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Stress measurement using area detectors: a theoretical and experimental comparison of different methods in ferritic steel using a portable X-ray apparatus

Abstract

Using area detectors for stress determination by diffraction methods in a single exposure greatly simplifies the measurement process and permits the design of portable systems without complex sample cradles or moving parts. An additional advantage is the ability to see the entire or a large fraction of the Debye ring and thus determine texture and grain size effects before analysis. The two methods most commonly used to obtain stress from a single Debye ring are the so called cos α and full-ring fitting methods, which employ least-squares procedures to determine the stress from the distortion of a Debye ring by probing a set of scattering vector simultaneously. The widely applied sin2 ψ method, in contrast, requires sample rotations to probe a different subset of scattering vector orientations. In this paper we first present a description of the different methods under the same formalism and using a unified set of coordinates that are suited to area detectors normal to the incident beam, highlighting the similarities and differences between them. We further characterize these methods by means of in-situ measurements in carbon steel tube samples, using a portable detector in reflection geometry. We show that, in the absence of plastic flow, the different methods yield basically the same results and are equivalent. An analysis of possible sources of errors and their impact in the final stress values is also presented.

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Stress measurement using area detectors: a theoretical and experimental comparison of different methods in ferritic steel using a portable X-ray apparatus

Author: Ramírez Rico, Joaquín; Lee, Seung Yub; Ling, Jingjing; Noyan, Ismail C.
Publisher: Springer Verlag
Year: 2016
DOI: 10.1007/s10853-016-9837-3
Source: https://idus.us.es/bitstreams/73c9ed2b-9b25-4704-8060-f39b44d41d03/download
S ess measu emen using a ea de ec o s. A heo e ical and
expe imen al compa ison o diffe en me hods in e i ic s eel
using a po able x- ay appa a us
J. Rami ez-Rico1,∗, S.-Y. Lee2, J.J. Ling2and I. C. Noyan2
1Fisica de la Ma e ia Condensada-ICMS, Uni e sidad de Se illa-CSIC, 41012
Se illa, Spain.
2Applied Physics and Applied Ma hema ics, Columbia Uni e si y, New Yo k, NY
10027
∗Co esponding au ho : [email p o ec ed]
Abs ac
Using a ea de ec o s o s ess de e mina ion by diff ac ion me hods in a single ex-
posu e g ea ly simplifies he measu emen p ocess and pe mi s he design o po able
sys ems wi hou complex sample c adles o mo ing pa s. An addi ional ad an age
is he abili y o see he en i e o a la ge ac ion o he Debye ing and hus de e -
mine ex u e and g ain size effec s be o e analysis. The wo me hods mos commonly
used o ob ain s ess om a single Debye ing a e he so called cos αand ull- ing
fi ing me hods, which employ leas -squa es p ocedu es o de e mine he s ess om
he dis o ion o a Debye ing by p obing a se o sca e ing ec o simul aneously.
The widely applied sin2ψme hod, in con as , equi es sample o a ions o p obe a
diffe en subse o sca e ing ec o o ien a ions. In his pape we fi s p esen a de-
sc ip ion o he diffe en me hods unde he same o malism and using a unified se o
coo dina es ha a e sui ed o a ea de ec o s no mal o he inciden beam, highligh ing
he simila i ies and diffe ences be ween hem. We u he cha ac e ize hese me hods
by means o in-si u measu emen s in ca bon s eel ube samples, using a po able de-
ec o in eflec ion geome y. We show ha , in he absence o plas ic flow, he diffe en
me hods yield basically he same esul s and a e equi alen . An analysis o possible
sou ces o e o s and hei impac in he final s ess alues is also p esen ed.
1 In oduc ion
A ea x- ay de ec o s allow he eco ding o esidual elas ic s ain in a ma e ial along a
se o sca e ing ec o s in a single measu emen , so ha he numbe o sample o a ions
equi ed o de e mina ion o he esidual s ess s a e is significan ly educed and, in some
cases, comple ely elimina ed. This well-known ac o med he basis o adi ional ‘film’
echniques, whe e Debye Ring(s) om a polyc ys alline sample we e cap u ed on x- ay
sensi i e pho og aphic film using labo a o y sys ems [1–3] o po able s ess analyze s
[4]. A comp ehensi e e iew o such ‘single-exposu e’ echniques was gi en by James and
Cohen in 1978 [5]. Wi hin he las decade mode n de ec o s which eco d and(o ) ead ou
inciden x- ay in ensi i es elec onically om he cells o a pixella ed a ea de ec o eplaced
film. Publica ions u ilizing hese new a ea de ec o s epo ed ‘new’ echniques o he
analysis o esidual s esses, whe e e ms like ‘XRD2: Bidimensional X-Ray Diff ac ion’
[6] o ‘2-dimensional x- ay diff ac ion’ [7] we e in oduced. In con as o he con en ional
1
sin2ψ echnique used wi h poin de ec o s, which equi es he measu emen o s ain in
a leas wo dis inc sample o ien a ions o plane s ess s a es [8, 9], wi h a ea de ec o s
he esidual s ess can in p inciple be de e mined in a single exposu e, i espec i e o he
ype o de ec o , o he e ms used o desc ibe i . This ad an age, combined wi h he
minia u iza ion o image pla es, x- ay sou ces and associa ed eading elec onics, ha e
esul ed in comme cial po able appa a us designed o in-line and field measu emen
applica ions, especially o e ous me als [10]. An addi ional ad an age o an a ea de ec o
is he abili y o see he en i e Debye Ring be o e analysis and hus de e mine ex u e and
g ain size effec s [11]. Due o hese benefi s, a ea de ec o s a e specially well sui ed o
pe o ming in-si u measu emen s, ei he a ele a ed empe a u es o as unc ion o applied
s ess, i.e. e e ences [12, 13].
Diffe en app oaches o he de e mina ion o he s ess s a e om he in o ma ion
con ained in a single Debye exposu e exis , such as he cos αme hod in oduced by Sasaki
e . al [14–16] o he di ec leas squa es fi ing o he measu ed s ain [17]. Despi e he
a ac i eness o hese po able de ices in bo h indus ial and scien ific applica ions, he e
is no cu en ag eemen among expe s on he mos efficien , p ecise and accu a e s ess
de e mina ion o malism.
In his wo k, we compa e he h ee p oposed me hods om bo h heo e ical and ex-
pe imen al poin s o iew. A code o he gene a ion o syn he ic 2D x- ay diff ac ion
pa e ns was de eloped and used o s udy he diffe en me hods’ sensi i i y o misalign-
men , de ec o calib a ion pa ame e s as well as sca e in he da a. Fo he expe imen al
assessmen we ha e used a po able x- ay esidual s ess measu emen appa a us (µ-X360
esidual s ess analyze om Puls ec Indus ial Co., L d.) o de e mine he esidual s ess
in 1010 Ca bon S eel cylind ical ubes in-si u du ing ensile loading. The measu emen
condi ions, wi h igh space cons ain s o he de ec o , as well as he use o a non-fla
specimen, we e chosen o app oach hose o ac ual applica ions. Se e al samples we e
es ed h ough he p opo ional limi and he esidual s ess a a ious loads was de e -
mined om single x- ay exposu es, using bo h he cos αand he di ec leas squa es fi ing
me hods. Measu emen s we e pe o med a diffe en sample o ien a ions wi h espec o
he incoming beam o bo h assess i s effec on he calcula ed s ess, as well as o allow us
o use he sin2ψ echnique o compa ison. We emphasize ha ou pu pose is compa ing
he s esses ob ained by hese echniques o each o he , no o a known (applied) s ess.
The la e case would be es ing he accu acy o he echniques. Howe e , po able esid-
ual s ess measu emen de ices a e easy o misalign du ing field measu emen s [10], and
i so, will measu e he w ong s ess alue independen o he echnique used. Ou esul s
show ha , o a mis-aligned machine all echniques will be in e o by he same amoun ,
and in he case o a pe ec ly aligned sample all h ee would yield he co ec s ess.
2 S ess de e mina ion using a ea de ec o s
X- ay based echniques o de e mine he (elas ic) s ain and s ess in a ma e ial ely on
he use o in e -plana spacing in a c ys alline ma e ial as a buil -in s ain-gauge [7–9].
By measu ing he la ice spacing din a s essed sample and compa ing i s alue wi h he
la ice spacing d0o a s ess- ee sample (ideally iden ical o he s essed one in e e y o he
aspec ), we ob ain he p ojec ion o he s ain enso along he sca e ing ec o used in
he de e mina ion o d. Le (ψ, ϕ) be he pola angles ha de e mine he sca e ing ec o
qsin sample coo dina es,
2
qS=

sin ψcos ϕ
sin ψsin ϕ
cos ψ

=

q1
q2
q3

(1)
Then he s ain measu ed along he sca e ing ec o a angles (ψ, ϕ) can be exp essed
in e ms o he s ain componen s ϵij in sample coo dina es as:
ϵψϕ = (dψϕ −d0)/d0=qiqjϵij =ϵ11 cos2ϕsin2ψ+ϵ12 sin 2ϕsin2ψ
+ϵ22 sin2ϕsin2ψ+ϵ33 cos2ψ(2)
+ϵ13 cos ϕsin 2ψ+ϵ23 sin ϕsin 2ψ
Due o he shallow pene a ion o x- ays in mos ma e ials, ypically only nea -su ace
s esses can be measu ed, whe e due o bounda y condi ions he no mal s esses anish o
ze o a he su ace [8]. An addi ional hypo hesis is he absence o s eep s ain g adien s
[18, 19]. I ha is no he case, a mo e de ailed ea men is needed [20]. I is hen
cus oma y o assume a biaxial (o plane s ess) s ess s a e so ha :
σij =

σ11 σ12 0
σ12 σ22 0
0 0 0

=⇒ϵij =

ϵ11 ϵ12 0
ϵ12 ϵ22 0
0 0 ϵ33

(3)
We will u he assume ha he ma e ial’s elas ic beha io can be desc ibed as iso opic
and homogeneous, so Hooke’s law akes he o m:
ϵij =1 + ν
Eσij −δij
ν
Eσkk (4)
Whe e Eins ein’s summa ion con en ion is used h oughou . Wi h hese assump ions
eq. (2) simplifies o:
ϵψϕ =dψϕ −d0
d0
=(ϵ11 cos2ϕ+ϵ12 sin 2ϕ+ϵ22 sin2ϕ−ϵ33)sin2ψ+ϵ33
O , in e ms o s esses:
dψϕ −d0
d0
=1 + ν
Eσϕsin2ψ−ν
E(σ11 +σ22) (5)
Whe e σϕ=σ11 cos2ϕ+σ12 sin 2ϕ+σ22 sin2ϕ. Equa ion (5) is he basis o he sin2ψ
me hod, ha has been used o o e 50 yea s as he x- ay me hod o choice o s ess
de e mina ion [8].
Now we need o in oduce he goniome e con en ions ha will ela e he o ien a ion
o he sca e ing ec o in labo a o y (diff ac ome e ) coo dina es wi h hose in sample
coo dina es (Figu e 1). We will conside a 2D x- ay a ea de ec o o ien ed so i is no mal
o he incoming (p ima y) beam and hus eco ds backsca e ed beams diff ac ed om
he sample (2θ > π/2). Diff ac ed x- ays will, o a ce ain amily o la ice planes, o m
cones ha will in e sec he de ec o o ming ci cles o Debye ings. The semi-angles o
hese cones will be defined as 2η=π−2θ, and he pola angle along each o he Debye
ings will be no ed as α. Thus, o each poin in he de ec o wi h coo dina es (x, y), he
equi alen cone coo dina es can be de e mined using [7]:
3
an 2η=√(x−x0)2+ (y−y0)2
z0
, an α=x−x0
y−y0
(6)
Whe e (x0, y0) desc ibes he loca ion o he inciden x- ay beam in de ec o coo dina es,
while z0is he sample o de ec o dis ance. The sca e ing ec o co esponding o each
poin in he Debye ing also esides in a cone, in his case o semi-angle η. Since each
poin in he ing co esponds o a diffe en o ien a ion o he sca e ing ec o , he e mus
exis a ans o ma ion ha ela es i s coo dina es qLin he lab sys em o hose qSin he
sample sys em.
qL=

−cos η
−sin ηsin α
−sin ηcos α

=

−sin θ
−cos θsin α
−cos θcos α

=⇒qS=

sin ηcos α
sin ηsin α
cos η

=⇒(ψ, ϕ) = (η, α) (7)
[Figu e 1 abou he e.]
We will now conside sample o a ions (ω0, ψ0, ϕ0) defined acco ding o Figu e 1. The
ans o ma ion ma ix be ween he wo e e ence sys ems is hen:
A=

−cos ω0sin ψ0cos ϕ0+ sin ω0sin ϕ0sin ω0sin ψ0cos ϕ0+ cos ω0sin ϕ0−cos ψ0cos ϕ0
−cos ω0sin ψ0sin ϕ0−sin ω0cos ϕ0sin ω0sin ψ0sin ϕ0−cos ω0cos ϕ0−cos ψ0sin ϕ0
−cos ω0cos ψ0sin ω0cos ψ0sin ψ0


(8)
And so we can ans o m he coo dina es by simple ma ix mul iplica ion.
qS=AqL=

a11 a12 a13
a21 a22 a23
a31 a32 a33



−cos η
−sin ηsin α
−sin ηcos α

=

sin ψcos ϕ
sin ψsin ϕ
cos ψ

=

q1
q2
q3

(9)
I is ins uc i e o conside some special cases o sample o a ions (ω0, ψ0, ϕ0) ha lead
o adi ional sca e ing geome ies commonly used in x- ay diff ac ion expe imen s.
2.1 No mal incidence
We conside now he case whe e ω0=ψ0=ϕ0= 0. Now he p ima y x- ay beam is
no mal o he sample su ace, and hus sample and de ec o planes a e pa allel. Now, in
sample coo dina es he sca e ing ec o is simply:
qS=

cos αsin η
sin αsin η
cos η

(10)
And hus we ha e ψ=η, ϕ =α. In his geome y he pola angle ψis fixed and he
azimu hal angle ϕis equi alen o he pola angle along he Debye ing.
2.2 Con en ional θ−θgeome y
In a con en ional θ−θexpe imen , he inciden beam makes an angle θwi h he sample
su ace and i ψ0= 0 he sca e ing ec o is no mal o he sample su ace, oo. This
implies ha ω0=η. In his geome y, he p ima y and sca e ed beam lie in a plane
con aining he sca e ing ec o when ψ= 0. In a wo dimensional ec o , his condi ion
is ulfilled a α=−π/2, and we ge qS= [001].
4
2.3 A bi a y ψ0 il wi h ω0= 0
This is he case mos ele an o ou pu poses, since i desc ibes he geome y in he
po able x- ay s ess measu emen de ice u ilized in his s udy. Now he sca e ing ec-
o in sample coo dina es can be w i en in e ms o sample o a ions and Debye ing
coo dina es as:
qS=

cos ηsin ψ0cos ϕ0+ sin ηcos ψ0cos ϕ0cos α−sin ηsin ϕ0sin α
cos ηsin ψ0sin ϕ0+ sin ηcos ψ0sin ϕ0cos α+ sin ηcos ϕ0sin α
cos ηcos ψ0−sin ηsin ψ0cos α

(11)
We mus emembe ha , in gene al, (ψ, ϕ)= (ψ0, ϕ0), and he ela ionship o pe o m
he ans o ma ion (η, α)→(ψ, ϕ) is a he complex. Two special cases can be desc ibed
a angles α= 0, π, as can be seen in Figu e 2: a α= 0 we ha e ψ=ψ0+η, while a
α=πwe ha e ψ=ψ0−η. This means ha , o his geome y, he poin s in he Debye
ing a α= 0, π can be used di ec ly in he sin2ψme hod once he ηangle is accoun ed
o .
[Figu e 2 abou he e.]
2.4 The cos αme hod
One o he me hods ha allows he calcula ion o s ess om a single measu emen wi h
an a ea de ec o is he cos αme hod desc ibed by Sasaki e al. and o he s [14, 21] and
implemen ed in comme cial ins umen a ion o esidual s ess de e mina ion. The basic
idea is o s a om he exp ession o he sca e ing ec o in sample coo dina es in e ms
o Debye ing coo dina es, in he case o a bi a y ψ0. Fo simplici y we will es ic
ou sel es o he sample-de ec o geome y depic ed in Figu e 1, whe e he incoming x- ay
beam is no mal o he fla 2D de ec o and only a o a ion along S2in sample coo dina es
is allowed. Fo a s ess- ee sample he sca e ing ec o s lie along cones wi h semi-apex
angle η=θ−π/2 o each se o la ice planes ulfilling B agg’s condi ion, p oducing a
se ies o concen ic Debye ings. Fo e e y poin in he de ec o wi h coo dina es (x, y)
qS=

cos ηsin ψ0+ sin ηcos ψ0cos α
cos ηsin ψ0sin ϕ0+ sin ηcos ψ0sin ϕ0cos α+ sin ηcos ϕ0sin α
cos ηcos ψ0−sin ηsin ψ0cos α

(12)
The s ain p ojec ion along (η, α) coo dina es could be w i en in e ms o he sca e -
ing ec o and s ain componen s as ϵα=qiqjϵij. We will assume plane-s ess condi ions
and conside an elas ic, iso opic and homogeneous ma e ial such ha :
ϵij =1 + ν
Eσij −δij
ν
Eσkk (13)
We can subs i u e o find he s ain p ojec ion in e ms o s ess componen s:
ϵα=1 + ν
Eqiqjσij −ν
Eσkk (14)
Now we define pa ame e s a1, a2as:
a1(ϕ0) = 1
2{[ϵ(α)−ϵ(π+α)] + [ϵ(−α)−ϵ(π−α)]}(15)
a2(ϕ0) = 1
2{[ϵ(α)−ϵ(π+α)] −[ϵ(−α)−ϵ(π−α)]}(16)
5

F om he e we can now ob ain:
a1(ϕ0) =1 + ν
Esin 2ψ0sin 2ηcos α[σ11(1 + cos 2ϕ0) + σ22(1 −cos 2ϕ0) + 2σ12 sin 2ϕ0)]
(17)
a2(ϕ0) =1 + ν
Esin ψ0sin 2ηsin α[σ22 sin 2ϕ0−σ11 sin 2ϕ0+ 2σ12 cos 2ϕ0)] (18)
And we now conside he special case o ϕ0= 0 o ge :
a1(ϕ0= 0) = 1 + ν
Eσ11 sin 2ψ0sin 2ηcos α(19)
a2(ϕ0= 0) = 21 + ν
Eσ12 sin ψ0sin 2ηsin α(20)
So by plo ing he pa ame e s a1, a2as a unc ion o cos αand sin αwe ob ain wo
linea ela ionships, he slopes o which will be p opo ional o σ11 and σ12, espec i ely.
2.5 Full Debye ing fi ing
Fo simplici y, le us con inue assuming ha ω0= 0, so he sca e ing ec o can s ill be
w i en as:
qS=

cos ηsin ψ0cos ϕ0+ sin ηcos ψ0cos ϕ0cos α−sin ηsin ϕ0sin α
cos ηsin ψ0sin ϕ0+ sin ηcos ψ0sin ϕ0cos α+ sin ηcos ϕ0sin α
cos ηcos ψ0−sin ηsin ψ0cos α

(21)
As we ha e seen, he e is a linea ela ionship be ween he expe imen ally de e mined
s ain p ojec ion ϵαand he s ain componen s in he sample coo dina es ϵij, whe e he
linea coefficien s qia e simply he componen s o he sca e ing ec o , meaning ha :
ϵα=qiqjϵij (22)
Now he qi’s depend only on sample geome y pa ame e s and Debye coo dina es
ψ0, ϕ0, η, α and a e hus known, so equa ion (22) ep esen s a se o linea equa ions o
each pola angle αa which he s ain is de e mined. The ou unknowns a e he ϵij (in
plane s ess ϵ13 =ϵ23 = 0) and he independen e ms ϵαa e de e mined expe imen ally.
Since he numbe o α alues p obed is mo e han ou ( ypically 360 a leas ), he sys em
is o e de e mined and can be nume ically sol ed in he leas -squa es sense.
Expe imen ally, he Debye ing is fi ed o ob ain 2θ(α) and hen he s ain is calcula ed
using:
ϵα= ln (sin θ0
sin θ(α))(23)
2.6 Effec o diff ac ion olume
Fo diff ac ion o occu , he inciden and diff ac ing beam ec o s and he no mal o he
diff ac ing planes mus be co-plana , wi h he no mal o he diff ac ing planes making equal
angles wi h he wo wa e ec o s. Consequen ly dis inc g oups o g ains, wi h pa allel
diff ac ing plane no mals, con ibu e o he diff ac ion p ofiles ob ained a he a ious
ψ, ϕ, η, α coo dina es. We define he o al olume o such a se o g ains as he in o ma ion
6
olume o hese angula coo dina es. All o mula ions discussed abo e o compu ing he
s esses om diff ac ion da a assume ha he same quasi-homogeneous bi-axial s ess
enso exis s wi hin all diff ac ing olumes sampled by all echniques. This is no a s ong
assump ion and mus be e ified expe imen ally on a case-by-case basis. Fo example,
his assump ion is jus ified in sho -peened samples whe e, because o he andom plas ic
de o ma ion field caused by mul iple impac s, any p e-exis ing c ys allog aphic ex u e is
des oyed in he peened laye , and he same mac os ess dis ibu ion is ob ained om all
eflec ions and all accessible ψ il s o a gi en eflec ion. Howe e , his is no he case o
samples plas ically de o med in uniaxial ension [8]. In such cases, he esul s om he
h ee o mula ions migh no ag ee.
3 Ma e ials and Me hods
3.1 Expe imen al se up
A minia u e po able 2D x- ay appa a us (Puls ec µ-X360, Puls ec Co p., Japan) was used
o de e mine esidual s esses in ca bon s eel ubula samples as a unc ion o applied load.
This appa a us has been desc ibed elsewhe e [10]; in b ie , i consis s o a low in ensi y
C Kαsou ce wi h a fil e and an image pla e 30 mm in adius posi ioned no mal o he
inciden beam. Unde hese condi ions, back-diff ac ed beams om he sample su ace
a e cap u ed by he image pla e a 50 µm esolu ion. Beam spo size is app oxima ely 2
mm o he de aul 1 mm pinhole collima o , and angula co e age o a 40 mm sample o
de ec o dis ance is 2θ= 145◦−175◦.
An Ins on 5984 Uni e sal Tes ing Machine was used o apply a ensile load o he
specimens ia pneuma ic g ips. The machine was ope a ed in load con ol and s ain was
eco ded using a clip-on ex ensome e . Nominal loads co esponding o s esses in he
ange o 0 - 275 MPa we e applied in 25 MPa inc emen s, and a each load one x- ay
diff ac ion pa e n was acqui ed. Once a a ge load was eached i was held o he o al
du a ion o he x- ay measu emen , which in ou case amoun ed o 40 s o exposu e plus
50 s o image pla e eadou and p ocessing ime.
3.2 Samples
Samples s udied in his wo k we e seamless ubes 25.4 mm in diame e and wi h a wall
hickness o 1.24 mm, con o ming o ASTM 179 and SAE J524 s anda ds. The ube
ma e ial was e y low ca bon s eel con o ming o AISI 1010 specifica ions, which was cold
d awn and hea ea ed a 650 oC. The mic os uc u e o his ma e ial is p esen ed in
Figu e 3: as expec ed om he composi ion, i consis ed o p ima y e i e wi h small,
isola ed islands o pea li e. Fe i e g ain size was de e mined o be (12 ±2)µm by he line
in e cep me hod.
Samples we e checked o ex u e and phase composi ion by using a labo a o y diff ac-
ome e using Cu- adia ion wi h a g aphi e monoch oma o (figu e S1 o he supplemen-
a y in o ma ion): no significan ex u e was de ec ed (see figu e S2). Due o he e y
low cemen i e con en , no Fe3C peaks we e obse ed. The use o ubula samples in o-
duced an addi ional se o alignmen difficul ies, when compa ed wi h he mo e ypical
fla specimens, ha we e in ou opinion mo e ep esen a i e o ac ual applica ions whe e
complex geome ies, igh space cons ain s and alignmen difficul ies a e o be expec ed
(see Figu e S3 in he supplemen a y in o ma ion o ac ual pic u es o he se up).
[Figu e 3 abou he e.]
7
3.3 Da a analysis and s ess calcula ion
In e nal so wa e supplied by he x- ay appa a us was used o compu e de ec o pa ame e s
(beam cen e and sample- o-de ec o dis ances) a ze o ex e nal load. This app oach
e e ed all subsequen measu emen s o his da um and ensu ed ha , as long as he
applied load s ayed below he elas ic limi (and, consequen ly, did no change any ini ial
esidual s esses), subsequen x- ay analysis would only yield he (uniaxial) applied s ess
alues. Nominal de ec o - o-sample dis ances we e in he 35-50 mm ange, which esul ed
in only one Debye ing, om he (211) eflec ion o he BCC e i e phase, being eco ded.
We used a = 2.8664 ˚
A as he uns essed la ice pa ame e a ze o load o calcula ing he
sample o de ec o dis ance.
De ec o il and/o dis o ion we e de e mined by fi ing he Debye ing o an ellipse
using he hypo hesis ha , o a esidual s ess- ee sample in he absence o applied load,
any ellip ici y in he Debye ing mus be due o de ec o o a ion. Since a de ia o ic s ain
enso would also esul in a de o med, ellip ical Debye ing, we fi ed he ings ob ained
a ze o applied s ess using he ull- ing p ocedu e desc ibed p e iously and ob ained a
‘fic i ious s ain’ ( he s ain s a e ha would esul in he same de o ma ion o he Debye
ing as obse ed due o de ec o il ) ha was used o co ec subsequen ly de e mined
s ains unde load.
Fo all s ess calcula ions, he x- ay elas ic cons an , 1+ν
E, was aken o be 5.71 TPa-1.
This alue was compu ed om he quasi-iso opic elas ic pa ame e s o e i e, E=
224 GPa and ν= 0.28 . U iliza ion o Nee eld-Hill o K oene x- ay elas ic cons an s, com-
pu ed om single-c ys al compliances o he (211) e i e eflec ion ( 5.94 and 6.21 TPa-1,
espec i ely) would ha e uni o mly shi ed all calcula ed s ess alues by app oxima ely
4% and 8% . Since he e m 1+ν
Eis a mul iplie in all h ee o malisms, compa ing he
equi alency o hei s ess ou pu is independen o he selec ion o elas ic cons an s.
Two se s o da a we e acqui ed o each o he h ee diffe en beam incidence angles
s udied, a ψ0= 0◦,35◦,45◦. This allowed us o s udy he effec o beam incidence angles
on s ess calcula ion, and also o ob ain a se o s ain alues a diffe en ψso as o be
able o use he sin2ψme hod o compa ison. Nominal ψ alues s udied we e 11.8, 23.2,
33.2, 46.8 and 56.8o; addi ionally he ex ensome e p o ided he s ain a ψ= 90◦.
A code sol ing equa ion (22) in he leas squa es sense was implemen ed in MATLAB.
A sligh modifica ion o he fi ing equa ion was pe o med so he a ia ion o sca e -
ing angle θ(α) wi h he pola coo dina e was pe o med di ec ly wi hou equi ing he
specifica ion o a s ess- ee e e ence angle θ0:
ln (sin θ(α)) = ln(sin θ0)−qiqjϵij (24)
This has he ad an age ha he s ess- ee angle θ0is now he independen e m and
can hus be ob ained as pa o he leas -squa es fi . The p e ious equa ion is, in heo y,
alid o he gene al case o a iaxial s ess s a e, howe e some simplifica ions can be
in oduced o plane s ess condi ions, namely ϵ13 =ϵ23 = 0 and ϵ33 =−ν(ϵ11 +ϵ22),
whe e νis he Poisson’s a io o he ma e ial.
The p oduced code was es ed by gene a ing syn he ic da a se s, adding no mal noise
and hen fi ing he esul ing da a o ob ain he s ess componen s and compa e wi h he
ini ial alues. Addi ionally, he impac o e o s in he de e mina ion o some o he inpu
pa ame e s (sample o a ion) in he final s ess esul was assessed by means o hese
simula ions.
8
4 Resul s and Discussion
Figu e 4 shows he aw in o ma ion om he image pla e, showing some spo iness o he
Debye ing, also e idenced in he a ia ion o he (211) Fe peak a ea along he Debye ing
and, o a lesse ex en , in he change in FWHM o he peak. The e a e also a ia ions in
he expe imen al 2θ s αp ofiles as can be seen in figu e 5, which shows he 2θposi ion o
he peaks as a unc ion o α, along he Debye ing, o es s pe o med a ψ0= 35◦,45◦.
The measu ed p ofiles exhibi sligh sys ema ic undula ions a ound he expec ed alues:
hese ‘undula ions’ a e along he αangle and a e no ela ed o he well-known oscilla ions
in sin2ψ[22–26], bu a e due o he (p op ie a y) pixel in ensi y-da a analysis algo i hm
in his pa icula machine; hese algo i hms a e inaccessible o he use s. We also obse ed
hese undula ions in da a measu ed om he calib a ion powde s (annealed e i e powde
wi h g ain size a ound 1 µm) supplied by he sys em manu ac u e [10]. Peak a ea plo s
as a unc ion o azimu hal angle (Figu e 4, lowe le panel) we e uni o m and allowed us
o discoun effec s o c ys allog aphic ex u e.
[Figu e 4 abou he e.]
[Figu e 5 abou he e.]
As we saw in sec ion 2.3 (and Figu e 2), a single exposu e ha co e s he whole Debye
ing also allows o he de e mina ion o s ess using he sin2ψme hod, al hough only
using he wo poin s ha co espond o ϕ= 0, namely hose a α= 0,180◦. In his
case he in o ma ion olume o he wo- il sin2ψme hod is a subse o he in o ma ion
olume o he Debye ing analysis. In ligh o his ac , we used diff ac ion da a om a
single exposu e o calcula e he a e age axial s ess and s anda d de ia ion using bo h a ea
de ec o -based single exposu e echniques, and he wo- il sin2ψme hod. This app oach
somewha alle ia ed he sampling issues a ising om he use o mul iple ψ il s, wi h
comple ely independen in o ma ion olumes. A compa ison be ween he sin2ψand he
ull Debye ing me hod can be seen in Figu e 5: in addi ion o expe imen al Debye ing
p ofiles a diffe en s esses, we plo simula ed Debye ings whe e he inpu s esses alue
is ob ained om he sin2ψme hod. Reasonable ag eemen is obse ed.
Figu e 6 shows axial (σxx) s esses calcula ed using single exposu e me hods (ei he
leas squa es fi ing o he en i e Debye ing o cos α) agains s esses calcula ed using
he con en ional ( wo- il ) sin2ψapp oach. Black symbols ep esen a e ages o e ou
measu emen s a ψ0= 35,45◦and e o ba s ep esen ±one s anda d de ia ion. Fo
comple eness, indi idual measu emen s a e plo ed as well, using ed symbols (hollow o
ψ0= 35◦and filled o ψ0= 45◦). The dashed line, wi h slope o 1, deno es he locus o
iden ical alues. The ollowing obse a ions can be made:
1-The p ecision o ‘ eal’ esidual s ess measu emen s on an engine ing sample, ob-
ained unde condi ions which a e simila o hose encoun e ed du ing ypical field p ac-
ice, is wo se, by an o de o magni ude, han he alues quo ed o ‘ideal’ samples, i.e,
±20 s. ±2 MPa. This is consis en wi h pas esidual-s ess measu emen p ac ice using
labo a o y and field ins umen s. We again no e ha he sca e in he measu ed da a in
his figu e is ela ed o he p ecision (no accu acy) o he pa icula sys em (ins umen ,
sample, measu emen condi ions).
2-The s ess alues ob ained om bo h a ea-de ec o based single exposu e echniques
a e, wi hin e o , equal o he wo- il sin2ψ o mula ion o applied s esses in he elas ic
ange (Figu e 7). Fo highe applied s esses we obse e a sys ema ic de ia ion o he
s esses measu ed by he single exposu e echniques om he dashed line deno ing 1- o-
1 co espondence wi h he wo- il sin2ψ o mula ion. As no ed be o e, his de ia ion
9
In e sec ion o he
cone o no mals
X- ay beam
Figu e 2: S e eog aphic p ojec ion sample coo dina es (S1, S2, S3) o he case o sample
o a ions wi h ω0=ϕ0= 0. In his case he sca e ing ec o s laying a α= 0, π
co espond o angles ψ=ψ0±ηin sample coo dina es.
16

Figu e 3: Mic os uc u e o he 1010 ca bon s eel samples s udied in his wo k: op ical
mic oscopy (le ) and scanning elec on mic oscopy ( igh ).
17
Figu e 4: Raw da a om he image pla e a ze o applied s ess, o he case o ψ0= 35◦.
Top: no malized diff ac ion in ensi y as a unc ion o 2θand α. Bo om-le : peak a ea
along he Debye ing. Bo om- igh : peak whm along he Debye ing.
18
0 60 120 180 240 300 360
156.1
156.2
156.3
156.4
156.5
0 60 120 180 240 300 360
156.0
156.1
156.2
156.3
156.4
25 MPa
50 MPa
75 MPa
10 0 MPa
12 5 MPa
15 0 MPa
17 5 MPa
20 0 MPa
22 5 MPa
25 0 MPa
27 5 MPa
2 (º)
(º)
0
= 35 º
0
= 45 º
2 (º)
(º)
Figu e 5: Debye ing adius (2θ) as a unc ion o azimu hal angle α o he e i e (211)
eflec ion, a diffe en loads. Symbols co espond o expe imen al da a while solid lines
a e calcula ed Debye ing p ofiles using he s ess ob ained om he sin2ψme hod.
19
0 50 100 150 200 250
0
50
100
150
200
250
35º 45º
cos
ull-2d
cos a e age
Full-2d a e age
Full-2d o cos measu ed s ess (MPa)
sin
2
measu ed s ess (MPa)
Figu e 6: S esses calcula ed om single exposu es ( ull-2d, cos α s sin2ψs ess. Black
symbols ep esen a e ages o e ou measu emen s a ψ0= 35,45◦and e o ba s ep e-
sen one s anda d de ia ion. Red symbols (hollow o ψ0= 35◦and filled o ψ0= 45◦)
co espond o indi idual measu emen s.
20
0.0000 0.0004 0.0008 0.0012 0.0016
0
50
100
150
200
250
300
350
S ess (MPa)
T ue S ain
Load cell
Ex apola ed elas ic s ess
0
10
20
30
40
(MPa)
210 GPa
Figu e 7: Uniaxial ensile es da a o he 1010 s eel ube sample used in he s udy. The
ex apola ed elas ic s ess line is calcula ed om leas -squa es fi ing o he 0-50 MPa load
ange, which yielded 210 GPa as he (effec i e) Young’s Modulus. The ∆σ alues ( igh
o dina e) show he diffe ence be ween he ex apola ed elas ic s ess and he ac ual load
cell ou pu .
21

155.5
156
156.5
157
30
210
60
240
90 270
120
300
150
330
180
0
0100 200 300
155.9
156
156.1
156.2
156.3
156.4
156.5
α(º)
2θ (º)
ǻ(2ș)=0.1º
155
156
157
158
30
210
60
240
90 270
120
300
150
330
180
0
0 100 200 300
156.05
156.1
156.15
156.2
156.25
156.3
156.35
156.4
α(º)
2θ (º)
ǻ(2ș)=0.01º
Figu e 8: Simula ed Debye ings and fi ing esul s o he ull- ing fi ing me hod, a e
adding gaussian noise.
22
10-3 10-2 10-1
10-2
10-1
100
101
102
103
-4 -2 0 2 4
-50
-25
0
25
50
75
100
125
150
∆σxx
∆σxy
∆σyy
∆σij
(MPa)
∆(2θ) (deg ees)
∆σyy
Calcula ed
σij
(MPa)
∆ψ0(deg ees)
ψ0=15º
ψ0=30º
ψ0=45º
∆σxx
Figu e 9: Top: E o in he de e mina ion o s ess as a unc ion o e o in 2θ(as one
s anda d de ia ion). The hollow symbols a e o he ull- ing fi ing me hod while he
filled symbols a e o he cos α. Bo om: s ess calcula ed as a unc ion o e o in sample
o ien a ion (see ex o de ails), o a uniaxial s ess s a e wi h σxx = 100MPa and o
diffe en ψ0 alues.
23