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IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
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P epa a ion o iclinic ali e wi h sho soakings in a small
expe imen al high- empe a u e u nace
S Ra aszo á1
1 Facul y o Ci il Enginee ing, B no Uni e si y o Technology, Ve e i 331/95, 602 00
B no, Czech Republic
E-mail: a aszo a.s@ ce. u b .cz
Abs ac . The a icle deals wi h a labo a o y p epa a ion o iclinic modi ica ion o clinke
mine al icalcium silica e. A subs an ial pa o he a icle is de o ed o he echnology and
echnique o i ing a sample o icalcium silica e, which would in he u u e allow he s udy o
he de elopmen o he c ys al la ice s uc u e o his clinke mine al a sho iso he mal
du a ions, in he o de o minu es. As pa o he esea ch, a small high- empe a u e
expe imen al u nace was designed and cons uc ed. Based on he esul s, we can exp ess he
sui abili y and applicabili y o his u nace o he s udy o he o ma ion o iclinic icalcium
silica e a sho soakings.
1. In oduc ion
The cu en main p oblem o he indus ial cemen p oduc ions is he a iabili y o hei mine alogical
composi ion. This depends on he p esence o impu i ies om he aw ma e ials o uel and he i ing
p ocess. The p ocess o syn hesis o clinke mine als becomes a decisi e ac o ha de e mines hei
subsequen beha iou in indus ially p oduced cemen s. To cha ac e ize and possibly in luence he
a iabili y o he mine alogical composi ion o clinke , i is necessa y o s udy he in luence o a ious
polymo phs o clinke mine als on he p ope ies o indus ially p oduced clinke s, especially om a
chemical and s uc u al poin o iew [1-3].
In gene al, mo e han wen y mine als can be iden i ied in clinke , bu only ou o hem a e
conside ed impo an , namely icalcium silica e (C3S, ali e), dicalcium silica e (C2S, beli e),
icalcium alumina e (C3A) and e a calcium alumina e e i e (C4AF). Due o hei cha ac e is ic
p ope ies, each o hese mine als in luences he speci ic p ope ies o indi idual cemen s. Excep o
C4AF, all majo clinke mine als show s ong polymo phism [4-5].
Mos o he s anda d me hods used o labo a o y p epa a ion o clinke mine als a e ela i ely ime
consuming. The composi ion o he aw ma e ial mix u e and he se ing o he combus ion pa ame e s
a e among he main ac o s ha de e mine he inal composi ion o he clinke .
The a icle deals wi h he s udy o he cou se o iclinic ali e o ma ion du ing sho soakings. The
aim is o assess he sui abili y o he p oposed small expe imen al high- empe a u e u nace and i s
applicabili y o his pu pose.
2. Ma e ials and me hods
Two aw ma e ials in chemical pu i y p.a. we e used o p epa e iclinic ali e, namely calcium
ca bona e (p.a. 99.0%, Pen a) and silica (99.9%, Lachne ). The aw ma e ials we e dosed in an amoun
co esponding o he mola a io o ali e in he pe cen ages o 73.6% CaO and 26.3% SiO2.
Young Scien is 2021
IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
IOP Publishing
doi:10.1088/1757-899X/1209/1/012045
2
The aw ma e ial mix u e was homogenized by we milling in he p esence o wa e in a
PULVERISETTE 6 plane a y mill a a milling speed o 500 pm o 30 minu es. A 500 ml g inding
capsule wi h 25 pieces o aga e g inding balls wi h a diame e o 20 mm was used.
The we milling slu y was hen d ied in a Binde C 170 labo a o y o en a 105 °C o 24 hou s.
The ma e ial hus p epa ed was used o p oduce able s o he ali e i ing i sel .
2.1. P epa a ion o able s
Samples o i ing we e p epa ed om powde ed aw ma e ial mix u e, which was comp essed in o a
cylind ical hole, om which, a e comp ession, cylind ical able s wi h a hollow cen e we e made.
This hollow cen e se es o hanging he sample on he weld o a he mocouple used o inse he
able in o he u nace.
A cus om-made comp ession mold was used o p epa e he able s, see igu e 1a. The mold wi h a
shaped pis on was made o ha dened s eel and g ound wi h high p ecision o p e en i om seizing up
and losing weigh . This allows o accu a e weighing. By pushing he ma e ial o he s op, a cons an
bulk densi y o he molding was main ained.
The bulk densi y o he able men ioned in li e a u e [7] is 1.8 g/cm3 based on which he weigh o
p oduce he able has been op imized. The p oduc ion o he able i sel ook place by means o a
comp ession olle using oil and g aphi e, which was hen placed in a hand p ess, whe e comp ession
was pe o med o a cons an olume o he able .
Figu e 1. a) able mold; b) made able o i ing.
2.2. Fi ing
The i ing ook place in an elec ic esis ance u nace wi h a manipula o , which is sui able o i ing
subs ances in which eac ions ake place in he solid phase o wi h only a pa ial p opo ion o he
mel . The i ing cycle is ully au oma ed, which gua an ees high ep oducibili y o hea ea men and
p ecise adhe ence o i ing pa ame e s.
a)
b)
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IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
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The sample was placed in a well in he o en cap when he selec ed o en empe a u e was eached
and s abilized. Then he soaking ime o he sample in he u nace was se on he con ol uni panel.
The ejec ion o he he mocouple weld wi h a small sample hole occu s a e one u n o he c ank.
The he mocouple li ed he sample and he cap opened. The closu e o he cap occu s a e he
e u n o he he mocouple wi h he sample o he cen e o he hea ing zone o he u nace. A e he
i ing ime has elapsed, he shu e opened, and he sample is ejec ed on he he mocouple o he uppe
posi ion. A e ejec ion, he cap is closed and he he mocouple lea es he sample in he cap well,
whe e ai lows om he an.
The able s p epa ed by an op imized me hod we e subjec ed o i ing in an expe imen al u nace a
a empe a u e o 1500 °C and wi h soaking imes calcula ed om he inse ion o he sample in o he
o en a 5, 10, 15 and 20 minu es, wi h addi ion o 60 s o wa m up he sample.
The XRD analysis was pe o med wi h a mul i unc ional di ac ome e XRD Empy ean
PANanaly ical wi h Cu anode; Kα was used as he adia ion sou ce wi h pa a me e s o 5° o 90° wi h
a scan-s ep o 0.01°. The ICSD da abase ( eleased 2012) was used o quali a i ely analyse he
di ac ion pa e ns. HighSco e plus so wa e was used o iden i y he indi idual phases.
Figu e 2. a) high- empe a u e u nace wi h manipula o ; b) able be o e i ing; c) able a e i ing.
3. Resul s and discussion
The a icle deals wi h he s udy o he p og ess o ali e o ma ion du ing sho soaking imes. The aim
o his a icle is o assess he sui abili y o he p oposed small expe imen al high- empe a u e u nace
and i s applicabili y o his pu pose.
3.1. P epa a ion o able s
Fo he i s sample p epa a ion, he alue o bulk densi y was aken om he li e a u e, namely 1.8
g/cm3. The weigh o he ba ch was calcula ed o be 58 mg. The pou ing in o he p ess olle ook place
a once and he sample was compac ed. The p essed able could no be emo ed wi hou damage.
Compac ion occu ed only in he uppe pa he lowe pa disin eg a ed du ing handling.
Subsequen ly, he op imiza ion ook place in s eps. The weigh o he ba ch and bulk densi y we e
inc eased. The indi idual weigh s o he samples a e gi en in able 1.
Fo sample no. 2, he weighing was op imized, he p essing od and he inne pa o he olle we e
ubbed wi h oil o p e en he sample om s icking and so ha he e was no p oblem du ing emo al.
The illing p ocess was op imized and di ided in o 3 d phases; each pou ed laye was compac ed wi h
a p essing od. A e illing and p essing, he sample was no s ong enough, he lowe pa
disin eg a ed du ing gen le handling and he ba ch was glued o he walls o he p essing de ice.
b)
c)
a)
Young Scien is 2021
IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
IOP Publishing
doi:10.1088/1757-899X/1209/1/012045
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A e u he op imiza ion, sample no. 3, he weigh and he me hod o sample sepa a ion we e
inc eased. The p ess olle and od we e coa ed wi h a combina ion o oil and ha d g aphi e. The ba ch
was pou ed in he same way as p e ious.
Finally, he whole p ocedu e was op imized as ollows. The amoun o sample was weighed o 73
mg. The ma e ial was g ound, wi hou addi ional compac ion, and so g aphi e was applied o he
p ess. This sample was su icien ly s ong and did no disin eg a e du ing handling. Wi h such a
p ocedu e, i was possible o epea edly o m 30 pelle s wi hou b eaking hem, see igu e 1.
Table 1. Densi y and weigh o indi idual samples when op imizing able s o i ing.
Weighing 73 mg (CaCO3, SiO2) o an assumed densi y o 2.285 g/cm3. Sepa a ing agen so
g aphi e in combina ion wi h oil. Filling p ocess con inuously, slowly wi h simul aneous cella ing,
p essing o cons an olume o he s op.
3.2. Fi ing
The p epa ed able s we e i ed in an expe imen al u nace a a empe a u e o 1500 °C and soaking
imes o 5, 10, 15 and 20 minu es. The p oposed able , p epa ed by an op imized me hod, has been
shown o be eliable and wo ks e y well o i ing in a small expe imen al high- empe a u e u nace.
The manipula o in he o en epea edly picks i up, inse s i in o he u nace and pushes i back ou .
The able does no disin eg a e du ing inse ion, i ing and emo al om he u nace and does no
end o explode o c ack.
By XRD analysis using he Rie eld quan i a i e me hod, in addi ion o he main mine al ali e,
mine al esidues such as ee lime and beli e we e also iden i ied in he i ed samples, see Fig. 3.
Figu e 3. G aphical ep esen a ion o he mine al con en du ing i ing.
158 1.878 x
265 2.034 x
370 2.191 x
475 2.347 x
573 2.285
Weigh
[mg]
Bulk densi y
[g/cm3]
Resul
Sample
no.
Young Scien is 2021
IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
IOP Publishing
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Based on he esul s, we can obse e an inc ease in he ali e mine al con en wi h inc easing i ing
ime. A e 5 minu es he ali e con en in he o mula is 25.29%, while a e 20 minu es i s con en
inc eases o 66.43%. Wi h inc easing i ing ime and he ela ed inc easing ali e con en , he ee lime
con en g adually dec eases, om 53.12% a e 5 minu es o 9.17% a e 20 minu es o i ing. This is
due o he sa u a ion o he mine al beli e and i s g adual con e sion o ali e. This is illus a ed by he
dec easing con en o beli e, which is g adually ans o med in o ali e, which is con i med by he
esul s o op ical phase analysis, see igu e 4.
Figu e 4. Op ical phase analysis.
A e only 5 minu es o i ing, we can obse e small nuclei o ali e in he images om he op ical
phase analysis. As he ali e c ys als g ow, he beli e con en disappea s and he ee lime con en
g adually dec eases.
4. Conclusion
The a icle deals wi h labo a o y p epa a ion o iclinic modi ica ion o clinke mine al icalcium
silica e. A subs an ial pa o he a icle is de o ed o he echnology and echnique o i ing icalcium
silica e a sho soaking imes. A u nace ha equi es special sample p epa a ion was selec ed and
designed. The e o e, a able p epa a ion p ocedu e was designed and op imized, making i possible o
epea edly p epa e iden ical able s wi h p ecise pa ame e s o his ype o o en. The esul ing able
weigh was 73 mg a a densi y o 2.285 g/cm3, which was comp essed o a cons an olume using an
oil and g aphi e comp ession olle and a hand p ess. The i ing o he able in a u nace wi h a
manipula o using sho i ing imes ook place unde iden ical condi ions and he ob ained esul s
show ha all p ocesses ake place e y quickly. The used u nace wi h a manipula o is he e o e
sui able and usable o he s udy o he cou se o iclinic ali e o ma ion a sho soaking imes.
5. Re e ences
[1] Je e y J W 1954 The icalcium silica e phase P oc. o he 3 d ISCC (London) p 30–48

Young Scien is 2021
IOP Con . Se ies: Ma e ials Science and Enginee ing 1209 (2021) 012045
IOP Publishing
doi:10.1088/1757-899X/1209/1/012045
6
[2] Kondo E R and Choi S 1968 Mechanism and kine ics o Po land cemen o ma ion o an
example o he solid-s a e eac ion in he p esence o a liquid phase P oc. 5 h ISCC
(London)
[3] Taylo H F W 1997 Cemen chemis y 2nd ed (London: Thomas Tel o d Publishing) p 459
[4] Hewle P 2004 Lea´s Chemis y o Cemen and Conc e e 4 h ed (Ams e dam: Else ie ) p 1088
[5] S anek T and Sulo sky P 2002 The in luence o he ali e polymo phism on he s eng h o he
Po land cemen Cemen and Conc e e Resea ch 32 7 p 1169-75
[6] Li X, Ouzia A and Sc i ene K 2018 Labo a o y syn hesis o C3S on he kilog am scale Cemen
and Conc e e esea ch 108 p 201-7
[7] Ch omý S and Za adil M 1980 Labo a o ní a ýpoče ní echnika: Pec s manipulá o em p o
izo e mní ýpaly labo a o ních zo ků p 62 - 65
Acknowledgmen s
We acknowledge he inancial suppo o p ojec ʺS udy o c ys alliza ion kine ics o a ious
polymo phs o icalcium silica eʺ (FAS -J-21-7309).