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Armstrong Indentation
Armstrong Indentation
Armstrong Indentation
H
G L/4Pd
)
/,5' 495
a val1e of
H
G DC9 &Pa' 6as o$tained for the !a:i!1! load val1e of I.+C ; in 3ig. -'
and
H
6as increased to DI* &Pa at -** ;' and to D-** &Pa at C** ; load' also
corresponding to 4d/D5 val1es of *.) and *.,' respectively. .he slo6er increase of
H
6ith change in displace!ent at the larger loads' and corresponding larger indentation
si7es' is in line 6ith the !entioned2a$ove indenter shapes $eing designed to achieve
effective large strains so as to o$tain a representative hardness stress that is relatively
insensitive to the i!posed strain. In this regard' a direct linear dependence in 3ig. - of
the ordinate val1e of L on h at relatively s!all h co!pared to D' see e=s. 4)5 and 495'
6o1ld correspond to a constant val1e of
H
. Close e:a!ination of the load vs.
penetration depth dependence in 3ig. -' ho6ever' reveals the trend for
H
to increase
strongly at first fro! an initial plastic yielding val1e' and s1$se=1ently to increase !ore
slo6ly at larger straining' pres1!a$ly' in an analogo1s !anner to the !aterial strain
hardening $ehavior in a co!pression test.
(eter!ination of the plastic hardness stress at varying 4d/D5 val1es !ay $e co!pared
6ith the Hert7ian elastic stress operative at the onset of plastic yielding of the speci!en
$y e!ploying the relationship $et6een $all contact dia!eter d
e
and h
e
as d
e
G >)h
e
(?
-/)
so
as to o$tain the analogo1s elastic hardness stress'
E
' as
E
G 4,/9P5E
r
4d
e
/(5' 4,5
in 6hich 4d
e
/(5 is taken as a !eas1re of the hardness strain. 3or 3ig. -' an elastic
hardness stress of D--* &Pa 6as esti!ated fro! the Hert7ian c1rve load' D*.) ;' and
displace!ent' -.B : -*
2,
!!' deter!ined at the onset of yielding. .h1s'
E
at the onset of
yielding for /Cl crystals is associated 6ith an i!!ediately lo6er val1e of
H
that
increased 6ith plastic straining to a hardness val1e near to that of the
E
level. In f1rther
researches involving other !aterials' the !ethod of perfor!ing a contin1o1s indentation
hardness test via a conventional testing !achine 6as e!ployed to o$tain elastic !od1l1s
eval1ations for 6ood2derived lignan !aterial >,? and to o$tain elastic/plastic defor!ation
res1lts on polycrystalline al1!in1! !aterial >C?. &ore recent elastic !od1l1s res1lts
6ere reported for solid and poro1s polycrystalline al1!in1! !aterials' incl1ding
co!parison of the c1rrent and previo1s loading !eas1re!ents 6ith !od1l1s esti!ations
o$tained fro! the initial part of the 1nloading c1rve >F?.
Nanoindentation test measurements
;anoindentation hardness testing' 6ith its e:ceptional !eas1re!ent sensitivity of load
and displace!ent val1es that are achieved on a contin1o1s loading $asis' nat1rally lends
itself to the st1dy of initial yielding in the indentation process' partic1larly' 6hen acco1nt
is taken of the consideration that the indenter tip' ho6ever shaped' 6ill generally $e
ro1nded at the !icro2 or nano2di!ensional scale. .h1s' fit of the Hert7ian elastic
relationship $et6een h
e
and L in e=. 4-5 to the de!onstrated reversi$le indentation c1rve
reported for an &g0 4**-5 crystal s1rface 6as e!ployed to specify a Berkovich tip
dia!eter of 9.+ !icrons in one test' and' in another test 6as fitted 6ith a tip dia!eter of
9.) !icrons. In the latter case' the analysis 6as e:tended to a description of higher load
val1es !eas1red $oth for the Hert7ian elastic stress at yield and for the initial plastic flo6
stress defined in e=. 495 and e!ploying the e=. 4)5 relationship $et6een d and h >+?.
3ig1re ) sho6s si!ilar application to an apparently significantly different &g0 crystal
loading c1rve reported $y Cha1dhri >B' I?. In this case' too' a Berkovich dia!ond
indenter 6as e!ployed for nanoindenting a cleaved 4**-5 &g0 crystal s1rface. .he
initial loading $ehavior is sho6n to $e fitted 6ith e=. 4-5 $eginning fro! an ass1!ed
offset displace!ent of ,.* n! and a trial2and2error2deter!ined indenter tip radi1s of ,**
n!' also e!ploying the sa!e PoissonMs ratio and No1ngMs !od1l1s val1es of *.*FB and
--,C EPa for a dia!ond indenter and *.-B- and 9-) EPa for the &g0 crystal' as
previo1sly e!ployed in reference >+?. .he onset of f1ll plastic yielding at the indentation
site is !arked at the Qpop2inR point in 3ig. )8 and' follo6ing the pop2in displace!ent' the
esta$lish!ent of a plasticity2infl1enced defor!ation c1rve is seen to take on a
significantly red1ced load dependence in the s1$se=1ent displace!ent. E:cept for the
very different !agnit1des of load and displace!ent scales sho6n in 3igs. - and )' the
overall shapes of the defor!ation c1rves appear reasona$ly si!ilar. In other
nanoindentation tests on &g0 crystals' ho6ever' s!aller Qpop2inR discontin1ities
representing only interr1ptions of the other6ise elastic loading c1rve have $een reported
>-*?. .he pre2yield Qpop2inR offsets $et6een contin1ed elastic loading seg!ents are
easily recogni7ed in these cases $y si!ply shifting the s1$se=1ent contin1ed elastic
loading c1rve to fit the earlier defor!ation. E=1ation 495 eval1ations for s1ch Qpop2insR
give 1nrealistically high val1es of
H
. Even for Cha1dhriMs test res1lt in 3ig. )' ho6ever'
it 6as not possi$le to locate the resid1al nanoindentation.
3ig1re 9 sho6s the previo1sly 1nreported elastic c1rve for fit of a Berkovich tip dia!eter
of 9)** n! to an other6ise f1lly analy7ed &g0 nanoindentation test res1lt reported $y
.ro!as et al. >--? and $y Co1pea1 et al. >-)?. .he fitted indenter tip dia!eter of 9)**
n! is eight ti!es greater than the ,** n! val1e deter!ined for 3ig. ). .he difference in
effective ( val1es acco1nts for the significantly different load and displace!ent
!eas1re!ents that are sho6n in the t6o defor!ation c1rves. ith the ass1!ption that
the onset of f1ll yielding in 3ig. 9 6as deter!ined $y the designated Qpop2inR
displace!ent' h
p
G 9- n! at a val1e of L G F.9C !;' and h
p
G h in e=. 4)5' then a val1e of
H
G )*.F EPa 6as co!p1ted for the yield stress $ased on the co!p1ted d G F)+ n! and a
val1e' then' of 4d/D5 G *.). A val1e of
E
G )-.9 EPa' only slightly greater than
H
' 6as
co!p1ted 1sing e=. 4,5. .he plastic hardness res1lt co!pares in 3ig. ) fro! Cha1dhri
6ith a co!p1ted val1e of
H
G )C.- EPa deter!ined for the lo6er val1es of h
p
G B.)C n!
and L G *.)CC !;. And a val1e of
E
G D9*.+ EPa is o$tained for this test res1lt O1st
prior to the yield2type Qpop2inR. Sery interestingly' 6ith co!p1tation of d G --9.+ n!
for the 3ig. ) test res1lt' a relatively high val1e of 4d/D5 G *.)B, is o$tained for the
sharper indenter tip. .h1s' the contin1ation of f1ll plasticity in this case is soon
controlled $y the trigonally2shaped indentations o$tained at a relatively lo6 load of DC
!;' or less' and leads to the Cha1dhri2reported hardness val1es of I.F EPa' o$tained at a
load of )* !;' and B., EPa' at C* !;.
A log/log hardness stress strain !ethod of co!parison of
E
and
H
stresses 6as
deter!ined as a f1nction of (d/D) for &g0 crystal !eas1re!ents $y Ha!!ond and
Ar!strong >-9? and 1pdated in reference >+? $y addition of the closed circle
!icroindentation res1lts reported previo1sly $y Ar!strong and Ragh1ra! >-,? and $y
addition of the co!p1ted hardness val1es o$tained fro! 3ig. 9. 3ig1re , sho6s the
f1rther 1pdate of res1lts' especially involving co!parison of $oth
H
and
E
deter!inations o$tained fro! 3igs. ) and 9. In 3ig. ,' the plotted (d/D) val1es 6ere
either directly deter!ined fro! the !eas1re!ents' as descri$ed a$ove' or 6ere
deter!ined $y kno6n conversion val1es' for e:a!ple' (d/D) G *.9+C for the dia!ond
pyra!id indentation 4as co!pared 6ith *.,) for the Berkovich indenter5. As indicated in
3ig. ,' the total plastic hardness res1lts 6ere o$tained for applied load val1es ranging
fro! C* ; to *.)CC !;' th1s prod1cing an increasing hardness val1e 6ith decreasing
load 1ntil in the t6o s!allest load tests' the plastic hardness stresses'
H
' approach the
Hert7ian elastic stresses'
E
' for 6hich the applied loads are only elastically s1pported.
.he open circle point on the Hert7ian elastic loading line in 3ig. ,' at D G F.9C !!' and
open s=1are point' at D G 9.+ !icrons' are for hardness stress val1es esti!ated on an
indentation fract1re !echanics 4I3&5 $asis' as 6ill $e descri$ed later in connection 6ith
other test res1lts.
Elastic vs. plastic strains
.he resid1al dislocation defor!ation patterns s1rro1nding aligned dia!ond pyra!id
!icroindentations p1t into 4**-5 &g0 crystal s1rfaces have $een e:tensively st1died' for
e:a!ple' as descri$ed in >-C?' partic1larly for resid1al plastic indentations having
conve:2like shapes acco!panying the indenter sides $eing aligned parallel to T--*U
directions and for concave2like shapes for the indenter sides $eing aligned parallel to
T-**U directions. Beyond the descri$ed scanning electron !icroscopy 4SE&5 and :2ray
diffraction topography res1lts descri$ed in >-F?' !ore recent ato!ic force !icroscopy
res1lts have $een reported also for dislocation etch2pitted nanoindentation res1lts !ade in
e:tension of original pioneering etch2pit res1lts o$tained at !icroindentations >-+?. 3or
the T-**U align!ent case' 3ig. C sho6s sche!atically the generally agreed 1pon !odel
dislocation distri$1tion that has $een investigated to 1nderstand $etter' for s1fficiently
large applied load val1es' the fo1r2fold pattern of cracking that occ1rs on vertical H--*J
planes containing the indentation direction >-C?. As 6ill $e disc1ssed' the !odel for the
dislocation pile21p ind1ced H--*J cracking' that has $een investigated !ost recently in a
spherical $all2type nanoindentation testing proced1re >-*?' occ1rs at a lo6er hardness
stress than predicted on an elastic I3& $asis $1t the i!!ediate point of interest here is
the relatively co!para$le contri$1tions of $oth the plastic dislocation displace!ents and
the 41nloading5 elastic recovery strains to the resid1al indentation shapes. 3or e:a!ple'
even at an applied load of C* ; for the lo6est hardness test res1lts in 3ig. ,' the elastic
strain is esti!ated as 4d/(5 G D*.*+' and this co!pares 6ith the $all2e=1ivalent plastic
strain val1e of 4d/(5 G *.9+C for the dia!ond pyra!id indentation.
At the increasing hardness val1es plotted in 3ig. ,' the ratio of elastic2to2plastic strains
for dia!ond pyra!id indentations increases significantly as the Hert7ian elastic loading
c1rve is approached. Ha!!ond and Ar!strong >-9? had de!onstrated a red1ction of the
indentation depth on 1nloading of dia!ond pyra!id !icroindentations thro1gh !eas1red
changes in the angle $et6een opposite indentation facets. oirgard et al. have
co!!ented on the flat nat1re of resid1al nanoindentations !ade in EaAs as part of a
research investigation also involving &g0 nanoindentations >-B?. Also' Co1pea1 et al.
>-)? reported ato!ic force !icroscopy i!ages and s1rface depth !eas1re!ents for the
resid1al indentation test res1lt descri$ed in 3ig. 9 that !atch the very s1$stantial depth
recovery sho6n in the 1nloading c1rve. 3or e:a!ple' the =1antitative !eas1re!ent
reported of a do6n6ard tro1gh2like displace!ent of D-, n! of the crystal s1rface O1st
o1tside of the resid1al indentation' along the >*-*? direction' is in agree!ent 6ith the
dislocation !odel description of 3ig. C' 6here$y the !eas1re!ent is acco1nted for $y the
indentation2for!ing T*--U B1rgers vector dislocations spreading in a scre6 orientation
along the >*-*? direction >+?.
Crystal comparisons on a hardness stress-strain basis
3ig1re F sho6s a co!pilation of hardness val1es of vario1s crystals 6ithin the fra!e6ork
of the proposed $all2type indentation stress 2 strain description' incl1ding for &g0 the D+
EPa average dia!ond pyra!id !icroindentation hardness val1e' involving H--*J plane
cracking of the type !odeled in 3ig. C. In the present case' different co!p1ted Hert7ian
elastic loading lines are sho6n on the left2side of the fig1re on the $asis of e!ploying a
steel $all indenter 6hereas the collected dia!ond pyra!id hardness val1es are plotted at
their $all2e=1ivalent val1e of 4d/D5 G *.9+C. In the fig1re' a solid Hert7ian line and
s1$se=1ent plastic flo6 c1rve is sho6n for an ;aCl crystal indented 6ith a F.9C !! steel
$all in a conventional !acroscopic loading test as descri$ed for the /Cl defor!ation
c1rve sho6n in 3ig. -. Also appearing in the fig1re are individ1al open2s=1are
!icrohardness !eas1re!ents !ade on a 4cyclotri!ethylentrinitra!ine5 R(< 4)-*5
crystal s1rface e!ploying a -.CI !! dia!eter steel $all8 see reference >-F? for f1rther
details a$o1t R(< crystal properties. And' at the 1pper end2points of the Hert7ian elastic
loading lines are a n1!$er of open2circle points co!p1ted in accordance 6ith the I3&
relationship reported $y #a6n >-I? as
C
G H,E
s
V/>PD4- K
s
)
54W
-
)
L W
)
)
5?J
-/)
4d/D5
2-/)
4C5
In e=. 4C5' V is the crack s1rface energy' 4W
-
)
L W
)
)
5 G ).C : -*
2C
6as specified as a
n1!erical factor' and the other para!eters 6ere already defined for e=. 4-5. E:a!ination
of e=. 4C5 sho6s that the cracking stress'
C
' decreases as D increases and this is sho6n to
$e the case in 3ig. F for the D G F.9C !! and D G *.-), !! points p1t onto the &g0
line8 the 1pper *.-), !! D val1e is the $all2dia!eter e=1ivalent of the dia!ond pyra!id
!eas1re!ent that is plotted.
3ig1re F !akes clear the increasing i!portance of the elastic defor!ation part of the
hardness property as the hardness itself increases a!ong the !aterial val1es that are
sho6n. .he ;aCl contin1o1s indentation stress strain and dia!ond pyra!id res1lt is
sho6n to have a negligi$le elastic strain contri$1tion of 4d/D) G D*.**+ for the hardness
at 4d/D5 G *.9+C. Also' the ;aCl stress strain c1rve follo6s the trend of
E
and
H
eval1ations that have $een descri$ed for the /Cl loading res1lt in 3ig. -. In addition'
co!parison of the elastic and plastic properties of ionically2$onded ;aCl and the
!olec1larly2$onded energetic crystal' R(<' sho6s that 6hereas ;aCl is elastically
stiffer' as e:pected on the $asis of the respective ionic and !olec1lar $onding types'
R(< is plastically stronger' as acco1nted for on the $asis of the hindrance to dislocation
!otion in the relatively co!ple: R(< orthorho!$ic lattice >)*?. 0f greater interest in
the present case' ho6ever' is co!parison in 3ig. F of the esti!ated elastic I3& cracking
stresses' say' either for the effective 4dia!ond pyra!id5 s!all2$all res1lt of D G *.-),
!! sho6n for &g0 or the calc1lated -.CI !! dia!eter $all cracking stress esti!ation
!ade for R(<. .he lo6er !eas1red cracking stresses in each case are nat1rally
attri$1ted to the crack2pro!oting capa$ilities of dislocations involved in the plasticity of
the respective !aterials' partic1larly' 6hen dislocation pile21ps occ1r to concentrate
locally the action of the applied stress >)-?. Ar!strong and El$an have recently revie6ed
the case for s1ch pile21ps playing an i!portant role in the e:plosive deco!position of
R(< and other energetic !aterials >))?.
Summary
Indentation hardness !eas1re!ents covering !acroscopic' !icrostr1ct1ral' and
nanoindentation test !ethods have $een co!pared on a hardness stress 2 strain $asis'
partic1larly involving !eas1re!ents !ade on /Cl' &g0' ;aCl' and R(< crystals. 3or
&g0 in partic1lar' a =1antitative assess!ent has $een !ade of the elastic' plastic' and
cracking $ehaviors deter!ined fro! !icro2 and nano2indentation hardness test res1lts.
.he hardness stress 2 strain description is sho6n to provide a 1sef1l $asis for co!paring
different !aterial $ehaviors over the f1ll defor!ation range fro! elastic loading to
plasticity2ind1ced cracking.
Acknowledgement
0ne of the co2a1thors' Ron Ar!strong' thanks (r. Nves Eaillard for providing $oth
helpf1l reprints and infor!ation concerning his co!prehensive !eas1re!ents !ade 6ith
colleag1es on nanoindenting &g0 4**-5 crystal s1rfaces.
References
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#ist of 3ig1res
3ig. -. &acroscopic load vs. indentation depth for a /Cl crystal in a $all2type contin1o1s
loading test' adapted fro! res1lts reported $y Ar!strong and Ro$inson >9?.
3ig. ). ;anoindentation load vs. depth for an &g0 4**-5 crystal s1rface indented 6ith a
Berkovich indenter of tip dia!eter ,** n!' as deter!ined for a test res1lt reported $y
Cha1dhri >B' I?.
3ig. 9. ;anoindentation load vs. depth for an &g0 crystal indented 6ith a Berkovich
indenter of tip dia!eter 9)** n!' as deter!ined for a test res1lt reported $y .ro!as et al.
>--?.
3ig. ,. Hardness stress 2 strain relationship for co!$ined &g0 crystal res1lts' adapted
fro! res1lts reported $y Ar!strong et al. >+? to incl1de 4closed triangle5 eval1ations
derived fro! a test res1lt reported $y Cha1dhri >B' I?.
3ig. C. (islocation !odel of plastic flo6 at a dia!ond pyra!id indentation in an &g0
4**-5 crystal s1rface' after Ar!strong and 1 >-C? and Ar!strong and El$an >-F?.
3ig. F. Hardness stress 2 strain res1lts for a variety of crystal !aterials' adapted fro!
Ar!strong and El$an >))?8 -.* kgf/!!
)
G I.B- &Pa.
3ig. -. &acroscopic load vs. indentation depth for a /Cl crystal in a $all2type contin1o1s
loading test' adapted fro! res1lts reported $y Ar!strong and Ro$inson >9?.
3ig. ). ;anoindentation load vs. depth for an &g0 4**-5 crystal s1rface indented 6ith a
Berkovich indenter of tip dia!eter ,** n!' as deter!ined for a test res1lt reported $y
Cha1dhri >B' I?.
3ig. 9. ;anoindentation load vs' depth for an &g0 crystal indented 6ith a Berkovich
indenter of tip dia!eter 9)** n!' as deter!ined for a test res1lt reported $y .ro!as et al.
>--?.
3ig. ,. Hardness stress strain relationship for co!$ined &g0 crystal res1lts' adapted
fro! res1lts reported $y Ar!strong et al. >+? to incl1de 4closed triangle5 eval1ations
derived fro! a test res1lt reported $y Cha1dhri >B' I?.
3ig. C. (islocation !odel of plastic flo6 at a dia!ond pyra!id indentation in an &g0
4**-5 crystal s1rface' after Ar!strong and 1 >-C? and Ar!strong and El$an >-F?.
3ig. F. Hardness stress strain res1lts for a variety of crystal !aterials' adapted fro!
Ar!strong and El$an >))?8 -.* kgf/!!
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G I.B- &Pa.