Cement and Concrete Research 162 (2022) 106999

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Cement and Concrete Research

journal homepage: www.elsevier.com/locate/cemconres

Effect of diethanolisopropanolamine and ethyldiisopropylamine on

hydration and strength development of Portland cement
Yifei Wang a, b, Lei Lei b, *, Xiang Hu a, Yi Liu a, Caijun Shi a, c, **
a
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil Engineering, Hunan University,
Changsha 410082, PR China
b
Technische Universität München, Chair for Construction Chemistry, 85747 Garching, Lichtenbergstraße 4, Germany
c
Department of Civil Engineering, The University of British Columbia, 6250 Applied Science Lane, Vancouver, BC V6T 1Z4, Canada

A R T I C L E I N F O A B S T R A C T

Keywords: Diethanolisopropanolamine (DEIPA) and ethyldiisopropylamine (EDIPA) are new types of alkanolamines, which
DEIPA can be used in grinding aids or accelerators. Effect of DEIPA and EDIPA at different dosages (0.05 % and 0.5 %)
EDIPA on cement hydration and strength development is studied by compressive strength, heat evolution, X-ray
Hydration
diffraction (XRD), thermogravimetry (TG), 1H nuclear magnetic resonance (1H NMR) and scanning electron
AFm
Complexation
microscope (SEM). Results indicate that both dosages (0.05 %, 0.5 %) of DEIPA or EDIPA accelerated the hy­
Air entraining dration of aluminate (C3A), ferrite (C4AF), alite (C3S) and belite (C2S) due to their complexation effect. The main
Strength hydration peak was advanced and enhanced by 0.05 % of DEIPA or EDIPA, while it was significantly weakened
with 0.5 % of DEIPA or EDIPA incorporation due to the large formation of calcium monosulfoaluminate hydrate
(AFm). Compared with DEIPA, EDIPA under both dosages caused more AFm formation and led to lower hy­
dration degree of C3S and C2S at early ages, and possessed higher air entraining property to cause pore structure
degradation. However, EDIPA contributed to higher hydration degree of C3S and C2S at later ages due to its
higher steric hindrance than DEIPA. As a result, cement mortars with 0.05 % of DEIPA or EDIPA present higher
or comparable compressive strength compared to the reference sample, with DEIPA005 primarily increased the
early strength while EDIPA005 mainly increased the later strength. Whereas, DEIPA or EDIPA at higher dosage
(0.5 %) considerably decreased early strength of cement mortars, especially EDIPA.

1. Introduction negative effect on long-term strength development [5,6], due to its

Alkanolamines are important chemical admixtures in cement in­
dustry, which are popularly used in grinding aids due to their role in
surface activation of clinker particles and are sometimes used in accel­
erators and early strength enhancers for their effects on cement hydra­
tion [1–4].
The commonly used alkanolamines are triethanolamine (TEA), trii­
sopropanolamine (TIPA), DEIPA, EDIPA, etc. TEA under low dosages
(0.01–0.1 % by binder weight) increases the early strength, especially
the 1 d strength of cement-based materials [1,5,6], due to its accelera­
tion effect on the hydration of C3A to form ettringite (AFt) [7–9] and the
second hydration of C3A to form AFm [1,10]. It was also reported to
accelerate the dissolution and hydration of C4AF [7]. However, TEA has
retardation effect on C3S hydration [6,11,12]. Ramachandran [12]
speculated that the adsorption of TEA on hydrating C3S grains to form a
thick complex layer with low permeability led to the retarded C3S hy­
dration. Yaphary et al. [8] reported that 0.4 % of TEA promoted the
formation of TEA-AFt composite on the surface of C3S phase, which
impeded C-S-H nucleation and growth. Xu et al. [1] claimed that the
formation of the TEA-Ca2+ complex inhibited the growth of portlandite
(CH), thus delaying the hydration of C3S. Lu et al. [11] and Zhang et al.
[6] held the opinion that the accelerated aluminate reactions including
both C3A and C4AF hydration led to the retarded C3S hydration, which
can be described as the negative interference of aluminate reaction on
silicate reaction. With respect to the hydration products and micro­
structure, it was reported that the complexation effect of TEA with Ca2+

* Corresponding author.
** Correspondence to: C. Shi, Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil
Engineering, Hunan University, Changsha 410082, PR China.
E-mail addresses: wangyf@hnu.edu.cn (Y. Wang), lei.lei@tum.de (L. Lei), cshi@hnu.edu.cn (C. Shi).

https://doi.org/10.1016/j.cemconres.2022.106999
Received 4 May 2022; Received in revised form 25 September 2022; Accepted 30 September 2022
Available online 7 October 2022
0008-8846/© 2022 Elsevier Ltd. All rights reserved.
Y. Wang et al.
resulted in morphological changes of CH from large and parallel-stacked
lamellar shape to smaller and distorted actinomorphic one. Zhang et al.
[6] furtherly concluded that the formation of distorted actinomorphic
CH resulted in a loose structure of cement-based materials, thus
decreasing the long-term strength. Besides, it was reported that proper
dosages of TEA (0.06–0.08 %) enhanced the dissolution of Si4+ and Al3+
from lithium slag to promote the pozzolanic reaction, contributing to
denser microstructure and increased mechanical strength of lithium
slag-cement mortar [13].
TIPA significantly increases later strength development of cement-
based materials [14–16], which is attributed to its complexation with
Fe3+ to accelerate the hydration of C4AF [1,16,17]. Gartner and Myers
[17] reported that compressive strength of Portland cement with TIPA
was influenced by C4AF content in cement, and higher C4AF content
resulted in higher strength at 28 d. In addition to that, the higher steric
hindrance of TIPA compared to TEA hinders the adsorption of TIPA on
hydration products such as CH [17], leading to higher concentration of
TIPA in pore solution and higher hydration degree of C3S and C4AF at
later ages [18]. However, TIPA decreases the early strength of cement-
based materials although TIPA can accelerate aluminate reactions
(C3A and C4AF) [1,19,20]. It is explained that TIPA introduces gas into
cement matrix due to the lipophilicity of methyl groups, thus leading to
the increased porosity and decreased early strength [1,14]. At a high
dosage of 1 %, TIPA resulted in a loose and porous structure at early age
owing to the emergence of numerous AFm platelets and the reduction of
Ca(OH)2 crystals, exhibiting negative effect on strength development at
early and later ages [21]. Li et al. [22] reported that TIPA combined with
C-S-H seed/PCE nanocomposites mitigated the negative impacts of the
increased air content and AFm content caused by TIPA to increase the
early age strength at 12, 24 and 72 h. In addition, TIPA was reported to
accelerate the aluminates reaction, especially C4AF of limestone-
calcined clay cement (LC3), favoring the limestone reaction to form
more hydrocarboaluminates [23].
DEIPA and EDIPA are new types of alkanolamines, which can be used
in grinding aids and accelerators. So far very few studies have focused on
such alkanolamines, especially under relatively high dosages. Ma et al.
[24] reported that DEIPA promoted the hydration rate of the aluminate
and ferrite phases and the formation of microcrystalline CH at early
stages. An accelerator composed of calcium chloride and DEIPA could
increase early strength development of mortars by enhancing cement
hydration, with DEIPA enhancing primarily the aluminates hydration
(C3A and C4AF) [25]. Compared with TEA, DEIPA contributed to C4AF
hydration to a larger extent, indicating a stronger complexation with
iron ions [26]. Lu et al. [27,28] reported that EDIPA accelerated alu­
minates and C3S hydration and remarkably enhanced mechanical
properties of cement mortars at 28 d. It was also reported that DEIPA
and EDIPA promoted the early hydration of aluminate phases and the
later hydration of alite, contributing to both early and later strength
enhancement of cement mortars [1]. However, DEIPA and EDIPA
showed significant differences on strength development of cement
mortars, which needs further investigation. A systematic investigation
on hydration and strength development of Portland cement under the
common dosage of 0.05 % and a relatively high dosage of 0.5 % was
conducted by compressive strength, heat evolution, XRD/QXRD, TG, 1H
NMR and SEM. It is expected to associate hydration and microstructure
of Portland cement with strength development in the presence of DEIPA
and EDIPA, and a deep understanding of the mechanism behind is also
discussed. This further understanding would lead to more efficient use of
the two alkanolamines in grinding aids and even in accelerators.
2. Materials and methods
2.1. Materials
Reference cement P⋅I 42.5 according to the Chinese standard
GB8076-2008 was used and its chemical and mineral compositions
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Cement and Concrete Research 162 (2022) 106999
analyzed by XRF and QXRD are listed in Table 1. The density and Blaine
fineness of Portland cement were 3.14 g/cm3 and 3500 cm2/g, respec­
tively. Commercial grade DEIPA and EDIPA with a solid content of 85 %
were used in this study. The dosages of DEIPA and EDIPA are selected as
0.05 % and 0.5 % by weight of cement. The molecular formulas of DEIPA
and EDIPA are given in Fig. 1. Both cement mortars and pastes were
prepared with a water to cement (w/c) ratio of 0.5. Deionized water was
used to prepare all samples. The nomenclature adopted to identify each
composition follows the pattern ‘alkanolamine type’ + ‘dosage’. For
example, DEIPA005 means the sample with 0.05 % of DEIPA.
2.2. Cement paste experiments
Isothermal calorimetry, X-ray powder diffractometry (XRD), differ­
ential thermograms analysis (DTG), 1H nuclear magnetic resonance (1H
NMR) and scanning electron microscopy (SEM) were carried out on
cement pastes with w/c ratio of 0.5 to study effects of DEIPA and EDIPA
on hydration and microstructure development. Paste experiments were
measured complying with the Chinese standard JC/T729-2005. For
XRD, TG and SEM measurements, flaky pieces retrieved from the inte­
rior core were selected. Solvent exchange with isopropanol was used to
terminate the hydration as it is the least destructive solvent for the
microstructure [29]. To ensure effective stoppage of hydration, 5–8
pieces of the sample were immersed into 200 ml of isopropanol. The
isopropanol was replaced twice, after 1 d and after 3 d. Until 7 d of
solvent exchange, the samples were dried in a desiccator with silica gel
beads and under vacuum for 3 d to evaporate the isopropanol.
2.2.1. Isothermal calorimetry
The heat of hydration of Portland cement pastes with DEIPA or
EDIPA was measured by a Thermometric TAM Air isothermal calorim­
eter (TA Instruments) at 20 ± 0.02 ◦ C. 4 g of dry cement were loaded in
glass ampoules, and syringes were loaded with 2 g of alkanolamine-
water solution. After a steady baseline reached, the solution was injec­
ted into glass ampoules and external stirred for 20 s. Then the glass
ampoule was sealed and placed into the isothermal calorimeter. The
heat of hydration was measured for 3 d to study the effect of DEIPA and
EDIPA on the hydration of Portland cement pastes.
2.2.2. XRD/QXRD analysis
The phase composition of hydrated cement pastes was investigated
by a MiniFlex600 diffractometer with a CuKa source, a scanning range of
5–65◦ and a scanning speed of 2◦ per minute. QXRD analysis utilized the
Rietveld method in the HighScore software, which was applied to
quantify the consumption of clinkers and sulfate carriers and the for­
mation of hydration products. Before testing, samples were grinded and
passed through a 300-mesh sieve and dried in a vacuum oven at 40 ◦ C
for two days. To quantify the amorphous content of the pastes, rutile
(ALDRICH) was added at 50.00 % bcw as an internal standard. All
structure models used for Rietveld refinement are shown in Table 2.
2.2.3. DTG analysis
DTG analysis is an effective method of quantifying and identifying
hydration products such as C-S-H, AFm, AFt and CH. The preparation of
samples in powder form was consistent with the preparation of XRD
samples. A TGA instrument type of Netzsch STA 409PC was used in this
test. Samples were heated continuously in a nitrogen atmosphere from
20 to 1000 ◦ C with a temperature rate of 10 ◦ C/min.
2.2.4. 1H NMR
The effect of DEIPA and EDIPA on pore size distribution of cement
pastes was studied by 1H NMR, using low-field nuclear magnetic reso­
nance in a MAGMED-PM-1030 cementitious materials analyzer (MAG-
MED, China). Cylinder specimens of Φ25mm * 25 mm were prepared for
1
H NMR measurement. Porosity was also measured by 1H NMR with the
same size cylinder specimens. The transversal relaxation time (T2) of
Y. Wang et al. Cement and Concrete Research 162 (2022) 106999

Table 1
The chemical and mineral compositions of Portland cement (wt%).
Chemical composition CaO SiO2 Fe2O3 Al2O3 SO3 MgO Na2Oeq f-CaO LOI
wt/% 63.32 20.58 3.38 5.03 2.06 2.01 0.55 0.68 1.76
Mineral composition C3S C2S C3A C4AF Gypsum Bassanite Calcite Syngenite –
wt/% 56.3 18.0 7.5 11.6 2.9 0.9 2.6 0.3 –

DEIPA EDIPA
Fig. 1. Molecular formulas of DEIPA and EDIPA.

Table 2
Structure models used for Rietveld refinement.
Phase Formula Crystal system ICSD cods Reference

Alite Ca3SiO5 Monoclinic 94,742 [30]

Belite Ca2SiO4 Monoclinic 81,096 [31]
Tricalcium aluminate Ca3Al2O6 Cubic 1841 [32]
Ferrite Ca2AlFeO5 Orthorhombic 98,830 [33]
Gypsum CaSO4⋅2H2O Monoclinic 151,692 [34]
Bassanite CaSO4⋅0.5H2O Monoclinic 79,529 [35]
Portlandite Ca(OH)2 Trigonal 202,220 [36]
Ettringite 3CaO⋅Al2O3⋅3CaSO4⋅32H2O Trigonal 155,395 [37]
Monosulfoaluminate 3CaO⋅Al2O3⋅CaSO4⋅12H2O Trigonal 24,461 [38]
Rutile (standard) TiO2 Tetragonal 93,097 [39]

pore solution was measured to reflect the pore diameter at 20 ◦ C and Chinese standard GB17671-1999 to study the effects of DEIPA and
with a resonance frequency of 9.89 MHz. To reflect the real pore size EDIPA on strength development. Cement mortars (40 × 40 × 160 mm)
distribution and porosity, specimens were vacuum saturated with water were prepared with w/c of 0.5 and an aggregate-to-cement ratio of 3,
to fill pores with water before measurement. The transversal relaxation and placed in standard curing chamber with relative humidity of 98 %
time T2 was obtained by Carr-Purcell-Meiboom-Gill (CPMG) pulse and temperature of 20 ± 2 ◦ C. Compressive strength was measured at
sequence and was transformed into pore size distributions according to hydration ages of 1, 3, 7 and 28 d with average results from at least three
the Eq. (1) [40,41]. samples.
( )
1 1 S ρ
≈ = ρ2 = FS × 2 (1) 3. Results and discussions
T2 T2,surf V Pore r
3.1. Heat evolution
where T2 is the relaxation time of water; T2,surf denotes the transversal
relaxation time due to surface relaxation; (S/V)pore is the specific surface
Cement hydration with DEIPA or EDIPA incorporation was measured
area of pore; Fs = 2.0 for cylinder pore; ρ2 and r refer to the surface
by isothermal calorimetry as shown in Fig. 2. For Portland cement, the
relaxivity and radius of the pore, respectively, ρ2 is 50 μm/s for cement
calorimetric curves are characterized by two hydration peaks and one
pastes and mortars [42].
exothermic shoulder after the second peak. The initial peak emerging
right after water-cement contact is assigned to the physical wetting and
2.2.5. SEM
the initial chemical reactions including the initial dissolution of various
Morphology analysis was conducted by Phenom LE Desktop SEM
mineral phases, setting regulator, and the initial precipitation of AFt
(Phenom World, Netherlands) with a high vacuum of 0.1 Pa. A voltage
[43]. The second peak, which is the main hydration peak, is mainly
of 5 kV was used to observe the samples with the scanning electron
attributed to the rapid dissolution of alite and the precipitation of CH
microscope in a Secondary Electron Detector (SE). Before doing the
and C-S-H [44], followed by the continued precipitation of ettringite. A
experiment, all the samples were dried in a vacuum oven at 40 ◦ C for two
small amount of ferrite and belite also dissolves during this period [24].
days and coated with a thin gold layer to improve electrical
The exothermic shoulder after the main peak is due to the second hy­
conductivity.
dration of aluminate phases after the complete consumption of setting
regulator, which is also called sulfate-depletion peak [45].
2.3. Compressive strength
As seen from Fig. 2(a), both DEIPA and EDIPA enhanced and
advanced the main hydration peak and sulfate-depletion peak under the
Compressive strength of cement mortars was tested based on the

3
Y. Wang et al.
Fig. 2. Hydration heat flow (a) and cumulative heat release (b) of cement pastes with different dosages of DEIPA or EDIPA.
dosage of 0.05 %, especially DEIPA, indicating that DEIPA and EDIPA
might promote alite hydration and the second hydration of aluminate
phases. However, when the dosage of DEIPA or EDIPA increased to 0.5
%, main hydration peaks were extremely weakened and delayed to
about 40 and 65 h, respectively. It is surprisingly observed that sulfate-
depletion peaks appeared earlier than main hydration peaks and were
fairly high under this dosage, indicating that high dosage (0.5 %) of
DEIPA or EDIPA, especially EDIPA, strongly retarded alite hydration but
accelerated the second hydration of aluminate phase. It seems that the
accelerated aluminate reactions had negative effect on the main hy­
dration peak. Lu et al. [11] also observed earlier appearance of sulfate-
depletion peak than main hydration peak in Portland cement with 0.5 %
of TEA. Fig. 2(b) presents the cumulative heat release of Portland
cement with different dosages of DEIPA or EDIPA. Cement pastes with
0.05 % of DEIPA or EDIPA, especially DEIPA, presented much higher
cumulative heat release than reference cement paste at 72 h. 0.5 % of
DEIPA or EDIPA dramatically decreased cumulative heat release of
cement pastes within several hours compared to reference cement paste.
However, cumulative heat release of samples with 0.5 % of DEIPA or
EDIPA was comparable to that of reference cement paste at 72 h, and the
cumulative heat release of DEIPA sample even exceeded that of refer­
ence cement paste at 72 h. Generally, cement pastes with DEIPA pre­
sented earlier and higher main hydration peak and much higher
cumulative heat release than that with EDIPA under the two dosages.
Fig. 3. XRD patterns of cement pastes with DEIPA or EDIPA at 3 and 28 d.
4
Cement and Concrete Research 162 (2022) 106999
3.2. Phase evolution analyses by XRD/QXRD and TG
3.2.1. XRD/QXRD analysis
XRD patterns of cement pastes with DEIPA or EDIPA incorporation at
3 and 28 d are shown in Fig. 3. The characteristic peaks of AFt, AFm, CH,
C3S, C2S and C4AF are clearly recognized. Generally, the intensity of C3S,
C2S, C4AF, AFt and CH decreased with the incorporation of DEIPA or
EDIPA, while the intensity of AFm enhanced with the incorporation of
DEIPA or EDIPA.
QXRD results of cement pastes with DEIPA or EDIPA incorporation at
3 and 28 d are shown in Fig. 4. For the aluminate reactions, both DEIPA
and EDIPA accelerated initial dissolution and hydration of C3A and
C4AF, resulting in lower mass ratios of C3A and C4AF. Correspondingly,
gypsum depletion and the conversion of AFt to AFm were advanced. The
mass ratios of AFm at 3 d were about 0.2 %, 2.0 %, 3.4 %, 5.4 % and 7.5
% in samples REF, DEIPA005, EDIPA005, DEIPA05 and EDIPA05,
respectively, revealing that the content of AFm increased with the in­
crease of DEIPA or EDIPA dosage and EDIPA was more capable of pro­
moting the formation of AFm. At 28 d, AFm contents were still higher in
cement pastes with EDIPA than that with DEIPA under both dosages.
For the silicate reactions, cement pastes with DEIPA or EDIPA also
presented lower mass ratios of C3S and C2S, indicating higher hydration
degree of calcium silicates compared to REF sample, which can be
related to their complexation effect on cement minerals [27]. The mass
Y. Wang et al.
Fig. 4. Quantitative XRD results of cement pastes with DEIPA or EDIPA at 3 and 28 d.
ratios of C3S + C2S at 3 d were about 26.8 %, 17.6 %, 21.2 %, 24.2 % and
25.8 % in samples REF, DEIPA005, EDIPA005, DEIPA05 and EDIPA05,
respectively. It can be concluded that calcium silicates hydration pro­
ceeded to larger extent with low dosage (0.05 %) of DEIPA or EDIPA and
DEIPA was more capable of promoting calcium silicates hydration at 3 d.
It can be concluded that calcium silicates hydration is closely related to
the aluminates hydration at early ages, and larger content of AFm leads
to lower hydration degree of calcium silicates. Wang et al. [46]
explained that thermodynamically stable AFm could wrap on the surface
of cement particles, leading less space for C3S dissolution and hydration.
Generally, competition between silicates and aluminates hydration ex­
ists in Portland cement system [47]. It is worth noting that reference
sample produced less AFm but showed lower hydration degree of cal­
cium silicates compared to that with DEIPA or EDIPA, which can be
explained by the acceleration effect of DEIPA or EDIPA on calcium sil­
icates hydration. However, cement paste with EDIPA presented higher
hydration degree of C3S compared to that with DEIPA at 28 d.
It is clearly seen that the incorporation of DEIPA or EDIPA had
negative effect on crystalline CH formation, especially under high
dosage (0.5 %). Wang et al. [48] investigated Ca(OH)2 precipitation by
CaCl2 and NaOH reaction in TEA solution and found that TEA strongly
hinders the nucleation and growth of Ca(OH)2 due to the complexation
effect with Ca2+ ions in solution. Considering that DEIPA or EDIPA can
complex with Ca2+ [49], saturation of Ca2+ in pore solution and
Fig. 5. DTG curves of cement pastes with DEIPA or EDIPA at 3 and 28 d.
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Cement and Concrete Research 162 (2022) 106999
crystallization of CH were delayed. DEIPA presented higher inhibition
effect on the formation of crystalline CH.
3.2.2. DTG analysis
Thermogravimetry test was conducted to further identify hydration
products in cement pastes with DEIPA or EDIPA incorporation, as shown
in Fig. 5. Three major endothermic peaks can be detected in DTG curve
of Portland cement paste, which are the peaks of C-S-H, AFt and AFm
from room temperature to 300 ◦ C, the peak of CH decomposition from
350 to 550 ◦ C, and the peak of CaCO3 decomposition from 600 to 800 ◦ C
[50–52].
At 3 d, DTG curve of REF sample presented a sharp endothermal peak
traced from 55 to 155 ◦ C. Combined with XRD results, the peak can be
attributed to weight loss of C-S-H and AFt. Compared with REF sample,
endothermal peaks in this temperature range were much smaller in
cement pastes with DEIPA or EDIPA incorporation and a new endo­
thermal peak emerged at around 170 ◦ C, which indicates that these two
alkanolamines promoted the conversion of AFt to AFm. Similar to XRD
results, endothermal peaks of CH were weakened by DEIPA or EDIPA
incorporation compared to REF sample, which means that these two
alkanolamines also decreased CH content obtained by TG analysis
(including crystalline and non-crystalline CH). At 28 d, CH contents of
cement pastes with DEIPA or EDIPA were still lower than reference
sample through DTG analysis. Cement pastes with EDIPA presented
Y. Wang et al.
lower decrease of CH content compared to DEIPA samples under both
ages.
3.3. Characterization of microstructure
3.3.1. 1H NMR
For samples with low strength or at early ages, 1H NMR analysis can
more accurately reflect pore structure compared to mercury intrusion
porosimetry (MIP) method because the very high pressure of the mer­
cury and pre-vacuum drying process before MIP would damage pore
structure of samples [53]. Besides, pore of cement fails to fulfill the
cylindrical pores required by Washburn equation in MIP and 1H NMR
can detect fairly small pores by measuring the internal water of samples
[54].
The 1H NMR results of cement pastes with DEIPA or EDIPA incor­
poration are shown in Fig. 6. The correlated diameter of pore calculated
by Eq. (1) is presented below the axis of relaxation time. It can be seen
that three main peaks related to the relaxation time or pore solution
distribution were detected. At 3 d, apart from sample EDIPA05, the pore
solution distribution of cement pastes with DEIPA or EDIPA shifted to
smaller diameter pores, which could be attributed to their complexation
effect to promote cement hydration. Meanwhile, larger pores also exis­
ted in cement pastes with DEIPA or EDIPA due to their air entraining
effect. High dosage (0.5 %) of DEIPA or EDIPA would result in much
larger diameter pores and higher peak values, especially high dosage of
EDIPA. The pore solution distribution of all samples shifted to smaller
diameter pores as hydration continued to 28 d. Larger pores still existed
in cement pastes with DEIPA or EDIPA at 28 d. Although cement pastes
with EDIPA presented larger diameter pores than that with DEIPA at 3 d,
pore solution distribution of cement pastes with 0.05 % of EDIPA was
smaller than that with 0.05 % of DEIPA at 28 d, which could be
attributed to the faster hydration and microstructure development of
cement pastes with EDIPA at later ages. The total porosities for cement
pastes with DEIPA or EDIPA at 3 and 28 d are also obtained by 1H NMR,
as shown in Table 3. Compared with samples with low dosage (0.05 %)
of DEIPA or EDIPA, samples with 0.5 % of DEIPA or EDIPA presented
much higher total porosity.
3.3.2. Morphology analysis
SEM images are applied to visualize the microstructure of hydrated
products at 3 and 28 d, as shown in Figs. 7 and 8. It can be seen that
needle-like AFt existed in reference cement pastes at 3 d, accompanied
with large amounts of stacked CH and C-S-H gel. However, needle-like
phases almost disappeared in cement pastes with DEIPA or EDIPA
incorporation and were replaced by a number of hexagonal plates which
Fig. 6. T2 relaxation time distribution of cement pastes with DEIPA or EDIPA at 3 and 28 d.
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Cement and Concrete Research 162 (2022) 106999
Table 3
The total porosity for cement pastes with DEIPA or EDIPA at 3 and 28 d.
Alkanolamines Dosage/% Total porosity/%
3d 28 d
Reference 0 0.4114 0.3133
DEIPA 0.05 0.3772 0.2795
0.5 0.4044 0.2768
EDIPA 0.05 0.4188 0.2838
0.5 0.4442 0.2961
were considered as AFm and presented a steel-frame structure. Addi­
tionally, scale and morphology of CH were greatly affected by DEIPA or
EDIPA incorporation. CH presented regular hexagonal plate shape with
good crystallization in reference cement paste while more irregular flake
shape of CH was seen in cement pastes with DEIPA or EDIPA, especially
under high dosage (0.5 %). CH in cement pastes with DEIPA presents
more irregular and amorphous morphology compared to that with
EDIPA. In fact, the crystallization and growth of calcium hydroxide in
cement paste include the crystal along the direction perpendicular to the
hexagonal cylinder ([00.1] direction) and the direction perpendicular to
the bottom axis ([10.0] direction) [55], corresponding to the formation
of hexagonal plate and irregular flake shape of CH, respectively. In
cement pastes with DEIPA or EDIPA, Ca2+ consumption attributed to
accelerated hydration of C3A and C4AF and the complexation of Ca2+
with these two alkanolamines resulted in low supersaturation of calcium
hydroxide, which made it difficult for CH to form regular hexagonal
plate shape with good crystallization.
It can be seen that more C-S-H and larger sized CH formed and
cemented into much denser microstructure at 28 d. Cement pastes with
0.5 % of DEIPA or EDIPA presented a relatively loose microstructure
compared to that with 0.05 % of DEIPA or EDIPA. Although there were
large amounts of well-crystallized hexagonal CH formed in cement
pastes with DEIPA or EDIPA at 28 d, irregular flake shaped CH still
existed in both cement pastes. In addition, although cement pastes with
EDIPA presented larger diameter pores than that that with DEIPA at 28
d, it presented a denser microstructure as more hydration products filled
in the pores.
3.4. Compressive strength
Fig. 9 shows compressive strength of cement mortars with DEIPA or
EDIPA incorporation. As can be seen, cement mortars with 0.05 % of
DEIPA or EDIPA present higher or comparable compressive strength
compared to the reference sample, which can be attributed to their
complexation effect on the accelerated aluminates and silicates
Y. Wang et al.
Fig. 7. SEM images of cement pastes with DEIPA or EDIPA incorporation at 3 d.
hydration to form much denser microstructure. However, ignore the
influence of error, compressive strength increased by 15.57 % for
cement mortar with 0.05 % of DEIPA but increased only by 2.65 % for
cement mortar with 0.05 % of EDIPA at 3 d. Conversely, compressive
strength increased by 13.85 % for cement mortar with 0.05 % of EDIPA
but increased only by 2.43 % for cement mortar with 0.05 % of DEIPA at
28 d. It can be concluded that 0.05 % of DEIPA was more capable of
increasing compressive strengths at early hydration ages of 1 and 3 d,
while compressive strengths at later hydration ages of 7 and 28 d were
more enhanced with 0.05 % of EDIPA incorporation. Compared with
cement paste with 0.05 % of DEIPA, more AFm formed in cement paste
with 0.05 % of EDIPA, leading to lower hydration degree of C3S and C2S
at early ages. On the other hand, EDIPA possesses higher air entraining
property compared to DEIPA to cause more serious pore structure
7
Cement and Concrete Research 162 (2022) 106999
degradation. The combination effect of lower hydration degree and
more degraded pore structure led to much lower early strength of
cement paste with 0.05 % of EDIPA. Besides, the formation of larger
content of crystalline CH in samples with EDIPA should be another
reason for the lower strength development, as CH is often considered as
the weakest part of hardened cement paste [56]. At later ages, hydration
of C3S and C2S proceeded to larger extent in cement paste with 0.05 % of
EDIPA, which refined microstructure and resulted in higher later
strength compared to that with DEIPA.
0.5 % of DEIPA or EDIPA decreased both the early and later
compressive strength of cement mortars, especially the early strength.
Compressive strength at 3 d decreased by 21.13 % for cement mortar
with 0.5 % of DEIPA while decreased by 45.0 % for that with 0.5 % of
EDIPA. High dosage of DEIPA or EDIPA would cause more serious air
Y. Wang et al.
Fig. 8. SEM images of cement pastes with DEIPA or EDIPA incorporation at 28 d.
entraining effect, as concluded by microstructure analyses, which is the
main reason for the strength decrease. Besides, much larger amounts of
AFm formed with the incorporation of 0.5 % of DEIPA or EDIPA, leading
to retarded main hydration peak and lower hydration degree of silicates
compared to that with 0.05 % DEIPA or EDIPA. Higher air entraining
property of EDIPA, more AFm formation and lower hydration degree of
cement paste with EDIPA resulted in higher strength loss of cement paste
with 0.5 % of EDIPA compared to that with 0.5 % of DEIPA. However,
compressive strength loss of cement mortars with 0.5 % of DEIPA or
EDIPA narrowed at later hydration ages, especially for mortars with
EDIPA. Compressive strength at 28 d decreased by 6.0 % for cement
mortar with 0.5 % of DEIPA while decreased only by 0.1 % for cement
mortar with 0.5 % of EDIPA. It can be concluded that cement paste with
0.5 % of EDIPA presented higher hydration degree of C3S and C2S to
8
Cement and Concrete Research 162 (2022) 106999
refine microstructure and compensate strength loss at later ages, which
is the main reason for the less later strength loss of cement paste with
0.5 % of EDIPA.
Although the mechanism of DEIPA and EDIPA on strength develop­
ment of cement mortars can be well revealed from aspects of cement
hydration and microstructure development. A problem still remains that
why EDIPA is more beneficial to later hydration and strength develop­
ment of Portland cement. Perez et al. [57] and Gartner and Myers [58]
proposed that more bulky hydroxypropyl groups on TIPA, relative to the
less bulky hydroxyethyl groups on TEA, led to higher steric hindrance
TIPA. Higher steric hindrance led to less adsorption of TIPA on CH,
resulting in more TIPA in pore solution to enhance C3S hydration at later
ages [57]. Considering that EDIPA has two hydroxypropyl groups and
one hydroxyethyl group while DEIPA has two hydroxyethyl groups and
Y. Wang et al.
Fig. 9. Effect of DEIPA or EDIPA on compressive strength of cement mortars at
different ages.
one hydroxypropyl group, EDIPA possesses higher steric hindrance than
DEIPA, which minimized its adsorption on CH at later ages to furtherly
promote cement hydration at later ages.
4. Conclusions
In this study, the following conclusions can be obtained:
• Both dosages (0.05 %, 0.5 %) of DEIPA or EDIPA accelerated the
hydration of C3A and C4AF to advanced gypsum depletion and AFm
formation and the hydration of C3S and C2S due to their complexa­
tion effect.
• The main hydration peak significantly weakened with 0.5 % of
DEIPA or EDIPA incorporation due to large formation of AFm.
Conversely, it was advanced and enhanced by 0.05 % of DEIPA or
EDIPA, which could be attributed to their complexation effect to
accelerate minerals dissolution and the not so pronounced formation
of AFm, leading to higher hydration degree of C3S and C2S compared
to that with 0.5 % of DEIPA or EDIPA.
• Compared with DEIPA, EDIPA was more capable of promoting AFm
formation and led to lower hydration degree of C3S and C2S at early
ages and possessed higher air entraining property to cause pore
structure degradation. However, EDIPA contributed to higher hy­
dration degree of C3S and C2S to refine microstructure development
at later ages.
• 0.05 % of DEIPA was more capable of increasing the early
compressive strength of cement mortars at 1 and 3 d, while the later
compressive strength at 7 and 28 d was more enhanced with 0.05 %
of EDIPA incorporation. 0.5 % of DEIPA or EDIPA considerably
damaged early strength development of cement mortars, especially
0.5 % of EDIPA.
• It can be concluded that compressive strength of cement mortars
with DEIPA or EDIPA was determined by their acceleration effect on
AFm formation, complexation effect to accelerate minerals dissolu­
tion and cement hydration and air entraining effect to cause micro­
structure degradation. The dosage of DEIPA or EDIPA plays an
important role on strength development.
CRediT authorship contribution statement
The manuscript was written through contributions of all authors. All
authors have given approval to the final version of the manuscript.
9
Cement and Concrete Research 162 (2022) 106999
Guarantors of integrity of entire study
Yifei Wang, Lei Lei, Xiang Hu, Yi Liu, Caijun Shi
Study concepts
Yifei Wang, Caijun Shi
Study design
Yifei Wang, Caijun Shi
Literature research
Yifei Wang, Lei Lei, Xiang Hu, Yi Liu, Caijun Shi
Experimental studies
Yifei Wang, Caijun Shi
Data acquisition
Yifei Wang
Data analysis/interpretation
Yifei Wang, Lei Lei, Caijun Shi
Manuscript preparation
Yifei Wang, Lei Lei, Caijun Shi
Manuscript definition of intellectual content
Yifei Wang, Lei Lei, Caijun Shi
Manuscript editing
Yifei Wang, Lei Lei, Caijun Shi
Manuscript revision/review
Yifei Wang, Lei Lei, Xiang Hu, Yi Liu, Caijun Shi
Funding acquisition
The Chinese Ministry of Science and Technology (Project No.
2018YFC0705400), National Natural Science Foundation of China
(Project No. U1806225 and 51638008), and financial support from the
program of China Scholarships Council (CSC No. 202106130057)
Final version of manuscript approval
Yifei Wang, Lei Lei, Xiang Hu, Yi Liu, Caijun Shi
Declaration of competing interest
The authors declare that they have no conflicts of interest to this
work. We declare that we do not have any commercial or associative
interest that represents a conflict of interest in connection with the work
submitted.
Data availability
Data will be made available on request.
Acknowledgement
The research was supported by the Chinese Ministry of Science and
Technology (Project No. 2018YFC0705400), National Natural Science
Foundation of China (Project No. U1806225 and 51638008), and
financial support from the program of China Scholarships Council (CSC
No. 202106130057).
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