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E ec o he p epa a ion o lime
pu ies on hei p ope ies
E a Na á ilo á1, E a Tihlaříko á1, Vilém Neděla1, Pa la Ro naníko á2 & Ja osla Pa lík3
In he s udy o lime as he basic componen o his o ical mo a s and plas e s, ou lime pu ies p epa ed
om a ious kinds o lime o a ious g anulome y and by a ious ways o p epa a ion we e e alua ed.
The heological p ope ies and mic o-mo phologic changes, g owing o calci e c ys als, and a e o
ca bona ion we e moni o ed. The lime pu y p epa ed om lump lime achie es he bes heological
p ope ies, yield s ess 214.7 Pa and plas ic iscosi y 2.6 Pa·s. The sui abili y o his lime pu y was
checked by es ing he de elopmen o calcium hyd oxide and calci e c ys als using scanning elec on
mic oscopy and en i onmen al scanning elec on mic oscopy. The diso de ed c ys als o calcium
hyd oxide exhibi be e ca bona ion esul ing in he la ge c ys als o calci e; he e o e, he mo a
p epa ed om he lump lime has he highes lexu al s eng h and comp essi e s eng h 0.8/2.5 MPa, i s
ca bona ion is he as es and exhibi s he longes du abili y. Also, hanks o he mic o-mo phological
cha ac e iza ion o samples in hei na i e s a e by means o en i onmen al scanning elec on
mic oscopy, he new way o lime pu y p epa a ion by mixing was p o en. The p epa a ion consis s in
he mechanical c ash o he lime pa icles immedia ely a e hyd a ion. This enables he p ope ies o
pu y p epa ed om lump lime o be nea ly eached.
In he pas lime pu y was adi ional ma e ial wi h a wide applica ion in cons uc ion. I used o be p epa ed om
lump lime and i ea u ed good wo kabili y, plas ici y and du abili y. The adi ional p epa a ion o lime pu y
was eplaced by mode n chemical- echnological p ocesses. Lime pu y is essen ial o he es o a ion o his o ic
plas e , wall pain ing, sg a i o e c1. Lime pu y is ob ained by he hyd a ion o calcined limes one in an excess o
wa e acco ding o he ollowing equa ion:
+→ +
−
·CaOHOCa(OH)65kJmol (1)
22 1
I is a s ongly exo he mic eac ion which leads o he enla gemen o olume. The a io o change in he pa i-
cles’ olume o CaO o Ca(OH)2 is 16.9/33.2. Lime pu y is an aqueous suspension o calcium hyd oxide pa icles.
A small p opo ion o calcium ca bona e can be p esen due o incomple e calcina ion o limes one o eac ion
wi h ca bon dioxide. The p ocess o hyd a ion o CaO is dependen upon he eac i i y o quicklime, which is
in luenced by he empe a u e o calcina ion o CaCO3. CaO is eleased om limes one and he po e s uc u e o
g ains is gene a ed du ing calcina ion. The physical p ope ies o quicklime, such as po osi y, densi y, g ain size
and hyd a ion a e, a e dependen on he empe a u e o calcina ion. Fu he mo e, he p ocess o CaO hyd a ion
is dependen on he dis ibu ion o pa icle size, he quan i y and quali y o he added wa e , he empe a u e o
he wa e , he p esence o impu i ies in he quicklime, and he p esence o ions in he mixing wa e 2,3. The speci ic
su ace a ea is he mos eliable pa ame e which can be used o e alua e he eac i i y o quicklime. The highe
speci ic su ace a ea o quicklime is he eason o i s highe eac i i y4–7. The bu ning o CaO leads o changes
in he mic os uc u e and hese di e ences in he mic os uc u e o CaO c ys als bu n a di e en empe a u es
esul in di e en hyd a ion ac i i y o CaO8. The hyd a ion p ocess o quicklime is also a ec ed by he pa icle
size o CaO. The ine pa icles a e mo e sin e ed and hus hey cause a low eac i i y o quicklime. The coa se
pa icles will con ain some amoun o unbu ned CaCO3, which is an ine ma e ial in quicklime4,9. Va ious me h-
ods and he empe a u e o hyd a ion o CaO lead o ob aining lime pu y wi h a di e en mo phology, size,
and size dis ibu ion o calcium hyd oxide c ys als. The calcium hyd oxide c ys als wi h a size o app oxima ely
100 –110 nm o igina e du ing he hyd a ion in he excess o wa e and a a lowe empe a u e5. Calcium hyd oxide
1The Czech Academy o Science, Ins i u e o Scien i ic Ins umen s, B no, 612 64, Czech Republic. 2Ins i u e o
Chemis y, Facul y o Ci il Enginee ing, B no Uni e si y o Technology, B no, 602 00, Czech Republic. 3Lhois ,
Lime kiln Če o y schody a.s., Tmaň, 267 21, Czech Republic. Co espondence and eques s o ma e ials should be
add essed o E.N. (email: [email p o ec ed])
Recei ed: 24 Augus 2017
Accep ed: 27 No embe 2017
Published: xx xx xxxx
OPEN
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hyd a ed in he excess o wa e exhibi s c ys als which ha e clea ly isible edges. Calcium hyd oxide hyd a ed in a
smalle amoun o wa e is wi hou he sha p edges o c ys al and ends o o m agglome a es10.
The long- e m ma u ing o lime pu y in an excess o wa e has a bene icial e ec on i s quali y. Such s o ed
lime pu y has be e plas ici y, wo kabili y, and i e ains su icien wa e o p epa e plas e o a high du abil-
i y11–13. The mic os uc u e o calcium hyd oxide is changed du ing he ma u ing o lime pu y14,15 and he
Ca(OH)2 c ys als diminish. The Ca(OH)2 c ys als wi h a size o be ween 37–50 nm occu in eshly hyd a ed lime
- he c ys als ha e a size o 34 nm a he age o wo mon hs and 28 nm a he age o 14 mon hs. The speci ic su ace
a ea o he calcium hyd oxide inc eases wi h his educ ion in he size o he calcium hyd oxide c ys als11,14–16.
Fu he mo e, he calcium hyd oxide c ys als change hei o m om la ge p isma ic c ys als o submic ome e
pla e c ys als and seconda y nuclea ion o nanome e pla e c ys als11,15,17. The change in he o iginal p isma ic
c ys als in o smalle submic ome e pla e c ys als wi h a highe speci ic su ace a ea leads o an inc eased adso p-
ion o wa e and he eby inc eases plas ici y and wo kabili y10,11,15,17. A zeni e al.16 examined he e ec o he
ma u a ion o lime pu y on i s iscosi y. They p epa ed h ee lime pu ies wi h di e en imes o ma u a ion.
Obse a ion o he lime pu ies by TEM e ealed ha he calcium hyd oxide c ys als educe in size o e ime. The
oldes lime pu y showed he g ea es shea esis ance and i was e en mo e iscous han he h ee-mon h-old
lime pu y as well as he non-ma u ed lime pu y. The non-ma u ed lime pu y con ains he agglome a es o
calcium hyd oxide and hese agglome a es a e co e ed by a hin ilm o wa e , which ac s as a lub ican , and so
his lime pu y is ex emely luid. The p olonged ageing o lime pu y leads o a highe iscosi y, which is caused
by he change in i s mic os uc u e and he speci ic su ace a ea o calcium hyd oxide du ing he ageing p ocess.
Analogous o he in es iga ion o lime, Pai a e al.18 p epa ed lime mo a s wi h a di e en ma u a ion pe iod. The
mo a s ma u ed o se en days we e mo e iscous in hei esh s a e, showed highe s eng hs a he age o 90
days, and exhibi ed a lowe capilla y abso p ion coe icien han he mo a s wi hou ma u a ion. Ma galha e al.19
ound ha slaked lump lime p o ides a binde wi h a highe p opo ion o ac i e lime han powde ed lime. The
mo a s p epa ed om he mic onized lime show a highe po osi y wi h la ge po es, leading o a educ ion in
hei mechanical s eng hs. The mo a s p epa ed om lump lime exhibi highe s eng hs, bu hey equi e
o e -ageing ea men because o hei sh inking.
Resul s
Rheology o he lime pu ies. The esul s o he measu emen o he plas ic iscosi y and he yield s ess
o lime pu ies SL-A, SL-B, SL-C, and SL-B1 du ing hei ma u a ion a he age o 3, 30, 60, and 90 days a e shown
in Figs1 and 2. The g aphs show an inc ease in he plas ic iscosi y and he yield s ess o he lime pu ies wi h
Figu e 1. A e age alues o plas ic iscosi y o lime pu ies a di e en ages.
Figu e 2. A e age alues o yield s ess o lime pu ies a di e en ages.
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a p olonged pe iod o ma u a ion. The inc ease in he alues o he plas ic iscosi y and he yield s ess in lime
pu ies SL-A, SL-B, and SL-B1 is no so appa en a he ages o 3, 30, and 60 days compa ed o lime pu y SL-C.
The alues o he plas ic iscosi y and he yield s ess o lime pu y SL-B inc ease signi ican ly a he age o 90 days.
The inc ease in he alues o he plas ic iscosi y and he yield s ess is slow a he age o 90 days o lime pu ies
SL-A and SL-B1. The highes plas ic iscosi y and yield s ess we e ound in he sample om lump lime C. Lime
pu y SL-A, p epa ed om lime con aining g ains unde 90 µm, showed he lowes plas ic iscosi y and yield
s ess. Lime pu y SL-B, p epa ed om lime con aining g ains unde 200 µm, eached only sligh ly highe alues
o plas ic iscosi y and yield s ess han lime pu y SL-A. Howe e , he di e ences in he alues o yield s ess and
plas ic iscosi y we e g ea e a he age o 90 days o lime pu ies SL-A and SL-B. The dis up ion o he pa icles
by mixing a ec ed he plas ic iscosi y and yield s ess o lime pu y SL-B1, which eached highe alues o plas ic
iscosi y and yield s ess han lime pu y SL-B, which was no exposed o mixing a e hyd a ion, and he g ains o
he lime a e no in any way dis up ed. The esul s o he heological measu emen s a e consis en wi h p e iously
published esul s16,18,19.
Image o he mic os uc u e o he lime pu ies. Figu es3–6 illus a e he mic os uc u e o lime
pu ies SL-A, SL-B, SL-C, and SL-B1 du ing hei ma u a ion a he age o 3, 30, 60, and 90 days. Figu es3I and 4I
show he p isma ic hexagonal c ys als o calcium hyd oxide c ea ed in samples SL-A and SL-B. Lime pu ies SL-C
and SL-B1 do no con ain he signi ican c ys als o calcium hyd oxide which a e p esen in samples SL-A and
SL-B. The c ys als in hese cases a e coa ed wi h a laye o hyd ogel (Ca(OH)2.aq), which is al eady disce nible
a e h ee days o hyd a ion (ma u a ion) Figs5I and 6I. Du ing he ma u a ion o all he lime pu y samples, he
egula hexagonal c ys als o calcium hyd oxide a e ans o med in o smalle i egula c ys als which a e coa ed
wi h a laye o hyd ogel. The g adual ans o ma ion o he calcium hyd oxide c ys als is well e iden in Figs3II–
IV, 4II–IV, 5II–IV, and 6II–IV. The ans o ma ion o he calcium hyd oxide c ys als and hyd ogel o ma ion o
lime pu ies SL-A and SL-B is slowe han in he samples SL-C and SL-B1. The mic og aphs in Figs5III and 6III
show he calcium hyd oxide c ys als coa ed wi h a laye o hyd ogel which o igina es as e and mo e in ensi ely
in samples SL-C and SL-B1. Con e sely, he mic og aphs in Figs3III and 4III p esen he mic os uc u e o lime
pu ies SL-A and SL-B wi h clea ly isible c ys als o calcium hyd oxide. The laye o hyd ogel inc eases du ing
he ma u a ion o lime pu ies. The amoun o hyd ogel is g ea es a he age o 90 days in sample SL-C and in
sample SL-B1 Figs5IV and 6IV. The o ma ion o hyd ogel on he su ace o he c ys als o calcium hyd oxide
p oceeds bes in sample SL-C, which was p epa ed om lump lime whe e he egula hexagonal c ys als o cal-
cium hyd oxide we e no ully de eloped. The p ocess o pa icle dis up ion immedia ely a e hyd a ion enables
he accele a ion o he p ocess o hyd ogel o ma ion on he su ace o he c ys als o calcium hyd oxide, and,
mo eo e , he p ocess o ans o ma ion o he egula c ys als o calcium hyd oxide o he smalle i egula ones
is as e . The mic os uc u e images o lime pu ies con i m he esul s p o ided by he pe o med heological
measu emen s.
The HR-ESEM images o lime pu y SL-A wi hou p epa a ion o he sample and spu e ing a he age o 3 and
30 days a e shown in Fig.7. Owing o he sophis ica ed and, in his wo k, expe imen ally p o en me hod o he
Figu e 3. Lime pu y SL-A a he age o 3 days (I), 30 days (II), 60 days (III) and 90 days (IV).
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p epa a ion o samples o HR-SEM, he images om he HR ESEM p o ide e y simila in o ma ion: signi ican
hexagonal c ys als o calcium hyd oxide see Fig.7I. The egula hexagonal c ys als o calcium hyd oxide a e
g adually ans o med in o smalle i egula c ys als coa ed wi h a laye o hyd ogel du ing he ma u a ion o
lime pu y Fig.7II. The HR-ESEM is a p e e able me hod o obse ing mic o-mo phological changes du ing he
ma u a ion o lime pu ies because i is no necessa y o use complica ed sample p epa a ion me hods. Inco ec ly
spu e coa ed samples can lead o he o ma ion o a e ac s which can dis o he mic o-mo phological
Figu e 4. Lime pu y SL-B a he age o 3 days (I), 30 days (II), 60 days (III) and 90 days (IV).
Figu e 5. Lime pu y SL-C a he age o 3 days (I), 30 days (II), 60 days (III) and 90 days (IV).
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in e p e a ion. The HR-SEM is a sui able me hod o he e alua ion o mo phological changes du ing he ma u a-
ion o lime pu ies; howe e , his me hod places heigh ened demands on he sample p epa a ion, and, he e o e,
i can in oduce inaccu acies in o he cha ac e iza ion o he mic os uc u e. The HR-ESEM is a mo e accu a e,
as e , and easie me hod o he e alua ion o he mo phology lime pu ies, as he samples a e no ea ed a all
be o e hei obse a ion20,21. Thus, he e a e no a e ac s dis o ing he mic os uc u al in e p e a ion.
The same speci ic di e ences in he sample mo phology may also be caused due o he samples d ying and
coa ing o a me al laye o SEM obse a ion. Con e sely, obse a ion in ESEM does no equi e he abo e p o-
cesses and he samples a e obse ed na u ally we and wi hou any modi ica ions. The su ace mo phology o he
c ys als obse ed using he ESEM a e somewha smoo h and ee o sha p edges and mic o-c acks see Fig.7I and II
s. Fig.3I and II.
Mic os uc u e o ca bona ed lime pu ies. Figu e8 shows he de elopmen o calci e c ys als in ca -
bona ed lime pu ies C-SL-A, C-SL-B, C-SL-C, and C-CL-B1 a e 14 days o s o age in a box wi h a high con-
cen a ion (20%) o CO2 and humidi y (70%). The leng h o he side o he calci e c ys als was measu ed. The
egula c ys als which g ew sepa a ely we e selec ed o measu emen . The images in Fig.8 and Table1 show he
Figu e 6. Lime pu y SL-B1 a he age o 3 days (I), 30 days (II), 60 days (III) and 90 days (IV).
Figu e 7. The lime pu y SL-A a he age o 3 days (I) and 30 days (II).

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di e en de elopmen o calci e c ys als in he ca bona ed lime pu ies. The size o calci e c ys als is a ec ed by he
p epa a ion me hod o he lime pu ies and he g anulome y o lime. The smalles calci e c ys als we e de eloped
in lime pu y C-SL-A, which was p epa ed om lime wi h a g ain size o unde 90 μm Fig.8I; whe eas he la ge
c ys als o igina ed in lime pu y C-SL-B Fig.8II. The la ges calci e c ys als we e ound in lime pu y C-SL-C
Fig.8III. The me hod o p epa a ion, i. e. he mixing o lime pu y SL-B1, a ec ed he size o he calci e c ys als
C-SL-B1 Fig.8IV. The mixing p ocess leads on o he easie dissolu ion o he g ains o quicklime, subsequen ly
o he o ma ion o la ge c ys als o calcium hyd oxide.
Di e en ial he mal analysis o he ca bona ed lime pu ies. The esul s o di e en ial he mal anal-
ysis o ca bona ed lime pu ies C-SL-A, C-SL-B, C-SL-C, and C-CL-B1 a e 14 days o s o age in a CO2 en i on-
men a e demons a ed in Fig.9. The cu es TG and DTG show ha he ca bona ion p ocess o he indi idual
lime pu ies is di e en . The ca bona ion o lime pu y samples C-SL-A and C-SL-B p oceeded simila ly. The
smalle g ains in lime A lead o a lowe con en o calcium hyd oxide and a highe con en o calcium ca bona e
(25.2% Ca(OH)2 and 65.7% CaCO3) compa ed o lime B (20.0% Ca(OH)2 and 68.7% CaCO3). Sample C-SL-C,
p epa ed om lump lime, ca bona es e y quickly (2.8% Ca(OH)2 and 85.8% CaCO3). Sample C-SL-B1 con ained
less calcium hyd oxide and, ac ually, mo e calcium ca bona e (8.9% Ca(OH)2 and 80.0% CaCO3) han lime pu y
C-SL-B due o he p ocess o ac i a ion.
S eng hs o lime mo a s. The e ec o lime pu y p epa a ion on he ca bona ion p ocess was also
assessed by de e mining he s eng hs o lime mo a s. The esul s o he ensile and comp essi e s eng hs meas-
u emen s o lime mo a s M-A, M-B, M-C, and M-B1 a he age o 28 days a e illus a ed in Table2. The s eng hs
Figu e 8. Mic os uc u e o ca bona ed lime pu ies C-SL-A (I), C-SL-B (II), C-SL-C (III) and C-SL-B1 (IV).
C-SL-A C-SL-B C-SL-C C-SL-B1
A e age side leng h o calci e
c ys als side [nm] 128.84 ± 10.77 236.00 ± 13.18 309.67 ± 14.96 244.06 ± 14.18
Table 1. A e age side leng h o he calci e c ys als. The epea abili y limi was calcula ed o each alue.
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o he lime mo a s a y depending on he g anulome y o he o iginal quicklime om which he lime pu ies
and he mo a s we e p epa ed. Mo a M-B, p epa ed om lime pu y SL-B, eached highe s eng hs han mo -
a M-A, which was p epa ed om lime pu y SL-A. Mo a M-C, which was p epa ed om he pu y made om
lump lime, eached he highes s eng hs.
The e ec o he me hod o p epa a ion o lime pu y is also no iceable because mo a M-B1 achie ed highe
s eng hs han mo a M-B. Bo h o hese lime mo a s we e p epa ed om lime wi h he same g anulome y, bu
lime pu y SL-B1 was mixed, unlike lime pu y SL-B.
Discussion
The aim o he a icle was o analyse he de elopmen o he lime pu ies in he dependence on ime by means o
selec ed me hods gi ing accu a e esul s. The ound esul s exac ly cha ac e ize he lime pu ies’ p ope ies and
co espond wi h he esul s published by o he au ho s. The au ho s o he a icle conside a high po en ial in
he mic o-mo phological cha ac e iza ion o he lime pu ies in hei na i e s a e, so wi hou any sample ea -
men wi h minimum occu ence o a e ac s, by means o ESEM. The a icle p esen s an e alua ion o he esul s
ob ained by means o classic SEM and ESEM o he objec i e a bi a ion.
Fou lime pu ies p epa ed in di e en ways om quicklimes wi h a ying g anulome y we e analysed in
he dependence on he ma u a ion ime. Du ing he ma u a ion o lime pu ies, he egula hexagonal c ys als
o calcium hyd oxide a e ans o med in o smalle i egula c ys als which a e coa ed wi h a laye o hyd ogel.
The heological p ope ies a e dependen on he amoun o hyd ogel p oduced du ing he ageing o lime pu ies.
• The use o lump lime o mixing a suspension o lime o he p epa a ion o lime pu y leads o he o ma ion
o incomple ely egula calcium hyd oxide c ys als and a high amoun o hyd ogel o ma ion. I esul s in
a as e o ma ion o calcium ca bona e, he g ow h o la ge calci e c ys als, and highe s eng hs o lime
mo a s.
• The alues o plas ic iscosi y and yield s ess inc ease wi h he inc easing pe iod o ma u a ion. The use o
aged limes leads o ob aining an in e media e p oduc o highe quali y o he p epa a ion o lime mo a s.
• The p ocess o pa icle dis up ion du ing he mixing o lime pu y helps accele a e he hyd ogel o ma ion as
well as inc easing plas ic iscosi y and yield s ess.
• The use o lump lime o he mechanical dis up ion o lime pa icles is he mos sui able o he p ope ies o
lime pu y and, consequen ly, o he p epa a ion o lime mo a s.
• Ma u ed lime pu ies p epa ed om lump lime and by mixing lime pu y a e he mos sui able o he p epa-
a ion o mo a .
The mos impo an con ibu ion o he a icle in he ield o conse a ion and es o a ion o his o ical mo -
a s consis s in he new way o lime pu ies p epa a ion by means o mechanical c ush o he lime pa icles.
Mo a s p oduced om such p epa ed lime pu y achie ed simila p ope ies as mo a s made om he ma u ed
Figu e 9. Di e en ial he mal analysis o he ca bona ed lime pu ies C-SL-A, C-SL-B, C-SL-C and C-SL-B1,
ed cu e – C-SL-A, g een cu e – C-SL-B, blue cu e – C-SL-C, black cu e – C-SL-B1.
MA MB MC MB1
Flexu al s eng h [MPa] 0.5 ± 0.01 0.6 ± 0.02 0.8 ± 0.02 0.7 ± 0.03
Comp essi e s eng h [MPa] 1.3 ± 0.06 1.5 ± 0.05 2.5 ± 0.08 1.8 ± 0.05
Table 2. A e age s eng hs o lime mo a s M-A, M-B, M-C and M-B1 a 28 days. The epea abili y limi was
calcula ed o each alue.
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lime pu y p epa ed om lump lime. An ad an age o he new way o lime pu y p epa a ion is he use o com-
monly a ailable powde lime wi hou he necessi y o using mo e di icul o ob ain lump lime. The p esen ed
esul s exhibi ed ha mo a s wi h highe s eng hs can be p epa ed om common powde lime. These mo a s
will be mo e du able wi h a highe esis ance o en i onmen al in luences and con amina ed a mosphe e.
Me hods
Limes. Lime A wi h a g ain size o unde 90 µm, lime B wi h a g ain size o unde 200 µm, and lump lime wi h
a g ain size om 10 mm o 63 mm (Lime kiln, Če o y schody a.s., Tmaň) we e used o p epa e he lime pu ies.
Lime A and lime B a e mix u es o lime bu ned pa ially (70%) in he co-cu en egene a i e u nace a 1000 °C
and in he coun e cu en sha u nace (30%) a 1300 °C. Lime C is a mix u e o lime bu ned in he co-cu en
egene a i e u nace a 1100 °C (50%) and in he coun e cu en sha u nace a 1300 °C (50%). The con en o
o al CaO/ac i e CaO in lime A was 96.05/93.74, in lime B 94.08/88.34, and in lime C 95.87/92.33. The eac i i y
o lime exp essed as he ime aken o each a empe a u e o 60 °C, acco ding o EN 459-2, was 2.3 min o lime
A, 2.6 min o lime B, and 3.5 min o lime C.
The g anulome y o lime A and lime B is shown in Table3. Lime A con ains mo e ine pa icles unde
0.063 µm and no pa icles abo e 200 µm. Lime B con ains less ine pa icles unde 0.063 µm and exhibi s a highe
con en o pa icles below 200 µm and abo e 200 µm.
P epa a ion o he lime pu ies and he lime mo a s. Lime pu ies SL-A, SL-B, and SL-C we e p e-
pa ed by mixing 200 g o lime and 640 ml o deionized wa e . Lime pu y SL-B1 was p epa ed by mixing 200 g
o lime and 640 ml o deionized wa e and his lime pu y was mixed (25,000 e /min) o 5 minu es a e i s
hyd a ion. The esh lime pu ies we e immedia ely s o ed in plas ic bo les and hey we e supplemen ed wi h
wa e o a oid eac ion wi h CO2 and ai d ying. The samples we e hen kep in closed bo les a a empe a u e
o 20 ± 1 °C. Samples SL-A, SL-B, SL-C, and SL-B1 we e s o ed in a box wi h 70% humidi y and a 20% concen-
a ion o CO2 o 14 days o accele a ed ca bona ion. Lime mo a s M-A, M-B, M-C, and M-B1 we e p epa ed
om he lime pu ies and sand wi h a a io o 1:3. The lime mo a s we e placed in moulds wi h dimensions o
40 × 40 × 160 mm. Specimens we e s o ed unde labo a o y condi ions a a empe a u e o 20 ± 1 °C and a ela i e
humidi y o 50 ± 5% a e hei emo al om he moulds.
Rheology. The heological p ope ies o lime pu ies SL-A, SL-B, SL-C, and SL-B1a e 3, 30, 60, and 90 days’
ma u a ion we e moni o ed by a Disco e y Hyb id Rheome e HR-1 (pa allel pla e diame e o 25 mm wi h
oughened su ace). The heological p ope ies o he lime pu ies we e de e mined om he cu es o low wi h
he inc easing and dec easing shea a e in he ange om 0 sec−1 o 200 sec−1 o e 2 minu es. The alues o yield
s ess and plas ic iscosi y we e de e mined acco ding o he Bingham model,
ττμγ=+(2)
0
whe e τ [Pa] is he shea s ess,τ0 is he yield s ess, μ [Pa·s] is he plas ic iscosi y, and
γ

[s−1] is he shea s ain
a e22. Tempe a u e o he measu emen appa a us and he labo a o y we e kep cons an a 20 (±0.5) °C.
Obse a ion in SEM and ESEM. Lime pu y samples SL-A, SL-B, SL-C, and SL-B1 we e obse ed in he
high esolu ion scanning elec on mic oscope (HR-SEM) JSM6700F JEOL (wi h a beam ene gy o 5 keV, a wo k-
ing dis ance o 8 mm, and an E e ha -Tho nley de ec o ) a e 3, 30, 60, and 90 days. The samples o he lime
pu ies we e p epa ed o obse a ion in he SEM in he ollowing manne : he samples we e insed wi h 10 ml o
ace one o emo e wa e and 10 ml o die hyl e he o d ying. Nex , he samples we e d ied in a ni ogen a mos-
phe e in o de o elimina e he in luence o CO2, and he samples we e spu e ed.
The sample o lime pu y SL-A was obse ed in he en i onmen al scanning elec on mic oscope (ESEM)
AQUASEM II (wi h a beam ene gy o 20 keV, a wa e apou p essu e o 800 Pa, and an ioniza ion de ec o ) a e
3 and 30 days. The sample was s udied di ec ly wi hou spu e ing.
The di e en de elopmen o he calci e c ys als in ca bona ed lime pu ies C-SL-A, C-SL-B, C-SL-C a C-SL-
B1 was moni o ed wi h he high esolu ion en i onmen al scanning elec on mic oscope (HR-ESEM) QUANTA
650 FEG (wi h a beam ene gy o 10 keV, wa e apou p essu e o 200 Pa, and a GSED de ec o ). The samples we e
s udied di ec ly wi hou spu e ing. The leng h o he side o he calci e c ys als was measu ed using he Scandium
so wa e.
Di e en ial he mal analysis. The di e en ial he mal analysis o ca bona ed lime pu ies C-SL-A,
C-SL-B, C-SL-C, and C-SL-B1 was pe o med using he he mal analyse NETSCH STA 2500 a e 14 days o
being s o ed in a box wi h 70% humidi y and a 20% concen a ion o CO2. The used ins umen exhibi s accu acy
wi h an e o ±10%. The measu emen was ca ied ou unde a ni ogen a mosphe e.
Lime <0.063 [µm] 0.063–0.090 [µm] 0.090–0.200 [µm] >200 [µm]
A 15.18 14.04 3.41 2.77
B 14.14 9.85 4.62 2.86
Table 3. G ain con en o lime A and B.
www.na u e.com/scien i ic epo s/
9
ScIen I Ic RepoR s | 7: 17260 | DOI:10.1038/s41598-017-17527-3
S eng hs. The lexu al s eng h and comp essi e s eng h o lime mo a s M-A, M-B, M-C, and M-B1 we e
de e mined a 28 days acco ding o EN 1015-11.
All p esen ed da a was calcula ed as a e age alue om he epea ed i e measu emen s and s anda d de ia-
ion and epea abili y limi (p obabili y le el 95%) we e calcula ed.
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Acknowledgemen s
This pape has been wo ked ou unde he p ojec No. L100651601, he Minis y o Educa ion, You h and Spo s
o he Czech Republic (p ojec LO1212), he esea ch in as uc u e was unded by he Minis y o Educa ion,
You h and Spo s o he Czech Republic and he Eu opean Commission (p ojec CZ.1.05/2.1.00/01.0017). This
pape also suppo ed by he p ojec No. LO1408 “AdMaS UP - Ad anced Ma e ials, S uc u es and Technologies”,
suppo ed by Minis y o Educa ion, You h and Spo s unde he “Na ional Sus ainabili y P og amme I”.
Au ho Con ibu ions
E. Na á ilo á, P. Ro naníko á and V. Neděla w o e he main manusc ip , E. Na á ilo á p epa ed Figu es 1, 2,
8 and 9, E. Tihlaříko á p epa ed Figu es 3–7 and J. Pa lík analyzed p ope ies o limes. All au ho s e iewed he
manus c ip .
Addi ional In o ma ion
Compe ing In e es s: The au ho s decla e ha hey ha e no compe ing in e es s.
Publishe 's no e: Sp inge Na u e emains neu al wi h ega d o ju isdic ional claims in published maps and
ins i u ional a ilia ions.
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