather then by TEM specimen
preparation process, A GaAs thin foil with
indentationsinducedwiththeloadof0.049Nwas
annealed at 500C for 60 min, and then TEM film
was prepared. The observations are shown in Fig.
24. It is found that microcrystalline grains appear
insidetheindentationintheannealedsample.The
SAED (see insert in Fig. 24a) taken from the
indenter shows polycrystalline rings with some
diffraction spots instead of amorphous ones,
implyingthatrecrystallizationtookplaceinsidethe
indentation where amorphous characteristic were
observedasshowninFigs.20and21.HREMimage
(see Fig. 24b) taken from the indenter in Fig. 24a
demonstrates that there are many nanograins in
theindentedregion.

Fig. 25 shows TEM images and corresponding

SAED taken from the same fields (marked by a
arrow) before (Fig. 25a) and after (Fig. 25b)
electronbeam irradiation. It can be seen that the
diffusion rings before electronbeam irradiation
(Fig.25a)becomestypicalpolycrystallineringswith
diffraction spots (Fig. 25b), implying that
recrystallization occurred in this field after
electronbeam irradiation. This can be also
confirmed by the changes of the diffraction
contrast.

FIG.25TEMOBSERVATIONSOFELECTRONBEAMINDUCED
STRUCTURECHANGEOFANAMORPHOUSREGIONSUBJECTED
TOANIRRADIATIONWITHCURRENTDENSITYOF73pA/cm2,(a)
BEFOREIRRADIATION,(b)AFTERIRRADIATION

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Fig.26showsaseriesofinsituHREMobservations
of the electronbeamirradiation crystallization in
an amorphous GaAs induced by indentation. The
same region was investigated after various
electronbeamirradiation time. Fig. 26a shows an
amorphousregioninducedbyindentationinGaAs
single crystal, showing a typical amorphous
structure. Fig. 26b shows a HREM image of the
samefieldasshowninFig.26aafterirradiationfor
10 min. One can see that there are several clusters
(marked by arrows) with atomic scale appeared.
After irradiation for 30 min, these clusters become
the nanograins with a certain crystallographic
orientation as shown in Fig. 26c. As the increasing
irradiation time, nanograins with random
orientationsincreaseasshowninFigs.26d,26eand
26f. When irradiation for 120 min (see in Fig. 26e),
this region appears many nanograins. And after
180 min irradiation, the whole area becomes
crystallinezoneasshowninFig.26f.

FIG.26INSITUHREMOBSERVATIONSOFTHE
CRYSTALLIZATIONOFAMORPHOUSGAASWITHDIFFERENT
IRRADIATIONTIME,(a)0MIN,(b)10MIN,(c)30MIN,(d)60MIN,
(e)120MIN,(f)180MIN

2)

CrystallizationMechanism

Itisbelievedthattheelectronbeamirradiationcan
result in the temperature rise of the samples.
According to the calculated temperature rise for
Fe78Si12B10 of 557C induced by electronbeam
irradiation, Fisher and Liu et al. proposed that the
crystallization
induced
by
electronbeam
irradiationistheresultofthetemperaturerise.
The temperature rise at the center of the specimen
induced during electronbeam irradiation is
expressedby
I
E
b
(
)(+2 ) (1)
T=
4 ke d
a
where, e is electron charge, is a Euler constant
(0.5772),aisGaussianwidthofthebeam(effective
diameter of the beam), b is the radius (equal to
diameterofthespecimen),kisthermalconductivity
coefficient (is 44 Wm1K1 for GaAs), I is the beam
current rate, and E is the loss of energy of an
electroncrossingthedistancedinthespecimen.

The Eq. (1) is modified as following when the

specimenhasaholeatthecenter:
Thole=

I
E
b
(
)ln (2)
ke d
r0

where,r0 iseffectivediameterofthecurrentbeam.
If the loss in energy is small relative to initial
energy, E/d becomes dE/dx (stopping power).
Therefore,itisfound:

dE r e 4
mc 2 2
=
[ln
+F()] (3)
dx m 2 c 2
I 2

where,
F()=

1
2
1 2
+
[
(2 +1)ln2] (4)
2
2( 1) 2 8

21

www.mejournal.org JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014

here, e is electron charge, n is the density of the

targetmaterial,mistheelectronmass,cisthelight
speed, =v/c, v the electron speed, is the radio of
theelectronenergytodynamicenergy(E/mc2).The
temperatureriseinGaAsinducedbyelectronbeam
irradiationat300keVis7.0CbyusingEqs.(3)and
(4).

crystallization can still occurred when both Si and

GaAswereirradiatedbyelectronbeamunder30K.
Alltheseindicatethattheirradiationcrystallization
isindependentoftemperaturerise.Meanwhile,the
present study shows that the electronbeam
irradiation could not induce crystallization of
amorphousGaAsevenforalongtime,e.g.120min,
until the beam current is larger than 50 pA/cm2.
This implies that there is a critical electronbeam
current to be required for occurrence of the
crystallization
induced
by
electronbeam
irradiation.

According to Eqs. (1) and (2), the temperature rise

in GaAs during irradiation with acceleration
voltageof200keVandthebeamcurrentdensityof
94pA/cm2wascalculatedtobeabout10.8C.While
the parameters were selected as following: the
radius b (equal to diameter of the specimen) is 1.5
mm,thewidthofthespecimendis20nm.Table3
liststhetemperatureriseofsomematerialsinduced
duringelectronbeamirradiationcollectedfromthe
references. It can be found that the temperature
rises of all materials listed in Table 3 are much
lower for them to reach their recrystallization
temperatures.Althoughthecalculatedtemperature
rises of the GaAs at 200 keV are different between
the present work and that by Jeni et al. for the
different effective diameters r0 of the current beam
and the beam current rates, both of which are not
large enough for obtaining the recrystallization
temperature of GaAs (300C). Therefore, it is
reasonable to propose that the crystallization in
GaAs induced during irradiation is related to the
electronbeam current density, rather than the rise
intemperature.

Ontheotherhand,thereareanumberofmodelsto
describe the interracial growth of crystallization
Jeni et al reported that crystallization occurs at
electronbeam energy of 50 keV (acceleration
voltageof50kV)inSi,Ge,GaPandGaAs,andthe
higher the electronbeam energy is, the lower the
growthrateofcrystallizationis.
Jeni et al also found that the growth rate of
crystallization is the lowest when the electron
energy is near the threshold value for atom
displacement. Therefore, inelastic energy loss
mechanismisresponsibleforthecrystallizationand
growthunderlowelectronbeamirradiation(<100
keV). However, when the electronbeam energy is
high, for example, higher than 100 keV, the elastic
energy is proposed to promote the motion and
rearrangement of the atoms or defects at the
interface between the amorphous and crystalline
(a/c) regions, implying that the elastic energy, on
onehand,mayinduceproductionofthedefectsin
crystalline materials, on the other hand, can make
thecrystallinegrowthatthea/cinterface.

On the other hand, Meldrum found that the

crystallization occurred when both the phosphate
glassandamorphousfluorapatiteinliquidnitrogen
were irradiated. Jeni et al also found that

TABLE3THEPARAMETERSOFTHETEMPERATURERISEFORVARIOUSMATERIALSINDUCEDDURINGELECTRONIRRADIATION

Electron
Energy(keV)

Temperaturerise(C)
Si

Ge

GaP

GaAs

GaAs

LaPO4

Zircon

ScPO4

50

0.2

0.6

0.4

0.9

7.1

6.6

100

0.5

1.8

1.3

2.7

11.9

10.9

150

0.8

2.6

1.9

3.8

19.1

17..4

200

0.3

0.9

0.7

1.4

10.8

41.1

19.0

40.0

250

0.4

1.3

0.9

1.9

300

1.4

4.8

3.5

7.00

Note:fromrefs.30and31;fromref.37;fromthiswork

22

JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014 www.mejournal.org

The present insitu HREM observation shows that

the crystallization of the amorphous GaAs is
relatedcloselytotheelectronbeamcurrentdensity.
The larger the electronbeam current results in the
larger the energy (E) obtained in an irradiated
zone in per area per time. When the energy (E)
reaches a critical value, it may excite the fracture
andrearrangementoftheatomicbonds,leadingto
nucleation and growth of the crystalline. On the
otherhand,whenthebeamcurrentdensityislower
than50pA/cm2inpresentwork,theenergycarried
by electrons is not large enough to make the
rearrangementoftheatomicbondintheirradiated
zone. However, the larger beamcurrent density,
for example, 74 pA/cm2, can obviously make the
occurrenceofcrystallization,andastheincreasein
the beamcurrent density (93 pA/cm2), the rate for
nucleationandgrowthofcrystallizationincreasein
theamorphousGaAs.

haveintrinsiclimitationinitscapacitytodealwiththe
structuralchangethatoccursintheblackboxatthe
atomic scale. Hockey and Lawn have investigated the
fracturebehaviorofthebrittlematerialsSi,GeandSiC.
Theysuggestedthatthecracktipsareatomicallysharp
and there is no evidence for dislocation activity or
plasticity associated with crack propagation at room
temperature.Theiratomicallysharpmodelisinfactin
agreement with the earlier idea of the latticetrapped
theoryandcohesiveforcetheory.Evidencesupporting
the concept ofan atomically sharp crack mainly came
from the earlier TEM studies of crack tips, and that
wasverifiedlaterbyHREMandhighvoltageelectron
microscope(HVEM)studies.Thosestudiescommonly
showedthattherewasnoevidenceofmicroplasticity
nearthecracktips,andsuccessivedebondingbetween
two adjacent lattice planes was the basic fracture
modelinthecovalentcrystals.Recentobservationsby
HVEM and atomic force microscopy (AFM) have,
however,indicated that dislocations might be emitted
from a crack tip induced by indentation in silicon
whenthetemperaturewasraisedtohigherthan552C
to activate dislocation sources. The key to
understandingthestructureanddeformationbehavior
of a crack tip in a brittle material is to make a crack
with a very sharp tip, and then to make direct
observationsattheatomicscale.

Sutton et al. also found that crystallization is an

instantaneous process, where a weak ordered
structureintheamorphouszoneisastheprecursor
of crystallization, and then this kind of weak
ordered structure may transfer the ordered
crystalline. Obviously, the weakordered structure
is similar to the atomic clusters observed in the
present work. It is found that the clusters with a
size of nanoscale occurred when the irradiation
reached10minasshowninFig.26b,andthiskind
of clusters may act as the nuclei of crystallization.
And as increasing irradiated time, the nuclei grow
gradually at the amorphous and crystalline nuclei
interface. So it is reasonable to propose that the
crystallization may involve two processes: the
atoms in the amorphous zone ahead of the cluster
form a new ordered cluster by diffusion, and then
these clusters growth into the nucleus of the
crystallinegrains.

DeformationandCrackingAheadofCracktip

Thebrittlefractureofstructuralmaterialshasbeenthe
project of numerous theoretical and experimental
investigations since the earliest explanations
developed by Inglis and Griffith, but the basic
mechanism of the phenomenon has hitherto been
unclear.Themajorreasonforthisisthatthestructure
anddeformationbehavioratthecracktipunderstress
isnotwellunderstoodatpresent.Thestructureatthe
cracktipinducedbystressisthesocalledblackbox,
although some models had been developed as shown
in Fig. 27. Continuum media mechanics is shown to

FIG.27ILLUSTRATIONOFVARIOUSCRACKTIPMODELS, (a)
ATOMICALLYSHARPCRACKMODEL,(b)
QUASIONEDIMENSIONALMODELOFASHARPCRACK,
WITHNONLINEARCHARPTIPBONDEMBEDDEDINA
LINEARLATTICE,(c)DUGDALEBARENBLATTMODELOF
THECRACKTIP

23

www.mejournal.org JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014

from a crystalline lattice to a disordered structure

alongthepropagationdirectionofthecracktipandthe
fact that the disordered regions between the crack
walls (Fig. 30a) are connected to form an amorphous
band (Fig. 30b) can be clearly seen. The displacement
inatomicarrangementbetweenbothsidesofthecrack
(indicatedbyFDinFig.30b)anddislocationsindicated
by D is apparent (Fig. 30b). Electron diffraction
analysis shows that the three group of atomic planes
are(001),( 111 )and( 11 1 ),respectively,andtheextent
of the atomic disorder is quite different in these three
planes as shown in Fig. 30b. The lattice disordered
extent is the lightest in ( 111 ), and the most severe in
( 11 1 ), in which the atom arrangement is completely
disordered.

Fig. 28 shows brightfield TEM images of the cracks

inducedbyVickersindentationwithaloadof0.049N
onthesurfaceof(110)SiandGaAs.Itisinterestingto
find that the mircocracks appear at the intersections
between the slip bands, rather than at the corners of
theindenterasshowninFig.28c.
To explore the origin and nature of the cracks, an
observation ahead of the cracktip was made on the
diffractioncontrastscaleasthefirststep.Fig.29shows
aimageatacracktipinducedbyindentationinsingle
crystal Si. It was found that the crack tip can emit
several groups of dislocations which can interact to
form the dislocation network. This implied that the
cracktipappearsplasticbehavior.

FIG.28TEMBRIGHTFIELDIMAGE,SHOWINGASMALL
CRACKWITHAVERYSHARPTIPAPPEAREDATTHE
INTERSECTIONBETWEENSLIPBANDS,(a)INSi,(b)INGaAs,
AND(c)SCHEMATICDIAGRAMOFTHECRACKPRODUCTION

FIG.30HREMIMAGESTAKENFROMAREGIONAHEADOFA
CRACKTIP,(a)ASERIESOFCLUSTERSWITHDISORDERED
LATTICEMARKEDBYABETWEENTHECRACKWALLS,(b)A
MAGNIFIEDHREMIMAGETAKENFROMTHECRACKTIP,
SHOWINGAMORPHOUSBANDWITH12NMINWIDTH,
DISLOCATIONS(DENOTEDBYD),ANDDISPLACEDLATTICE
(DENOTEDBYDL)AHEADOFTHECRACKTIP

In order to confirm further the results obtained by

HREM observations mentioned above, fastFourier
transformation (FFT) and Inversefast Fourier
transformation (IFFT) were performed on areas
selected near the crack tip. Fig. 31 shows an HREM
image of a crack tip, and the FFT results (denoted as
FFTSAED) from two selected regions marked by the
squaresIandIIareinserted,respectively.Accordingto
the FFTSAED, IFFT transition was performed to get
the corresponding IFFT fringe images for the three
planes of ( 111), (001) and ( 11 1 ), respectively. Figs.
32a, 32b and 32c present the IFFT fringe images
resultingfromtherelatedFFTSAEDs( 111 ),(001)and
( 11 1 ), respectively, corresponding to the region II as
shown in Fig. 31. It is fascinating to find that the
fringes are not changed on the ( 111) plane, and the
atomarrangementisstillessentiallyordered(Fig.32a).

FIG.29CROSSSECTIONIMAGEOFDISLOCATIONEMISSION
FROMTHECRACKTIPINSILICONSINGLECRYSTAL
DEFORMEDUNDERINDENTATION

Fig. 30 is a group of HREM images taken from the

cracktipinFig.28b.Fig.30ashowsindetailthecrack
tipstructureinducedbyanindentationwithaloadof
0.049 N. It is fascinating to find that a series of
amorphousclusters(indicatedbya)about23atoms
in width are separated by areas of crystalline fringes
(indicatedbyc),andtheyaredistributedalternately
between the crack walls. As the indentation load
increases to 0.098 N, an amorphous band of 12 nm
width forms between the crackwalls and the crack
propagatesalongtheamorphousbandasshowninFig.
30b,whichisamagnifiedHREMimagetakenfromthe
left part of the Fig. 30a. The process of the transition

24

JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014 www.mejournal.org

ofthegrainsduringannealing.

However, the lattice arrangement ahead of the crack

tipisdistortedseriouslyonthe(001)and( 11 1 )planes
and dislocations occurring on the (001) and ( 11 1 )
planes as shown by arrows in Figs. 32b and 32c.
SimilarresultswereobtainedfromsquareIinFig.31.
As shown by arrows in Figs. 32d, 32e and 32f, the
fringes keep a normal arrangement essentially on the
( 111)plane,seriouslatticedistortionoccurson( 11 1 ),
anddislocationsappearinboth(001)and( 11 1 )planes.
All these results observed in GaAs single crystal are
surprisinglysimilartothoseobtainedbyHREMforSi
singlecrystals.

FIG.31HREMIMAGEOFACRACKTIP,ANDFASTFOURIER
TRANSFORMATION(FFT)RESULTSFROMTWOSELECTED
SQUARESMARKEDBYIANDIIARESHOWN,RESPECTIVELY

Sofar,onemaystillarguethattheamorphousregions
between the crack walls observed ahead of the crack
tip in this study could probably be introduced by
specimen preparation such as grounding or ionbeam
thinning. In order to rule out these possibilities, an
EDX determination of the chemical composition in an
amorphous band was performed using a
fieldemissiongunTEM2000(FEGTEM2000)withan
electronbeamspot1nmindiameter.Theresultshows
thatinadditiontoGaandAs,therearenoimpurities
to be detected inside the amorphous band, and the
chemical composition of the amorphous band is
completelythesameasthatfromaregionofthematrix
far away from the crack tip. This implies that the
amorphousbandbetweenthecrackwallsaheadofthe
crack tip could not have been introduced by either
impurities or contamination during specimen
preparation. To confirm this point further, the
specimenwithanamorphousbandaheadofthecrack
wasannealedat500Cfor60min,asdescribedinFig.
24.Itwasfoundthattheamorphousbanddisappeared
and recrystallized grains appeared along the band
aheadofthecracktip.Theserecrystallizedgrainshad
thesamelatticestructureasthematrix,althoughtheir
sizeisslightlylargerthanthewidthoftheamorphous
bands.Thisisprobablytobeattributedtothegrowth

FIG.32FFTSAEDANDCORRESPONDINGIFFTFRINGESFROM
DIFFERENTLATTICEPLANESINSELECTEDSQUAREII(a,b,
ANDc)ANDSQUAREI(d,eANDf),RESPECTIVELY

All the observations reported above provide new

insightsintothepossiblestructureatthecracktipand
the fracture mechanism in highly brittle crystalline
materials such as GaAs single crystal. Deformation
alongdifferentcrystallineplanesaheadofthecracktip
is anisotropic and the crack tip induced during
indentation at room temperature under stress is not
atomicallysharp.Dislocationsareproduced,leadingto
crystal lattice distortion, and even a transformation
from a crystalline lattice to a disordered structure
ahead of the crack tips. The crack propagation is
proposed to be a result of decohesion by the
amorphousband,ratherthanthesequentialruptureof

25

www.mejournal.org JournalofMetallurgicalEngineering(ME)Volume3Issue1,January2014

cohesivebands.

A.

Meldrum,

L.A.

Boatner

and

R.C.

Ewing,

Electronirradiationinduced nucleation and growth in

Conclusions

amorphous LaPO4, ScPO4, and zircon, J. Mater. Res.,

(1)Rosettedislocationsoccurredandinhomogenously
distributed around an indentation in the ambient
temperature brittle materials such as Si and GaAs
singlecrystals.Theshortrosettearmdislocationswith
theBurgersvectorof1/2[110]belongtotypemixture
dislocations, and the longrosette one with Burgers
vector of 1/2[1 1 0] belong to the type screw
dislocations. Twins and stacking faults are also the
partsofcrystaldeformation.

vol12,pp.18161827.July,1997.
A.A. Griffith, The phenomena of rupture and flow in
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October,1920.
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August,2000.

(2) Transition from crystal lattice to nanocrystalline

and amorphous structure took place in silicon and
galliumarsenidesinglecrystalsunderindentation.The
shear stress rather than hydrostatic pressure is
proposed to attribute to the transition, and there are
criticalshearstressesforthetransitions.

A.L. Ruoff and T.Li, Phase transitions in IIIV compounds

tomegabarpressures,Annu.Rev.Mater.Sci.,vol25,pp.
249271.August,1995.
B.J. Hockey and B.R. Lawn, Electron microscopy of
microcracking about indentations in aluminium oxide

(3)Theatomlevelstructureaheadofthecracktipshas
been successfully captured by using the HREM
observations with both plane and cross sectional
views. The crack tips are not atomically sharp. The
dislocations can be emitted from the crack tip during
indentation, leading to crystal lattice distortion and
even to a transition from a crystalline lattice to
disordered structure, forming an amorphous band
withawidthof12nm.Thecrackpropagatesalongthe
amorphousband,ratherthanthesequentialruptureof
cohesivebonds.

andsiliconcarbide,J.Mater.Sci.,vol10,pp.12751284.
August,1975.
B.R.Lawn,Physicsoffracture,J.Am.Ceram.Soc.,vol66,
pp.8391.February,1983.
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study,J.Mater.Sci.,vol15,pp.12071223.May,1980.
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December,1975.

(4) The analysis of fast Fourier transformation

(FFT)SAED and corresponding inversefast Fourier
transformation(IFFT)fringeimagesofdifferentlattice
planesshowsthatdeformationaroundthecracktipis
anisotropic.Thelatticefringesalong( 111)planedoes
notchangeandtheatomarrangementonthisplaneis
still essentially ordered, and serious lattice distortion
occursontheplanesof(001)and( 11 1 ).

C.E.Inglis,Stressesinaplateduetopresenceofcracksand
sharp corners, Trans. Inst. Naval. Archit., vol 55, pp.
219241.March,1913.
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(5)InsituobservationsbyHREMshowthatthereisa
critical electronbeam current density, instead of the
irradiationinducedtemperaturerise,forthecrystalline
nucleation during crystallization process. Critical
electron beam current density for the crystalline
nucleationis50pA/cm2.Thelargerthecurrentdensity
is,thefasterthecrystallizationrateis.

Hockey,Amorphizationandconductivityofsiliconand
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Le

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G.

Patriarche,

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of

nanoindentations in heavily n and pdoped (0 0 1)

GaAs, Acta Materialia, Vol. 56, pp. 14171426, April,
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