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Ma e ials and S uc u es (2025) 58:103
h ps://doi.o g/10.1617/s11527-025-02634-9
ORIGINAL ARTICLE
E ec o nano silicon ni ide on hemic os uc u al
cha ac e is ics andmechanical p ope ies
o ul a‑high‑pe o mance s eel ibe ein o ced conc e e
J.D.RuizMa ínez· J.D.Ríos·
E.M.Pé ez‑So iano· H.Ci uen es· C.Lei a
Recei ed: 28 No embe 2024 / Accep ed: 11 Ma ch 2025
© The Au ho (s) 2025
wi h he ma ix. This, in u n, educed mac opo os-
i y a ound he ibe s, enhancing he ma ix in eg i y.
TGA indica ed a educ ion in ee calcium hyd ox-
ide, co obo a ing he obse ed s eng hening o he
ma ix. Fu he mo e, he addi ion o 0.75 w % NSIN
yielded he op imal esul s, wi h a 17.3% imp o e-
men in comp essi e s eng h and a 66% inc ease
in c ack p opaga ion esis ance du ing he elas ic
phase. These esul s highligh he po en ial o NSIN
as a nano- ein o cemen o signi ican ly imp o e
he mechanical and mic os uc u al p ope ies o
UHPFRC.
Keywo ds Ul a-high-pe o mance conc e e· S eel
ibe - ein o ced conc e e· Nano silicon ni ide·
F ac u e· Fibe -ma ix in e ac ion
1 In oduc ion
Ul a-high-pe o mance ibe - ein o ced conc e e
(UHPFRC) is conside ed one o he mos p omising
cons uc ion ma e ials o u u e sus ainable and
esilien in as uc u es due o i s high comp essi e
s eng h (abo e 120 MPa) and supe io lexu al
ensile s eng h (15–20 MPa) compa ed o
con en ional conc e e [1–4]I also has ema kable
ene gy abso p ion capaci y and duc ili y hanks o i s
ein o cemen , which ypically consis s o s eel ibe s
in quan i ies a ound 2% by olume [3, 5]. Howe e ,
despi e i s ema kable pe o mance, UHPFRC aces
Abs ac This s udy in es iga es he inco po a-
ion o an inno a i e nano- ein o cemen , nano sili-
con ni ide (NSIN), o enhance he wo kabili y and
mechanical pe o mance o ul a-high-pe o mance
ibe ein o ced conc e e. The addi ion o NSIN a
dosages o 0.25, 0.5, 0.75, and 1.5 w % o cemen
was analyzed o e alua e i s impac on he dis ibu-
ion and in e ac ion be ween s eel ibe s and he
cemen i ious ma ix. Expe imen al analyses, includ-
ing he mog a ime ic analysis (TGA), ansmission
elec on mic oscopy (TEM), and scanning elec on
mic oscopy (SEM), we e conduc ed o es ablish a
ela ionship be ween he mic os uc u al modi ica-
ions, ibe -ma ix in e ac ions, and he esul ing
mechanical beha io . The indings e ealed ha NSIN
inc eased wo kabili y and ex ended se ing ime, ena-
bling imp o ed s eel ibe dispe sion and in e ac ion
J.D.RuizMa ínez· C.Lei a(*)
Depa men o Chemical andEn i onmen al Enginee ing,
Escuela Técnica Supe io de Ingenie ía, Uni e sidad de
Se illa, 41092Se ille, Spain
e-mail: clei [email p o ec ed]
J.D.Ríos· H.Ci uen es(*)
Depa men o Con inuum Mechanics andS uc u al
Analysis, Escuela Técnica Supe io de Ingenie ía,
Uni e sidad de Se illa, 41092Se ille, Spain
e-mail: [email p o ec ed]
E.M.Pé ez-So iano
Depa men o Ma e ials Science andEnginee ing
andT anspo , Escuela Poli écnica Supe io , Uni e sidad
de Se illa, 41011Se ille, Spain
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challenges such as low wo kabili y, e a ic ma ix
ibe in e ac ion, and limi ed ibe e icacy, which
can educe i s po en ial mechanical p ope ies and
du abili y [4, 6].
Addi ionally, ibe -ma ix in e ac ion is a key ac o
a ec ing he s eng h o he UHPFRC because he
s ess is ans e ed h ough he ibe -ma ix in e ace
[7]. Fu he mo e, Rios e al. [3, 4] concluded ha he
highes concen a ion o po es is dis ibu ed a ound
he s eel ibe . The e o e, imp o ing he in e ac ion
be ween ibe and ma ix is c ucial o imp o ing he
mechanical p ope ies o conc e e.
On he o he hand, because o hei la ge speci ic
su ace a ea, nanoma e ials exhibi a a ie y o
special beha io s wi hin he conc e e, including he
pozzolanic eac ion, he nuclea ion e ec and pa icle
illing e ec [8–10]. P e ious s udies ha e shown ha
he addi ion o nanoma e ials, such as SiO₂, CaCO₃,
Al2O3, TiO2, Fe2O3, g aphene oxide and ca bon
nano ubes can imp o e he mechanical p ope ies
o UHPC by enhancing he hyd a ion p ocess and
educing po osi y [11, 12]. Because o hei ensile
s eng h and high elas ic modulus, nanoma e ials
including ca bon nano ubes, nano ibe s and g aphene
nanopla ele s (GNPs) ha e been used o imp o e he
mechanical p ope ies o cemen i ious composi es
[13–15]. Mo eo e , nanopa icles ha e been
included in cemen -based ma e ials o enhance hei
mechanical p ope ies h ough chemical eac ions o
physical illing [16]. The chemical composi ion and
la ge speci ic su ace a ea o nanoma e ials acili a e
and accele a e cemen hyd a ion nuclea ion si es,
inc easing pozzolanic in e ac ions wi h po landi e
(CH) and consequen ly p oducing g ea e quan i ies
o calcium silica e hyd a e (C–S–H) gel [17–20]. The
p opo ion o po landi e-Ca(OH)2 in he conc e e
combines wi h nanopa icles o p oduce a dense
conc e e ma ix [21–23].
Rega ding UHPFRC imp o ed wi h
nanopa icles, No has i e al. [24] ound ha he
addi ion o 1% nano me akaolin had an op imal
e ec on comp essi e s eng h. Wu e al. [11, 25]
enhanced he mechanical p ope ies o UHPC
wi h he addi ion o nano-SiO2 and nano-CaCO3,
bu his e ec dec eased beyond alues o 1% and
3.2% espec i ely, because he educ ion o he
wo kabili y. This was asc ibed o a highe olume
o en apped ai and capilla y oids. By con as ,
Camile i e al. [26] ound ha he addi ion o
nano-limes one educed se ing ime and Gha a i
e al. [12] epo ed ha nano-SiO2 educed he
wo kabili y o UHPC due o he shape and s uc u e
o he nanopa icles. While p e ious s udies ha e
ocused on nanopa icles such as SiO₂, CaCO₃,
Al2O3, TiO2, Fe2O3, g aphene oxide and ca bon
nano ubes o modi y UHPFRC p ope ies [11, 12,
20, 23, 27], his esea ch in es iga es nano-silicon
ni ide (NSIN) as a no el nano- ein o cemen .
NSIN p esen s a unique combina ion o p ope ies:
i s sphe ical mo phology enhances wo kabili y, i s
nano- illing e ec e ines he ma ix s uc u e, and
i s in e ac ion wi h hyd a ion p oduc s con ibu es
o u he s eng hening he composi e.
Nano-Si3N4 (NSIN) has demons a ed excep ional
mechanical quali ies, high ha dness and obus
wea esis ance in cemen -based ma e ials [28]. By
using NSIN, Zhang and Wang we e able o de elop
ce amic ool ma e ials wi h good cu ing wea
quali ies [29]. Acco ding o Sun e al. [30], adding
NSIN can inc ease he bending s eng h and wea
esis ance o ce amics. Zhu e al. [28] concluded ha
he su ace e ec , illing e ec and g ea e su ace
ene gy o NSIN a e he p ima y componen s o i s
ac ion mechanism, which enhances he mechanical
quali ies o cemen -based ma e ials. Yin e al. [31]
used β-Si3N4 whiske s in Cu composi es, esul ing in
enhanced composi e ha dness and bending s eng h.
Howe e , he use o NSIN in UHPFRC has no
been ex ensi ely explo ed, explo ed in conc e e,
only in some ce amic compounds [32], p esen ing
a no el oppo uni y o ad ance he unde s anding
o nano- ein o ced cemen i ious composi es. This
s udy aims o ill his gap by in es iga ing he e ec s
o NSIN on he mic os uc u al and mechanical
p ope ies o UHPFRC, wi h a ocus on imp o ing
wo kabili y, ibe in e ac ion, and c ack esis ance.
This pape p esen s an expe imen al analysis o he
beha io o UHPFRC composi es wi h a ying NSIN
concen a ions. Fou dosages, anging om 0.25 o
1.5 w %, we e es ed. Me cu y in usion po osime y,
he mog a ime ic analysis and s e eomic oscopy
cha ac e ized he ma ix po e size dis ibu ion and
composi ion. Mechanical and ac u e pa ame e s
we e de e mined using es ablished expe imen al
p ocedu es. The s udy s a es a ela ionship be ween
mechanical p ope ies and cha ac e iza ion da a,
analyzing how NSIN addi ion modi ies he ma ix
mic os uc u e, enhancing wo kabili y, ibe -ma ix
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in e ac ion, and s eel ibe o ien a ion, hus impac ing
he conc e e’s ac u e and mechanical cha ac e is ics.
2 Ma e ials andspecimen p epa a ion
2.1 Ma e ials
Type I 52.5 R/SR cemen complian wi h he EN
197–1 s anda d [33] was used o manu ac u e he
specimens o ul a-high-pe o mance s eel ibe -
ein o ced conc e e. Silica ume (SF) wi h a speci ic
su ace a ea o 92 m2/g and G ound-g anula ed blas -
u nace slag (GGBS) we e used. Se e al s udies ha e
demons a ed he bene i s o using slag in UHPC.
Fo example, [34, 35] ound ha he combina ion
o slag and silica ume in UHPC esul ed in a
dense mic os uc u e, imp o ed mechanical
p ope ies and du abili y p ope ies, educing he
CO2 emissions associa ed o he high amoun o
cemen use. The e o e, he inclusion o slag in ou
s udy was based on i s p o en abili y o imp o e he
pe o mance o UHPC, pa icula ly when combined
wi h o he ma e ials and p ope mix design.
Fo he agg ega es, wo a ie ies o qua z
sand we e added: ine sand (FS) wi h a maximum
pa icle size o 0.315 mm, and coa se sand (CS)
wi h pa icles below 0.800 mm. S eel ibe s wi h
a leng h o 13 mm and a diame e o 0.2 mm we e
used. A polyca boxyla e-based supe plas icize (SP)
and NSIN wi h a pu i y o o e 98% we e used. The
chemical composi ions o he binde aw ma e ials
we e analyzed using X- ay luo escence spec ome y
(XRF), wi h de ailed esul s p esen ed in Table1.
The NSIN powde was analyzed using a ZEISS
LIBRA 120 ansmission elec on mic oscope (TEM)
o de e mine he mo phology o i s nanopa icles.
Figu e1 depic s he esul s ob ained ia TEM, which
con i med he p edominan ly sphe ical mo phol-
ogy o he pa icles, wi h an app oxima e diame e
o 50 nm. Addi ionally, pa icle agglome a ion was
obse ed, unde sco ing he need o use speci ic dis-
pe sion echniques o achie e a uni o m dis ibu ion
and p e en agglome a ion. Al hough NSIN could be
mo e easily inco po a ed in o cemen -based ma e ials
wi h lowe ene gy consump ion h ough con en ional
mixing p ocesses [28], in his esea ch we op ed o
dispe sion ia ul asonica ion o ob ain op imal dis-
pe sion [36].
The mic os uc u e o he UHPFRC ma ix and
he dis ibu ion o nano silicon ni ide (NSIN) pa i-
cles we e analyzed using a Hi achi S5200 scanning
elec on mic oscope (SEM) equipped wi h Ene gy-
Dispe si e Spec ome y (EDS). SEM wi h EDS was
Table 1 XRF chemical composi ion o he binde aw ma e i-
als
Cemen GGBS SF
Loss on igni ion
(LOI)
19.42 17.39 18.97
Al2O36.59 9.83 0.20
BaO 0.06 – –
CaO 45.61 35.12 0.30
Cl2O30.07 – –
CuO 0.04 – –
Fe2O32.85 0.31 0.06
K2O 1.09 2.01 0.42
MgO 1.00 6.63 0.35
MnO20.05 0.11 –
Na2O 0.29 0.21 0.12
P2O50.13 – –
SiO218.29 27.81 79.58
SO34.02 – –
S O 0.05 0.08 –
TiO20.41 0.48 –
ZnO 0.02 – –
Fig. 1 TEM image o NSIN pa icles
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chosen in his s udy because i allowed us o ob ain
high- esolu ion images o he ma ix mic os uc u e
while simul aneously pe o ming elemen al mapping
o con i m he p esence and dis ibu ion o NSIN
pa icles. This app oach p o ided a comp ehensi e
unde s anding o he in e ac ion be ween he NSIN
pa icles and he cemen i ious ma ix.
2.2 Mix p opo ions and specimen p epa a ion
Fi e di e en mixes o UHPFRC ha di e ed only
in NSIN con en we e manu ac u ed. Table2 shows
he designa ion o he i e mixes and he p opo ion
o cons i uen s o each. The i s mix NSIN- 0,
con ained no NSIN and was he e e ence mix. Fo
he o he mixes, NSIN was added in he ollowing
p opo ions: 0.25 w %, 0.50 w %, 0.75 w %, and 1.50
w %, espec i ely.
The manu ac u ing p ocess o hese ypes o
conc e es plays a c ucial ole in he inal p ope ies o
he ma ix, which is why i is de ailed below. Ini ially,
NSIN was added o he mixing wa e along wi h
he supe plas icize , and mode a e sonica ion was
applied o he mix. Speci ically, an ULTRASONS
3000513 de ice wi h a powe o 150 W was used o
30 min o imp o e he dispe sion o NSIN pa icles
in he wa e . In addi ion, he solid ma e ials—cemen ,
silica ume, blas u nace slag, ine and coa se
agg ega es—we e mixed o 5min in a e ical mixe
o achie e a homogeneous solid mix. Subsequen ly,
all cons i uen s, bo h solid and liquid, we e combined
in he mixe and mixed o an addi ional 20 min un il
he desi ed wo kabili y was achie ed. Nex , s eel
ibe s we e added and mixed o i e mo e minu es.
Fo each o he i e mixes, h ee 40 × 40 × 160 mm3
p isms we e cas . A e 24 h, he samples we e
demolded and subjec ed o a u he cu ing pe iod
o 25 days subme ged in wa e a oom empe a u e.
Nex , he samples we e le o d y o 48 h.
3 Expe imen al p og am
3.1 The mog a ime ic analysis
Specimens ha e been s o ed in sealed bags o a oid
ca bona ion a e cu ing ime, hen samples weighing
100–150 mg was collec ed om he su ace o
he samples o he TG SDTA measu emen s. A
he mog a ime ic analysis (TG-SDTA Me le -
Toledo 851) was conduc ed om oom empe a u e
o 900 °C. A hea ing a e o 10 °C/min was chosen,
using N2 as he pu ging gas, consis en wi h s anda d
p ac ice [37, 38].
3.2 Wo kabili y
A downscaled slump es was de ised o e alua e
he wo kabili y o esh conc e e, ollowing he
p ocedu es ou lined in he EN 12350–2:2020 [39]
s anda d. Each es was pe o med on a la aluminum
shee using a s eel mini-slump cone. The se up o
he mini-slump es in his s udy in ol ed a modi ied
Ab ams cone geome y wi h dimensions o 50 mm a
he op, 100 mm a he bo om and 150 mm in heigh .
The esh conc e e was p omp ly in oduced in o
he mini-slump cone and g adually li ed o minimize
ine ial impac s. Following he usual p o ocol,
measu emen s we e made using a s anda d gauge
and a e aged ac oss ou eadings wi h a p ecision
o one millime e . The sel -compac ing abili y o he
conc e e was de e mined using he a e age alue o
he low ex ension acco ding o he speci ica ions and
guidelines o sel -compac ing conc e e [40]
3.3 Ini ial and inal se ing ime
The ini ial and inal se ing imes o he UHPFRC
mix u es we e de e mined in acco dance wi h
he EN 196–3 s anda d [41], which speci ies he
Table 2 Mix p opo ions
and designa ion Cons i uen (kg/m3)
Mix Cemen SF GGBS FS CS Wa e SP S eel ibe s NSIN
NSIN- 0 540 210 310 470 470 205 42 196 0
NSIN- 0.25 540 210 310 470 470 205 42 196 1.35
NSIN- 0.50 540 210 310 470 470 205 42 196 2.70
NSIN- 0.75 540 210 310 470 470 205 42 196 4.05
NSIN- 1.50 540 210 310 470 470 205 42 196 8.10
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p ocedu e o measu ing he se ing imes o cemen
pas es using he Vica needle me hod. Addi ion-
ally, he EN 480–2:2007 [42] s anda d, which ou -
lines he es me hods o de e mining he se ing
ime o conc e e admix u es, was also ollowed o
ensu e consis ency and accu acy. The ini ial se ing
ime was de ined as he ime when he Vica nee-
dle pene a ed he cemen pas e o a dep h o 6 ±
3mm, while he inal se ing ime was iden i ied as
he ime when he needle could no longe pene a e
mo e han 0.5 mm in o he pas e. These measu e-
men s we e conduc ed a a con olled empe a u e
o 20 °C o simula e eal-wo ld condi ions.
3.4 S eel ibe —ma ix in e ac ion
A SMZ25 Nikon s e eomic oscope (New Yo k,
USA) was used o his s udy. I was connec ed o a
compu e equipped wi h NIS-Elemen s BR so wa e
o image cap u e.
The s udy in ol ed he ca e ul manu ac u ing o
small speci ic specimens measu ing 20 × 40 × 40
mm3, main aining he in eg i y o he unmolded
su ace. This p ecau ion ensu ed he iden i ica ion
o ma ix- ibe in e ac ions, allowing o he isual
de ec ion o any disce nible impac s o NSIN on
he UHPFRC. S e eomic oscopic imaging enables
o a wide ield o iew, exac mic oscopic ea u es
in 3D, and quan i a i e measu es [43–45]. The
esul s o his me hodology a e consis en wi h
p io esea ch [46–49], demons a ing he me hod’s
use ulness o in es iga e ibe -ma ix bonding
in UHPRC. Alongside image magni ica ion, he
equipmen gene a ed a 3D model o he image and
a Z-axis g aph, o e ing mic ome ic p ecision o
illus a e he a e age p o ile o he mix’s su ace.
3.5 Po osi y
Po osi y was assessed wi h a Mic ome i ics
Au opo e IV (No c oss, USA) me cu y in usion
po osime e . Po e size anged om 0.007 o 150
μm. To p epa e he samples, 5 mm pelle s we e
o med and hen subjec ed o d ying in an o en a
105 °C un il a cons an mass was ob ained.
3.6 Mechanical p ope ies
3.6.1 Comp essi e s eng h
Fo each ype o mix, h ee 80 × 40 × 40 mm3
specimens we e used o assess comp essi e s eng h
in acco dance wi h he EN 12390–3 s anda d [50].
A 3000 kN load capaci y se o-hyd aulic es ing
machine was used o his es .
3.6.2 Flexu al s eng h
All he conc e es designed in his s udy unde wen
h ee-poin bending es s. The es s we e conduc ed
acco ding o he EN 14651 s anda d [51]. The
dimensions o he specimens p epa ed o hese
es s we e 40 × 40 × 160 mm3, simila o p e ious
s udies [11, 52]. All specimens we e no ched a he
cen e o a dep h equi alen o 1/6 o hei wid h.
The use o no ched specimens wi h a no ch dep h o
1/6 o he specimen wid h is widely accep ed in he
s udy o UHPFRC [53, 54]. This me hod e ec i ely
cap u es he ma e ial’s esponse o c acking and ibe
b idging, p o iding aluable insigh s in o he lexu al
beha io o UHPFRC. By ollowing his s anda dized
app oach, we ensu e ha ou esul s a e compa able
o hose o o he s udies and ha ou indings can
be eliably applied o he design and e alua ion o
UHPFRC in p ac ical applica ions.
Du ing he es , measu ing ins umen s included
a 10-mm e ical ansduce o eco d he de lec ion
a he cen e o he specimen and a 5 mm clip gauge
o measu e he CMOD. The expe imen s we e
conduc ed using a se o-hyd aulic machine capable
o wi hs anding a maximum load o 3000 kN, using
CMOD displacemen con ol. An i- o sion de ices
we e ins alled on he loading and suppo olle s.
The es s and esul s we e conduc ed acco ding he
EN 14651 s anda d [51], whe e he esidual s eng h
is calcula ed using Eq. (1):
whe e Rj and Pj ep esen he esidual lexu al ensile
s eng h and he applied load, espec i ely, co e-
sponding o CMODj. Speci ically, R1, R2, R3 and R4
we e calcula ed using he ma ching CMOD alues o
(1)
Rj=
3P
j
L
2bh2
sp
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0.5 mm, 1.5 mm, 2.5 mm and 3.5 mm, espec i ely.
In Eq. (1), b is he wid h o he beam, hsp is he heigh
o he beam excluding he no ch heigh , and L is he
span leng h (Fig.2).
4 Resul s anddiscussion
4.1 The mog a ime ic analysis
The TGA cu es, p esen ed in Fig.3, show he a ia-
ion o mass loss (%) and hea low (mW) om oom
Fig. 2 SEM image and EDS o he UHPFRC ma ix: a iden i ica ion o C-S–H gel and NSIN pa icles; b elemen al composi ion
mapping o NSIN pa icles
Fig. 3 The mog a ime ic
analysis o NSIN- 0, NSIN-
0.75 and NSIN- 1.5 a 28
days
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empe a u e o 900 °C. Se e al peaks can be obse ed
in hea low.
In he i s s age (20–250 ºC), an endo he mic
peak obse ed (50 ºC) co esponds o he e apo a ion
o mois u e and wa e in capilla y po es [55, 56],
ollowed by he dehyd a ion o C–S–H gel a 150 °C.
Figu e3 shows ha a highe NSIN dose accele a ed
he cemen hyd a ion eac ion h ough he nuclea ion
e ec (as seen in Fig. 2), esul ing in a lowe mass
loss o 3.83% in NSN- 0 compa ed NSN- 1.5., while
NSIN- 0.75 emains a pa i y.
In he second s age (250–500 ºC), an endo he mic
peak a 450 °C was due o he decomposi ion o
calcium hyd oxide [56]. The addi ion o NSIN slowed
down he decomposi ion o Ca(OH)2, wi h mass
loss dec easing o 2.56% in NSIN- 1.5 and 2.05% in
NSIN- 0.75.
In he hi d s age (500–800 ºC), a peak in he
he mog a ime ic da a a 580 °C e ealed a mass
loss o 2.94% in NSIN- 0, while NSIN composi ions
eached 2.34% in NSIN- 0.75 and 2.56% in NSIN-
1.50. This indica es ha NSIN helped p e en he
decomposi ion o calcium ca bona e [57, 58].
In he las s age (800–900 ºC), weigh loss
occu ed due o he loss o OH − esiduals. Unlike
all o he peaks, his las eac ion in he composi ions
con aining NSIN was exo he mic [58].
The he mog a ime ic analysis (TGA) e ealed
ha he addi ion o nano silicon ni ide (NSIN)
signi ican ly educes he con en o ee calcium
hyd oxide (CH) and p omo es he o ma ion
o addi ional calcium silica e hyd a e (C–S–H)
gel, leading o a dense and mo e homogeneous
ma ix. This educ ion in CH con en is consis en
wi h he obse ed imp o emen s in comp essi e
s eng h and c ack esis ance, as a dense ma ix
p o ides be e s ess ans e and educes he
o ma ion o mac opo osi y [55]. Addi ionally,
he TGA esul s showed ha NSIN helps s abilize
he calcium ca bona e (CaCO₃) con en , educing
i s decomposi ion a high empe a u es. This
s abiliza ion is likely due o he ille e ec o
NSIN, which educes he po osi y and imp o es he
he mal s abili y o he ma ix [58]. These indings
a e suppo ed by p e ious s udies [59], which also
obse ed simila imp o emen s in he mal s abili y
and mechanical pe o mance wi h he addi ion o
nanoma e ials in cemen -based ma e ials.
4.2 Wo kabili y
The ou comes o he slump es s o each mix a e
depic ed in Fig.4. As illus a ed, i is e iden ha he
slump alues did no ollow a linea ela ionship wi h
he di e en NSIN dosages used. Ins ead, a cu e was
o med ha ini ially showed a la ge slump adius
wi h inc easing NSIN, achie ing a highe wo kabil-
i y (14.4% g ea e han NSIN- 0) wi h he inclusion
o NSIN a 0.75%. This may be due o a ball-bea -
ing e ec o he sphe ical g anula e shape o NSIN
Fig. 4 Mini-slump low
measu emen s we e con-
duc ed in UHPFRC samples
con aining a ying NSIN
con en s
Ma e ials and S uc u es (2025) 58:103
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(Fig.1) wi hin he conc e e [48]. Ne e heless, a he
highes NSIN dosage (1.5%), an opposi e end was
obse ed, wi h he slump alue dec easing o a le el
like ha o he mix wi hou NSIN. This sugges s ha
o e sa u a ion o NSIN hinde s u he imp o emen
in wo kabili y.
Addi ionally, all mixes demons a ed sel -
compac ing p ope ies. This indica es he conc e e’s
abili y o low and ill o mwo k unde i s sel -
weigh , e en in he p esence o dense ein o cemen ,
wi hou he need o ib a ion, main aining uni o m
consis ency h oughou [49].
4.3 Ini ial and inal se ing ime
As depic ed Table3, a ia ions in se ing imes we e
obse ed ac oss di e en NSIN dosages. Speci ically,
he e was a 2.58-h di e ence in ini ial se ing
ime be ween NSIN- 0 and NSIN- 1.5, sugges ing
a p opo ional a ia ion depending on he NSIN
dosage. The dispa i ies we e mo e ma ked in he
inal se ing ime, wi h composi ions con aining
mo e NSIN se ing 2.65 h (NSIN- 0.75) and 5.3 h
(NSIN- 1.5) la e han NSIN- 0, showing a signi ican
inc ease o 20% and 40.1% espec i ely.
The esul s show ha he addi ion o NSIN signi i-
can ly educed bo h he ini ial and inal se ing imes.
Fo example, he ini ial se ing ime dec eased om
8.10 h o he e e ence mix (NSIN- 0) o 5.52 h o
he mix wi h 1.5% NSIN. Simila ly, he inal se ing
ime dec eased om 12.80 h o NSIN- 0 o 7.50 h o
NSIN- 1.5. This educ ion in se ing ime is a ibu ed
o he nuclea ion e ec o NSIN, which accele a es
he hyd a ion p ocess by p o iding addi ional si es o
he o ma ion o hyd a ion p oduc s. These indings
a e consis en wi h p e ious s udies [60], which also
obse ed a educ ion in se ing imes wi h he addi-
ion o nanoma e ials in cemen -based ma e ials.
Mo eo e , he gap be ween ini ial and inal se ing
imes con ac ed wi h highe NSIN concen a ions,
dec easing by 14.89% o he lowes NSIN addi ion
and by 42.12% o he highes NSIN con en . These
indings unde sco e he ole o NSIN in dec easing
bo h ini ial and inal se ing imes, hus na owing
he ime in e al be ween hem. These empo al shi s
sugges consequen ial al e a ions in he physical and
mechanical cha ac e is ics o he composi ions.
4.4 S eel ibe —ma ix in e ac ion
Figu e5 shows images o he in e ac ion be ween a
s eel ibe and he cemen i ious ma ix. Ini ially, i
was challenging o disce n he in luence o NSIN.
Table 3 Se ing imes a 20 ºC
Mix Ini ial se ing ime (h) Final
se ing ime
(h)
NSIN- 0 8.10 12.80
NSIN- 0.25 7.50 11.50
NSIN- 0.50 7.05 11.10
NSIN- 0.75 6.55 10.15
NSIN- 1.5 5.52 7.50
Fig. 5 Images wi h hei espec i e 3D modeling o each mix
o NSIN: a NSIN- 0, b NSIN- 0.25, c NSIN- 0.50, d NSIN-
0.75, and e NSIN- 1.5
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None heless, he p o ile o med jus be o e he eme -
gence o he s eel ibe , depic ed a he cen e o
Fig.5, p o ides compelling e idence o a co ela ion
be ween NSIN dosage and he expanded conc e e
a ea su ounding he ibe . This expanded a ea indi-
ca es enhanced adhesion and in eg a ion o he s eel
ibe wi hin he ma ix, likely a ibu able o he a y-
ing NSIN dosages.
Resul s depic ed in Fig.6 suppo he hypo hesis
ha he addi ion o NSIN, due o i s pa icle- illing
and in e ace e ec s [8, 9], po en ially inc eased he
su ace a ea o he ibe embedded in he ma ix.
Fu he mo e, i was in e ed ha , in UHPFRC wi h
app oxima ely 2% s eel ibe s, he luidiza ion o he
cemen i ious ma ix helped o achie e a mo e uni o m
dis ibu ion o s eel ibe s, he eby mi iga ing signi i-
can po es and po en ially enhancing he mechanical
p ope ies o he specimens.
I is impo an o no e he clea and di ec
ela ionship obse ed in Figs. 4 and 6. Bo h es s
showed ha , as he NSIN con en inc eased,
wo kabili y also inc eased, esul ing in a g ea e
in e ac ion su ace be ween he ma ix and he ibe .
By con as , an opposi e end was obse ed in he
composi ion wi h he highes NSIN con en (NSIN-
1.5), which may be explained by an o e sa u a ion
o NSIN, sugges ing an op imal poin below he
1.5% addi ion. Despi e his, he in e ac ion su ace
emained la ge han ha o he e e ence sample.
The s e eomic oscope images (Fig. 6) e ealed
ha NSIN imp o ed he ibe -ma ix in e ac ion,
educing gaps be ween he ibe s and he ma ix. This
imp o emen is a ibu ed o he e is a highe local
ic ion be ween ma ix and ibe s when NSIN due
o he lowe po osi y a ound he ibe (Fig. 5), and
he e o e, he g ea e o ce o he pull-ou o he s eel
ibe s om he ma ix is necessa y.
The addi ion o NSIN signi ican ly enhanced he
hyd a ion p ocess and e ined he po e s uc u e o
he UHPFRC ma ix, as e idenced by he s e eomi-
c oscope and po osime y esul s (Figs.6 and 7). This
imp o emen in ibe -ma ix in e ac ion is a ibu ed
o he nuclea ion e ec o NSIN, which p o ides
addi ional si es o he o ma ion o hyd a ion p od-
uc s, accele a ing he ea ly-age hyd a ion p ocess, as
shown in TGA (Fig.3). These indings a e consis en
wi h p e ious s udies [11], which also obse ed ha
nanoma e ials can enhance he hyd a ion p ocess and
e ine he po e s uc u e o cemen -based ma e ials.
Fu he mo e, he imp o ed ibe -ma ix in e ac ion
obse ed in his s udy aligns wi h p e ious esea ch
on he impo ance o ibe in e ac ion in UHPFRC.
Huang e al. [61] demons a ed ha be e ibe -
ma ix in e ac ion co ela es wi h inc eased lexu al
Fig. 6 S e eomic oscope
images de ailing he a e age
ibe -ma ix in e ac ion
ela ed o 3D images
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ad anced damage s ages in he ma ix. Fu he mo e,
he addi ion o NSIN, which imp o ed ibe -ma ix
adhesion (see Fig.6), imp o ed esidual s eng hs in
he la e s ages R3 and R4.
Figu e 14 illus a es he ela ionship be ween
esidual s eng hs and NSIN con en . Each se o ba s
in he diag am shows he pe cen age o imp o emen
o each esidual s eng h compa ed o i s equi alen
alue in he NSIN- 0 diag am (ligh blue). A signi i-
can imp o emen in all esidual s eng hs was e iden
when he ma ix was supplemen ed wi h NSIN. The
0.5 w % con en showed he mos no able inc eases in
esidual s eng hs.
The mos signi ican imp o emen was eco ded
o R3 and R4 in NSIN- 0.5, wi h inc eases o 103%
and 99%, espec i ely. This beha io was a ibu ed
Fig. 13 Rela ionships
be ween he esidual
s eng hs and he ibe -
ma ix in e acial su ace
Fig. 14 Rela ionships
be ween esidual s eng hs
and NSIN con en
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o he combina ion o a high LOP (Fig.11.a) and an
inc eased ibe -ma ix in e acial a ea (Fig. 6). I is
impo an o highligh he c ucial ole o ein o cing
he ma ix wi h NSIN in he pos -c acking beha io
o s eel ibe - ein o ced conc e es.
4.6.5 In luence o LOP and ibe ‑ma ix in e acial
su ace onene gy abso p ion capaci y
This esea ch also explo ed how he LOP and he
ibe -ma ix in e acial su ace in luenced ene gy
abso p ion capaci y in UHPFRC ein o ced wi h
NSIN. Figu e 15 p esen s he esul s o he linea
eg ession analysis be ween he i s esidual s eng h
a a CMOD o 0.5 mm and he subsequen esidual
s eng hs a la ge no ch openings o 1.5, 2.5 and 3.5
mm CMOD. I was obse ed ha R2 and R3 exhibi ed
a e y high linea co ela ion wi h R1, wi h R2 alues
o 0.95 and 0.99, espec i ely. Howe e , his co ela-
ion was weak o R4, wi h an R2 alue o 0.56.
The high co ela ions be ween R2 and R3 on one
side and R1 on he o he we e due o he ac ha ,
o small CMOD openings whe e ma ix damage
mainly mani es ed as mic oc acking, esidual
s eng h was mo e dependen on he ma ix’s
p ope ies (i.e., po osi y, ibe dis ibu ion and
o ien a ion). Fo R4 (3.5 mm CMOD), he esis ance
mechanism was qui e di e en . I was cha ac e ized
by mac oc acks in he ma ix whe e he ibe s we e
mo e ac i a ed, p ima ily esis ing ensile s esses
h ough b idging e ec s. This di e ence in he
esis ing mechanism explains he loss o co ela ion
wi h he ea lie s ages.
The abili y o abso b ene gy can be quan i ied by
he a e o dec ease, which co esponds o he slope
o he linea eg ession lines. Fo R2, he a e o
dec ease ela i e o R1 was 86%, o R3 i was 77%,
and o R4 i was 53%. This indica es ha he ene gy
abso p ion capaci y dec eased mode a ely o 1.5 and
2.5 mm openings bu d opped by abou hal o 3.5
mm openings, e lec ing he ex en o in e nal damage
in he ma ix.
A inal concep wo h highligh ing is ha he
highes esidual s eng h R1 was ob ained o he
NSIN- 0.50 ma e ial. Howe e , he highes LOP was
achie ed wi h NSIN- 0.75 (Fig.13). This is because a
less po ous ma ix is ini ially s onge bu also mo e
b i le. Thus, al hough i had a highe LOP, once his
i s c acking (LOP) was exceeded, R1 was eached
mo e quickly, as demons a ed by he esul s.
Figu e16 illus a es he ene gy abso p ion capaci y
de e mined om h ee-poin bending es s o UHP-
FRC modi ied wi h di e en NSIN con en s. Ene gy
abso p ion capaci y inc eased wi h NSIN con en up
Fig. 15 Rela ionships
be ween esidual s eng hs
R2, R3, R4 and R1
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o 0.75 w %. Howe e , i dec eased wi h a highe con-
en o 1.50 w %. This end was quali a i ely simi-
la o ha obse ed in comp essi e s eng h (Fig.9.a)
and in he LOP (Fig.11.a).
The ene gy abso p ion and CMOD cu es showed
a nonlinea ela ionship o all UHPFRCs, sugges ing
ha he a e o inc ease in ene gy abso p ion
dec eased as CMOD inc eased. Resul s sugges ed
ha he addi ion o NSIN o UHPFRC signi ican ly
imp o ed i s mechanical and ac u e beha io . This
imp o emen was due o wo undamen al easons:
he educ ion o mac opo es in he ma ix (Fig. 7),
leading o highe comp essi e s eng h and LOP; and
he inc ease in he ibe -ma ix in e acial su ace
a ea, which imp o ed ibe adhesion.
In he ini ial s ages o loading, in e nal s esses
gene a ed mic oc acks in he ma ix whose
p opaga ion was hinde ed by ibe s ac ing as
ba ie s. As mic oc acks coalesced and he c acks
widened (inc easing CMOD), he ibe s b idged
he gap be ween he c ack aces. The addi ion o
NSIN inc eased he ibe -ma ix in e acial su ace,
imp o ing ibe adhesion. Ne e heless, he e iciency
o ibe b idging dec eased as CMOD inc eased.
Fibe s can slip, s e ch, o e en b eak, educing
he ma e ial’s abili y o abso b addi ional ene gy
e ec i ely.
5 Conclusions
This s udy in es iga ed he e ec s o nano silicon
ni ide (NSIN) on he mic os uc u al and mechanical
p ope ies o ul a-high-pe o mance ibe - ein o ced
conc e e (UHPFRC). The mos signi ican indings
can be summa ized as ollows:
1. The addi ion o NSIN signi ican ly enhanced
he wo kabili y and ex ended he se ing ime o
UHPFRC, acili a ing ibe -ma ix in e ac ion.
This led o an inc ease o he ma ix a ound he
ibe s acco ding o S e eomic oscope analysis.
2. NSIN ac ed as bo h a pozzolanic ac i a o and
a ille agen , educing he p esence o capilla y
po es and mac opo es. This dual ole con ibu ed
o a 17.3% inc ease in comp essi e s eng h
and a ema kable 66% imp o emen in c ack
p opaga ion esis ance du ing he elas ic phase,
pa icula ly a an op imal dosage o 0.75 w %
NSIN.
Fig. 16 Ene gy abso p ion
capaci y and CMOD cu es
gene a ed om expe imen-
al h ee-poin bending es s
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3. The unique ela ionship be ween comp essi e
s eng h and lexu al pe o mance was a key
inding o his s udy. Speci ically, we obse ed
a linea inc ease o 4.37 MPa in he Limi
o P opo ionali y (LOP) o e e y 10 MPa
inc ease in comp essi e s eng h. This a e o
imp o emen is signi ican ly highe han hose
epo ed in p e ious s udies in ol ing o he
nanoma e ials.
4. The imp o emen in in e acial adhesion
was pa icula ly e iden in he pos -c acking
beha io , whe e esidual lexu al s eng hs (
alues) showed signi ican inc eases, especially
o la ge c ack openings (e.g., 103% and 99%
imp o emen s in 3 and 4, espec i ely).
5. The ene gy abso p ion capaci y o UHPFRC was
also enhanced by NSIN, wi h he op imal dosage
(0.75 w %) showing he highes pe o mance.
This imp o emen was a ibu ed o he combined
e ec s o educed mac opo osi y and enhanced
ibe -ma ix in e ac ion.
The addi ion o NSIN o e s a p omising
app oach o imp o ing he mechanical and
mic os uc u al p ope ies o UHPFRC,
pa icula ly in applica ions equi ing high
lexu al s eng h and c ack esis ance.
Funding Funding o open access publishing: Uni e sidad de
Se illa/CBUA. This esea ch was unded by he Spanish Minis-
y o Science and Inno a ion unde p ojec s numbe PID2019
- 110928RB-C33 and PID2023 - 147971OB-C32.
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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.
