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De elopmen o he in e nal s uc u e o an alkali-ac i a ed
pas e ela ed o he leng h o cu ing
D Kocáb1, V Bílek2, N Náp a ník1 and B Kucha czyko á1
1B no Uni e si y o Technology, Facul y o Ci il Enginee ing, Ve eří 331/95, B no,
Czech Republic
2B no Uni e si y o Technology, Facul y o Chemis y, Pu kyňo a 464/118, B no,
Czech Republic
E-mail: dalibo .kocab@ u b .cz
Abs ac . This pape deals wi h he in luence o he leng h o he mois cu ing pe iod on he
de elopmen o he in e nal s uc u e o a pas e based on alkali-ac i a ed slag. Wa e glass was
used as he ac i a o . Fo he pu pose o expe imen , he es specimens subjec ed o he
expe imen we e di ided in o i e se s wi h di e en cu ing egimes combining mois and ai
cu ing. The e e ence se was kep in an en i onmen wi h ela i e ai humidi y ≥ 95% du ing
he en i e ma u ing pe iod. The de elopmen o he in e nal s uc u e o he alkali-ac i a ed pas e
was mainly moni o ed using he esonance me hod. The ob ained esul s show ha he cu ing
egime applied o he es specimens signi ican ly in luences he de elopmen o he in e nal
s uc u e o he ma e ial. The de elopmen o he obse ed dynamic p ope ies (dynamic moduli
and Poisson’s a io) shows he o ma ion o damage o he in e nal s uc u e o he pas e a e i s
exposu e o he ai . In e es ingly, a massi e dec ease in dynamic modulus o elas ici y
immedia ely a e exposu e o ai d ying was no p e en ed, e en by in ensi e mois cu ing
o he pas e o 28 days.
1. In oduc ion
Many yea s ago, high CO2 emissions ha accompany he p oduc ion o Po land cemen igge ed
a su ge o in e es in al e na i e ino ganic binde s. Today, his end is gaining momen um. One o he
mos common binde s ha a e an al e na i e o cemen is alkali-ac i a ed slag (AAS). The p esence
o a high alkaline ac i a o in his binde induces he eac ion o he g ound g anula ed blas u nace
slag. Apa om he ob ious en i onmen al aspec , he main ad an ages o AAS ma e ials include
esis ance o agg essi e en i onmen s [1,2] and high empe a u es [3] o a apid inc ease in s eng h [4].
On he o he hand, one o he bigges disad an ages o AAS is undoub edly i s suscep ibili y o ela i ely
subs an ial olume changes. Sh inkage is accompanied by c ack o ma ion, which limi s he wide use
o AAS-based ma e ials in p ac ical applica ions. I should also be no ed ha he esul ing p ope ies
o hese ma e ials s ongly depend on he ype o he employed ac i a o , i s concen a ion, he ela i e
a io o he p ecu so o he ac i a o solu ion, o he ma u ing condi ions. Commonly used alkaline
ac i a o s include hyd oxides, silica es and o he sal s o alkali me als (mos o en sodium). The ype
o he gi en ac i a o signi ican ly in luences he hyd a ion p ocess o AAS ma e ials, which in u n
a ec s hei esul ing physical and mechanical p ope ies. Wa e glass ac i a ion, o example, can esul
in high comp essi e s eng hs and e y good wo kabili y [5], bu is a isk o massi e au ogenous
sh inkage [6] and d ying sh inkage, which is usually accompanied by c ack o ma ion. The use
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o sodium hyd oxide, on he o he hand, usually p o ides high ini ial comp essi e s eng hs due o he
high a e o hyd a ion bu does no lead o signi ican s eng h inc ease in he subsequen ma u ing
p ocess when compa ed o o he ac i a o s. A slow dec ease in capilla y po osi y has been iden i ied as
one o he main easons o ha [5,7].
Ma e ials based on ino ganic binde s can unde go di e en s ages o deg ada ion du ing hei
li e ime, which is e lec ed in he quali y o hei mic os uc u e. The s a e o a mic os uc u e in e ms
o size and dis ibu ion o po es o he deg ee o c acking damage can be desc ibed, o example, by
mic oscopic me hods, compu e omog aphy o me cu y po osime y [8,9]. Howe e , all he cases a e,
in a way, des uc i e es me hods ha equi e ela i ely demanding sample p epa a ion. I a mic opo e
analysis is equi ed, he samples mus o en be ex ac ed om la ge es specimens o di ec ly om
building elemen s. In mos cases, he size o he ex ac ed sample is incompa ably smalle han he size
o he o iginal es ed elemen , and he e o e makes i almos impossible o comp ehensi ely desc ibe he
dis ibu ion o po es o he deg ee o damage o he gi en ma e ial in i s en i e olume. The use
o non-des uc i e es ing me hods (NDT) he e o e seems only app op ia e since hey a e sensi i e o
he p esence o local damage and c acks. These me hods include, o example, he ul asonic pulse
eloci y me hod and he esonance me hod. In his case, he de elopmen o deg ee o damage o he
in e nal s uc u e can easily be moni o ed using he change in he dynamic modulus o elas ici y, he
so-called ela i e moduli o elas ici y (RDM). In p inciple, he assessmen can be iden ical o
eeze- haw esis ance es ing o conc e e ma e ials acco ding o ASTM C666/C666M-15 [10] o
CEN/TR 15177 [11]. The ela i e dynamic modulus can be de e mined using bo h o he
abo e-men ioned NDT me hods, howe e , he esonance me hod p o ed o be much mo e sui able o
his pu pose. This is because i is mo e sensi i e o damage o he in e nal s uc u e and shows a highe
dec ease in RDM han he ul asonic pulse eloci y me hod [12]. The ad an age o he esonance me hod
is no only i s non-des uc i e cha ac e , which allows epea ed measu emen s on he same specimen
o e any equi ed ime ange, he eby educing he demands on he numbe o es specimens, bu i also
allows calcula ions o se e al dynamic p ope ies o he examined ma e ial simul aneously. In addi ion
o he dynamic Young’s modulus, which can be calcula ed om he na u al equency o longi udinal
and ans e se ib a ions, he dynamic shea modulus and he dynamic alue o Poisson’s a io can also
be de e mined [13]. This o e s a be e desc ip ion o he de elopmen o he in e nal s uc u e o he
ma e ial, bo h om he poin o iew o i s ma u ing and om he poin o iew o damage due o
deg ada ion mechanisms.
The main objec i e o he pe o med expe imen is o employ he esonance me hod as
a non-des uc i e es ing me hod o moni o ing he ma u a ion p ocess om he specimens’
manu ac u ing up o long- e m ageing, as he me hod is sensi i e o local damage and mic o-c acks. The
a e o in e nal de e io a ion is exp essed h ough he changes in he na u al equencies measu ed in
egula in e als on he same se o specimens du ing he whole ime o ageing. This app oach p omises
an e ec i e ool o p omp mic o-c acking and in e nal de e io a ion e i ica ion wi hou demanding
mic oscopic analysis. Especially, he ob ained dynamic Poisson’s a io could gi e a good idea abou he
end o inne de e io a ion.
2. Expe imen
Fi e se s o alkali-ac i a ed slag es specimens we e p oduced o his expe imen . The slag was
ac i a ed wi h wa e glass. The main moni o ed pa ame e s we e he de elopmen o he esonan
equencies o he es specimens and subsequen ly calcula ed RDM and Poisson’s a io. These
pa ame e s we e moni o ed as a unc ion o age and he me hod o es specimens cu ing du ing hei
ma u ing.
2.1. Ma e ial
G ound g anula ed blas u nace slag (LB Cemix, s. .o.) wi h he majo i y o he amo phous phase was
used. I s Blaine speci ic su ace a ea was 400 m2/kg. The slag was ac i a ed by he wa e glass solu ion
wi h a silica e modulus o 1.5 and a Na+ concen a ion o 4M. The olume ac ion o he slag in he
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pas e was 0.52. The inal ac i a ing solu ion was p epa ed a ew days in ad ance by mixing o he aw
wa e glass wi h a silica e modulus o 1.9 and d y ma e o 47.9% (Vodní sklo, a.s.) wi h 50% sodium
hyd oxide solu ion (Ca l Ro h GmbH + Co. KG) and wi h demine alized wa e . The pas e was mixed
using a Hoba mixe o 3 minu es, wi h he slag being added e enly in o he p e-weighed ac i a o
du ing he i s 50 seconds. A e mixing, he consis ency o he pas e was de e mined using he low
able es acco ding o s anda d [14] and he densi y acco ding o s anda d [15]. The diame e o he
pou ed pas e a e li ing he cone was 178 mm and 217 mm a e i een jol s. The densi y o he esh
pas e was 2080 kg/m3. Th ee gang s eel molds we e used in he p oduc ion o he es specimens
o nominal dimensions 40×40×160 mm. The molds we e illed in wo laye s and each laye was
compac ed using a high equency ib a ing able o 3 seconds. The desc ibed expe imen in ol ed
i een es specimens, which we e di ided in o 5 se s. Ma u ing du ing he i s 24 hou s occu ed in he
molds co e ed wi h PE oil unde labo a o y condi ions a a empe a u e o (22±2)°C. The cu ing me hod
o he es specimens o he indi idual se s a e hei emo al om he molds was as ollows:
• REF – always s o ed in an en i onmen wi h ela i e humidi y (RH) ≥ 95% (excep o he
es ing pe iod),
• 24H – d ying in he ai immedia ely a e demolding,
• 48H – addi ional 24 hou s unde RH ≥ 95%, hen d ying in he ai ,
• 7D – addi ional 6 days unde RH ≥ 95%, hen d ying in he ai ,
• 28D – addi ional 27 days unde RH ≥ 95%, hen d ying in he ai .
2.2. Tes me hods
The na u al equencies o ib a ion we e measu ed a egula in e als on all es specimens – in he
case o he e e ence se con inually, in he case o he o he se s only a e exposu e o he specimens
o d ying in he ai . The i s measu emen on he e e ence se was conduc ed immedia ely a e
demolding, and he es specimens we e hen placed in a chambe wi h a ela i e humidi y ≥ 95%.
Sho ly be o e each subsequen measu emen , he es specimens we e emo ed and su ace-d ied, hei
mass and na u al equency o ib a ion we e de e mined, and he specimens we e hen immedia ely
e u ned o he chambe . The second se o 24H was measu ed in an analogous way, wi h he only
di e ence being he ac ha he specimens we e le o d y in he ai a e he i s measu emen . The
es specimens o he o he se s 48H, 7D and 28D we e demolded and placed in he chambe wi h
a ela i e humidi y ≥ 95%, and he i s measu emen was conduc ed only a e hey we e emo ed om
he chambe o he i s ime and exposed o d ying in he ai – i.e. a he age o 48 hou s, 7 days,
espec i ely 28 days. The measu emen s we e conduc ed un il he pas e eached he age o 120 days.
The ai d ying was pe o med in an ai -condi ioned labo a o y a a empe a u e o (22±2)°C and
RH (55±5)%.
A each measu emen in e al, he mass o he es specimen was de e mined oge he wi h he i s
na u al equency o longi udinal L, ans e se and o sional ib a ion . The de e mina ion o he
na u al equencies was conduc ed using an impac hamme (exci e ), an accele a ion senso (senso ),
an oscilloscope and e alua ion so wa e, which wo ks on he p inciple o as Fou ie ans o ma ion
(see igu e 1). The measu emen o he na u al equencies o he es specimens and de e mina ion o
dynamic p ope ies (Young’s modulus E L and E , shea modulus G and Poisson’s a io ν ) was
conduc ed in acco dance wi h s anda d [13]. Subsequen ly, RDM was calcula ed using he measu ed
equencies acco ding o he p ocedu e in [10]. The alues o he na u al equencies o he e e ence se
REF, acqui ed du ing he i s measu emen a e demolding a he age o 24 hou s, we e conside ed as
e e ence alues o he calcula ion o RDM(L), RDM(F) and RDM(T) o all es se s. The ela i e
modulus o elas ici y was de e mined acco ding o he equa ion:
𝑅𝐷𝑀𝑖=𝑓
𝑖2
𝑓
0
2∙100, (1)
whe e RDMi is he ela i e dynamic modulus o elas ici y o he i- h measu emen , i is he a e age
na u al equency o he specimens in a se a he i- h measu emen and 0 is he a e age equency
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o he es specimens o he REF se a he i s measu emen a e demolding. RDM is he e o e no
calcula ed o indi idual es specimens, bu o en i e se s. This me hod was selec ed o allow
compa isons be ween indi idual se s. The measu emen was ini ia ed a di e en ages o each se ,
he e o e he e is no eason o ela e RDM o he i s measu emen o he indi idual specimens. The
measu ed na u al equencies o he es specimens a e demolding (se s REF and 24H) exhibi ed such
low a iabili y ha i is possible o conside he a e age na u al equencies o he REF se as he i s
0 measu emen o all o he se s wi hou signi ican s a is ical e o .
Mass change, howe e , was de e mined o all specimens sepa a ely acco ding o he equa ion:
∆𝑚𝑖=𝑚𝑖−𝑚0
𝑚0∙100, (2)
whe e Δmi is he ela i e change in mass o he i- h measu emen , mi is he specimen mass a he
i- h measu emen and m0 is he specimen mass a i s i s measu emen . The esul ing mass change
Δm is de e mined o each se a each measu emen as he a e age alue o he indi idual mass changes
o h ee es specimens in a se .
Figu e 1. Dis ibu ion o senso s (S) and exci e s (E) o he de e mina ion o he i s na u al
equencies (le ), illus a i e pho o o he de e mina ion o he i s na u al equency
o longi udinal ib a ion ( igh ).
3. Resul s and discussion
The de e mined Young’s moduli, shea modulus, Poisson’s a io and mass changes a e p esen ed in he
ollowing igu es as a i hme ic means o h ee independen measu emen s conduc ed on he specimens
o each es se . Va iabili y o he measu emen esul s, exp essed wi h he sample s anda d de ia ion, is
shown in he g aphs using e o ba s.
Figu e 2 p esen s he de elopmen o he dynamic moduli o elas ici y E L and E . Figu e 3 shows
he de elopmen o he dynamic shea modulus G and he dynamic Poisson’s a io ν . In he case o he
REF se , a g adual inc ease o all h ee de e mined dynamic moduli o elas ici y can be obse ed
h oughou he en i e measu emen pe iod up o 120 days o age, which co esponds o he no mal
de elopmen o mechanical p ope ies o conc e e ma e ials du ing ma u ing a high ela i e humidi y
[16,17].
Howe e , his is no he case o he se s whose specimens we e exposed o d ying in ai a a ce ain
age. The AAS pas e ha was le wi hou cu ing immedia ely a e demolding (24H se ) exhibi s
an inc ease in dynamic elas ic moduli up o 21 days o age, wi h he inc ease being lowe han ha o
he REF se . A e he 21s day o age, he e is a g adual dec ease in Young’s modulus, which was
de e mined using he na u al equency o longi udinal and ans e se ib a ions. The dynamic shea
modulus does nei he dec ease no inc ease signi ican ly – a pe sis en s agna ion has been eco ded
om he age o 21 days. A i s glance, i may seem ha he pas e wi hou cu ing ma u es in a s anda d
manne only a a slowe a e when compa ed o cu ed specimens. In his case, howe e , he imp o emen
in he quali y o he in e nal s uc u e o he pas e is only supe icial since i al eady exhibi s c ack
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o ma ion. This is e y well illus a ed by he de elopmen o he dynamic Poisson’s a io. Fo he
e e ence se , he alue o he Poisson’s a io a he age o 3 days is 0.30, hen i g adually dec eases o
he alue o 0.25 a he age o 21 days and emains cons an he eina e . In he case o he 24H se , he
alue o he Poisson’s a io a he age o 3 days is only 0.15, which is alid un il he age o 21 days,
howe e , i hen exhibi s a sha p dec ease o an un ealis ic alue o -0.20. O cou se, his does no mean
ha he AAS pas e will become an auxe ic ma e ial wi hou cu ing. This only indica es a s a e when he
in e nal s uc u e o he es ed ma e ial is so damaged (in his case by c acks om d ying sh inkage) ha
he heo e ical ela ionships o he na u al equencies o he indi idual ib a ion modes cease o apply.
Figu e 2. De elopmen o he dynamic Young’s modulus, de e mined using longi udinal ib a ion
E L (le ) and ans e se ib a ion E ( igh ).
Figu e 3. De elopmen o he dynamic shea modulus G (le ) and Poisson’s a io ν ( igh ).
All es specimens ha we e cu ed o a leas 1 day unde he en i onmen wi h RH ≥ 95% beha e
essen ially iden ically a e exposu e o he ai d ying. A he same ime, hei beha iou is en i ely he
opposi e o REF and 24H. A e emo al om he en i onmen wi h RH ≥ 95%, all dynamic modulus
alues immedia ely (wi hin 24 hou s) dec ease sha ply, up o 70% o he o iginal alue de e mined
immedia ely a e emo al om he humid chambe . A e his ex eme dec ease in he alues o he
dynamic moduli o elas ici y, he e is a slow g adual inc ease, howe e , he in e nal s uc u e o he AAS
pas e has al eady been i e e sibly damaged. The damage is e y well illus a ed (especially o he 48H
and 7D se s) by he de elopmen o he Poisson’s a io, which immedia ely inc eases o un ealis ic
alues exceeding 0.5. In he case o he 28D se , he Poisson’s a io does all wi hin ealis ic limi s, bu

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he luc ua ions du ing he i s 14 days a e exposu e o he specimens o he ai d ying indica e issues
in he in e nal s uc u e o he pas e.
The ex eme dec ease in he dynamic modulus o elas ici y o he cu ed se s (48H, 7D and 28D) a e
he end o cu ing is pa ly caused by a massi e mass loss o he AAS pas e (see igu e 4), since mass is
inco po a ed in he calcula ion o he modulus o elas ici y. The g aph in igu e 4 e eals ha he la e
cu ing inishes, he smalle he mass loss, which can be a ibu ed o wa e binding in he hyd a ion
p oduc s du ing ongoing hyd a ion. Simul aneously, he mass o all he se s somewha s abilizes a e
28 days o d ying. I is also impo an o no e ha he impac o mass loss on he dec ease in modulus
o elas ici y is no signi ican . All he es ed cu ed specimens exhibi ed a signi ican dec ease in RDM
(see igu e 5), al hough his is ma hema ically independen o he mass o he es specimens, see
equa ion (1).
Figu e 4. A e age mass change o he es
specimens o indi idual se s a e he s a o he
measu emen o na u al equencies.
Figu e 5. Rela i e dynamic modulus de e mined om he na u al equency
o longi udinal (le ), ans e se (middle) and o sional ib a ions ( igh ).
When using wa e glass as an ac i a o , he p oduced pas es a e damaged by sh inkage c acks always
a e cu ing has been e mina ed, ega dless o he leng h o he cu ing pe iod. I cu ing las ed o a leas
48 hou s, he c acks become qui e p onounced a e he end o he cu ing pe iod, see igu e 6. When he
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AAS ge exposed o d ying in he ai only a e 28 days o cu ing, a dec ease in he dynamic modulus
o elas ici y o 50% (G ) o up o 30% (E ) o he o iginal alue was eco ded in jus 24 hou s.
The di e en beha iou o he specimens exposed o d ying immedia ely a he age o 24 hou s
compa ed o all o he cu ing in e als unde speci ic humidi y is closely ela ed o di e en s ages
o hyd a ion, i.e. o di e ences in he mic os uc u e, especially in e ms o he ineness o i s po osi y.
I has been obse ed [18] ha a simila AAS pas e, only wi h a sligh ly lowe olume ac ion o slag
(0.52 s 0.50) and a a sligh ly highe empe a u e (25°C), exhibi ed he maximum o he main hyd a ion
peak on he calo ime ic cu e a e app oxima ely 24 hou s. I we conside he s ong dependence
o he a e o alkali-ac i a ion o he slag on empe a u e [19,20], his s udy can assume ha he main
calo ime ic peak will appea a li le la e . This peak is ela ed o a massi e o ma ion o hyd a ion
p oduc s, which p oduces ine mic os uc u e and a he same ime signi ican ly inc eases mechanical
p ope ies [21]. This means ha he mic os uc u e o he specimens om he 24H se was undamen ally
di e en om he mic os uc u e o all he o he se s o he es specimens exposed o d ying a e
a longe cu ing pe iod. As a esul , signi ican ly coa se po osi y can be expec ed, and he e o e smalle
o ces leading o sh inkage [22,23] bu a he same ime a smalle s ess concen a ion in he pas e sample
due o i s low s i ness/lowe se ing. The e is also he highes po en ial o pa ial healing o any de ec s
ha may ha e o med as a esul o he simul aneously ongoing hyd a ion. These ac o s, he e o e,
p obably led o he ac ha he dynamic modulus o elas ici y con inued o inc ease app oxima ely h ee
weeks a e he specimens had been exposed o ai , despi e he ac ha he i s c acks appea ed on he
su ace o he specimens wi hin 24 hou s o he s a o d ying ( igu e 6, abo e). On he o he hand,
specimens ha we e cu ed o longe pe iods exhibi an immedia e and e y sha p dec ease in dynamic
moduli, because he ine po es d y ou and c acks o m e y in ensi ely due o he associa ed la ge
sh inkage, ( igu e 6, below). A e his sha p dec ease, he dynamic moduli o elas ici y inc ease again,
which can be a ibu ed o g adual pa ial closing o he c acks – p obably mainly due o d ying and
sh inkage o he inside o he specimen, which may ha e bound he sh inkage in he ea ly s ages
o d ying, and hus con ibu ed o he ini ial o ma ion o su ace c acks in pa icula . An impo an
ac o can also be he na u e o he o med c acks, which can a y depending on he leng h o cu ing
pe iod. The e i ica ion and u he analysis o hese assump ions is he subjec o ano he ongoing
ollow-up esea ch.
Figu e 6. Tes specimens a e 24 hou s o exposu e o d ying in he ai – he specimen
om he 24H se (abo e), he specimen om he 7D se (below).
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4. Conclusion
This s udy ocused on he in luence o he cu ing pe iod (in an en i onmen wi h RH > 95%) o slag
pas es ac i a ed by wa e glass wi h a silica e modulus o 1.5 on hei dynamic p ope ies. Based on he
conduc ed expe imen , he ollowing can be s a ed:
• he examined alkali-ac i a ed pas e is ex emely p one o c ack o ma ion du ing d ying,
• he pas es exposed o ai immedia ely a e demolding (aged 24 hou s) we e ela i ely leas
p one o c ack o ma ion and, despi e he appea ance o c acks, exhibi ed an inc ease in dynamic
moduli du ing he i s weeks o d ying,
• on he o he hand, cu ing unde humidi y up o he age o 2, 7 and 28 days led o he same end
beha iou in he o m o a conside able dec ease in he dynamic moduli (up o 30% o he
o iginal alue) du ing he i s 24 hou s o d ying, wi h he dec ease being mos p onounced,
especially, o specimens cu ed o 28 days,
• he esonance me hod has demons a ed i s bene i s o moni o ing o he de elopmen o he
in e nal s uc u e o he AAS pas e, no only he ela i e modulus o elas ici y bu also he
de elopmen o he dynamic Poisson’s a io, which in he case o de ec s eached un ealis ic
alues o he s udied ype o ma e ial.
The esul s p esen ed in his pape a e pa o an ongoing complex expe imen , which is planned o
end when he samples a e 1 yea old. Cu en ly, he esul s acqui ed om he scanning elec on
mic oscope, me cu y po osime y and di e en ial he mal analysis a e being con inually e alua ed, he
de elopmen o esonan equencies and s eng h cha ac e is ics a e being measu ed, as well as
moni o ing o c acks o e ime. The esul s will be g adually p esen ed in u u e publica ions.
Acknowledgemen
This esea ch was unded by he Czech Science Founda ion, g an numbe 22-02098S, p ojec i le
“Expe imen al analysis o he sh inkage, c eep and c acking mechanism o he ma e ials based on he
alkali-ac i a ed slag”.
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