Construction and Building Materials 125 (2016) 974980

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Construction and Building Materials

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

Microstructural insights into the lime mortars mixed with sticky rice
solgel or water: A comparative study
Rongwei Yang, Zhiling Zhang, Meijie Xie, Kefei Li
Civil Engineering Department, Tsinghua University, 100084 Beijing, PR China

h i g h l i g h t s

Sticky rice slurry refines pore structure and increases strength of lime mortar.

Fractal dimension of pore structure is decreased by adding rice slurry.

Sticky rice slurry forms more compact inter-granular microstructure.

a r t i c l e i n f o a b s t r a c t

Article history: This paper is dedicated to studying the effect of sticky rice solgel on the microstructure (including pore
Received 19 October 2015 structure and texture) and properties of lime mortar. Uniaxial compressive strength tests, scanning elec-
Received in revised form 1 August 2016 tron microscopy (SEM), and mercury intrusion porosimetry (MIP) were utilized to investigate the macro-
Accepted 28 August 2016
scopic behaviors and microstructure, respectively. Based on the MIP data, a surface fractal dimension
Available online 4 September 2016
analysis is performed to study the impact of sticky rice solgel on pore structure. The addition of sticky
rice solgel is demonstrated to improve the uniaxial compressive strength of lime mortar. The SEM, MIP
Keywords:
and surface fractal dimension analysis results show that the addition of sticky rice solgel facilitates the
Lime mortar
Sticky rice solgel
formation of compact texture, fine pore structure and elevates the bonding strength of the lime mortar. A
Microstructure microstructrual mechanism is proposed to explain how properties of the lime mortar are affected by the
Surface fractal analysis addition of sticky rice solgel.
Microscopic mechanism 2016 Elsevier Ltd. All rights reserved.

1. Introduction
Acting as Roman mortar in ancient Europe, tabia (referred to
as lime mortar), composed of clay, lime and/or other assemblies
in designated proportions, is extensively used as an essential build-
ing material in ancient China. The lime mortar is often mixed with
the organic admixture, e.g. sticky rice solgel, tung oil, juice of
vegetable leaves, egg white and animal blood to form the inor-
ganicorganic composites [1,2]. These composites, used as the
main building materials in Chinese ancient relics, were found to
greatly improve the performance and durability of the ancient Chi-
nese buildings [1]. Among these inorganicorganic composites, the
sticky rice sol gellime mortar (SLM) has been most widely used in
the historical monuments, e.g. the Great Wall and the Forbidden
city in Beijing.
As shown in Fig. 1, owing to the weathering and/or other dete-
rioration actions such as drying-wetting and freezing-thawing
Corresponding author.
E-mail address: likefei@tsinghua.edu.cn (K. Li).
cycles [3,4], most of the ancient relics are subjected to surface spal-
ling and scaling [2]. The fresh organic admixturelime mortars
have been often used in situ replacement to preserve ancient
earthen ruins [1,5]. Inappropriate use of the organic admixture
lime mortars can result in the failure of the restoration work, and
even probably further damage to the original historical construc-
tion [1]. Therefore, it is indispensable to understand the
microstructure and macroscopic properties of these replacing
(fresh) organic admixturelime mortars.
In order to understand the relationship between the microstru-
ture and macroscopic properties of organic admixturelime mor-
tars, extensive studies were undertaken experimentally [1,2,58].
However, little work has been carried out to investigate the pore
structure of organic admixturelime mortars so far. Such pore
structure is believed to relate intimately to the macroscopic trans-
port and mechanical properties of the organic admixturelime
mortars.
The most used parameters in characterizing the pore structure
are porosity, pore size distribution and specific surface [9]. How-
ever, these parameters are global features of the pore structure,

http://dx.doi.org/10.1016/j.conbuildmat.2016.08.119
0950-0618/ 2016 Elsevier Ltd. All rights reserved.
 R. Yang et al. / Construction and Building Materials 125 (2016) 974980
Fig. 1. Surface spalling arising from the weathering on the lateral side of the Great
Wall.
and no information upon the texture is provided [9]. To overcome
this shortcoming, an additional parameter, fractal dimension, is
introduced to characterize the packing patter of the solid grains
[912]. Experimental devices such as nitrogen adsorption/desorp-
tion (NAD) [1012], small-angle X-ray/neutrons scattering (SAXS/
SANS) [13,14], nuclear magnetic resonance (NMR) [15], scanning
electronic microscopy (SEM) [15,16], and mercury intrusion
porosimetry (MIP) [17,18] are used extensively to evaluate the
fractal properties of internal surface of porous media [9]. Among
these available methods, MIP was the most used characterization
method owing to its ability to cover a large pore size range, from
nanometer to millimeter [9,17,18].
The objective of this study is to investigate the influence of the
sticky rice solgel on the macroscopic properties and microstruc-
ture, particularly the pore structure of the lime mortars by means
of uniaxial compressive strength test, SEM, MIP test and surface
fractal dimension analysis. A microstructural mechanism is pro-
posed to address how the sticky rice solgel affects the bonding
strength of the organic admixturelime mortar.
2. Materials and methods
In order to study the impact of the sticky rice solgel on the
microstructure and macroscopic properties of lime mortar, two
groups of lime mortars, one mixed with water (denoted as WLM)
and another with sticky rice solgel (denoted as SLM), were
prepared.
2.1. Materials and preparation
The clayey soil came from Bajia, Haidian district, Beijing, having
a liquid limit of 24.2% and a plastic limit of 13.7%. The sticky rice is
a species grown widely in Southeast and East Asia, with amy-
lopectin as its main component [1]. The accumulative particle size
distribution of the clayey soil is depicted in Fig. 2.
The sticky rice solgel was made by heating a mixture of sticky
rice powder (1 kg), distilled water (10 kg) and potassium alum
(0.055 kg) at 100 C for 4 h. The addition of the potassium alum
was to prevent the sticky rice solgel from decaying during preser-
975
Fig. 2. Accumulative particle size distribution of the clayey soil.
vation, because generally the sticky rice solgel would be pre-
served for several months before adding into the lime mortar. In
order to ensure the final concentration of the sticky rice solgel
to be 10 wt.%, the distilled water was subsequently added into
the mixture.
The clayey soil and hydrated lime were mixed following a mass
ratio of clayey soil: hydrated lime = 7:3, which was consistent with
the ratio reported in the ancient building work Tian Gong Kai Wu
[19]. According to ASTM-D1557, we estimated the optimum water
content of WLM and SLM by determining their maximum density.
Thus, as shown in Table 2, the optimum water contents of WLM
and SLM were wt.22.4% and wt.21.5%, respectively. More precisely,
the mix proportion for WLM (i.e., water: (soil + lime)) was wt.22.4%
and that for SLM (i.e., sticky rice solgel: (soil + lime)) was
wt.21.5%. Following ASTM-D3551 [20], the soil and lime mixture
were placed in the mixer and dry-mixed the mixture for 1 min.
Afterwards, distilled water or sticky rice solgel was added in the
mixture and stirred for an additional 5 min until a stable consis-
tency was achieved. Immediately after mixing, lime mortar mixed
with water (WLM) and lime mortar mixed with sticky rice solgel
(SLM) were respectively poured in the cubic steel molds of
40 mm  40 mm  40 mm. The specimens were compacted by
hammer following ASTM-D1557 [21] to achieve the optimum
water content (OWC). After compaction, the specimens were cov-
ered with a thin plastic film and cured in the curing room at
20 C, 62% relative humidity (RH). After curing for 3 days, the spec-
imens were demolded and remained in the same curing room until
testing. A total of 12 specimens for each material were prepared for
the following experimental study.
The chemical compositions of the clayey soil, hydrated lime,
WLM and SLM measured through the X-ray fluorescence spec-
trometer (XRF) are given in Table 1.
2.2. Experimental methods
Several experimental methods were employed to investigate
the microstructure and properties/strength of WLM and SLM. The
cubic specimens were used to measure the uniaxial compressive
strength. Cut from the cubic specimens, several samples with a
characteristic size of 5 mm were prepared for the scanning elec-
tron microscopy (SEM) and mercury intrusion porosimetry (MIP)
experiments, respectively. A prepared sample was ground and fil-
tered with 0.075 mm sieve, and the obtained powder with charac-
teristic size less than 0.075 was prepared for the X-ray diffraction
(XRD) experiment.
The X-ray diffraction (XRD) patterns were recorded on a Rigaku
D/Max 2500H diffractometer with Cu-Ka radiation source. The 2h
976 R. Yang et al. / Construction and Building Materials 125 (2016) 974980
Table 1
Chemical compositions in wt.% oxides, measured from XRF analysis.
Sample SiO2 CaO Al2 O3
Clayey soil 60.66 9.45 13.79
Hydrated lime 7.0 78.0
WLM 43.41 28.08 11.65
SLM 47.74 21.70 12.70
range is 1090 at a step size of 0.02. The results were compared
with the database within Jade-5.0 software to identify the compo-
sitions of the sample. The morphology of the samples were inves-
tigated with a scanning electron microscope (SEM, FEI quanta
200F) with accelerating voltage of 15 kV.
The uniaxial compressive strength of cubic specimens cured for
7 days and 28 days and that of the cubic specimens after 6 freeze
thaw cycles were measured by hydraulically controlled materials
testing machine following ASTM-D5102 [22], and the loading rate
was 5 mm/min. Three specimens were measured for each case, and
the average value was taken as the compressive strength.
MIP test was performed using a device Micromeritics AutoPore
IV 9500. Intrusion pressures ranging from 1.4 kPa to 414 MPa, cor-
responding to filling pore diameter from 800 lm down to 3 nm,
were employed. Prior to the MIP test, the samples were dried by
freeze-drying method. Compared to other drying methods such
as oven-drying, freeze-drying provides favorable condition, e.g.
smaller surface tension at pore scale, to preserve the microstruc-
ture during drying [18]. The freeze-drying was proved to be effec-
tive for soil sample [18,23].
3. Results and discussion
3.1. XRD analysis
The XRD analysis was performed to identify the mineral and
crystalline products within clayey soil, WLM and SLM. As depicted
in Fig. 3, within WLM and SLM, there all exist the quartz and pyrox-
ene (main mineral composition), unreacted portlandite CaOH2 ,
dolomite (CaMgCO3 2 ), and the carbonation product calcite [1].
The formation of dolomite within WLM and SLM is probably aris-
ing from the large quantity of MgO in hydrated lime (see Table 1).
Though there has been certain amount of calcite (i.e. 9.45% CaO) in
the clayey soil, according to Fig. 3, we can find that the intensity
peaks of calcite for SLM and WLM increase, which indicates the for-
Fig. 3. XRD patterns of clayey soil, WLM and SLM.
Fe2 O3 K2 O MgO TiO2 Na2 O MnO
7.90 3.24 2.84 1.04 0.70 0.12
12.7
7.64 2.46 5.11 0.88 0.33 0.13
7.75 2.83 5.57 0.92 0.34 0.13
mation of calcite within SLM and WLM during the carbonation
process.
As shown in Fig. 3, compared with WLM, the addition of sticky
rice solgel in SLM does not facilitate the formation of calcite,
which is different from observations so far in Refs. [2,6]. The differ-
ence may stem from the different composition and experimental
condition of the testing materials in our experiment from those
in literature. Firstly, calcium hydroxide solution was used with
sticky rice solgel in the experiments of Refs. [2,6], while hydrated
lime powder was used in our experiment, moreover, in addition to
hydrated lime powder, a large amount of clayey soil was mixed in
our experiment; the experiments in the literature surely provided
a more favorable condition for carbonation reaction than our
experiment. Secondly, samples in Refs. [2,6] were either cured in
carbon dioxide chamber [2] or cured in curing room at 20 C, 70%
relative humidity (RH) for much longer time (i.e., 180 days in Zeng
et al. [6]), portlandite in these studies was expected to react more
completely than that in our samples.
3.2. Physical and mechanical properties
As shown in Table 2, the addition of the sticky rice solgel
improves the physical properties and the strength of SLM. Com-
pared to WLM, the density of SLM increases about 10%. This may
be attributed to the lower optimum water content (OWC) of
SLM. Moreover, the 7-day (7d) strength (resp. 28-day (28d)
strength) of the SLM is slightly greater than that of WLM. Further-
more, the uniaxial compressive strength of the SLM after 6 freeze
thaw cycles (AFC) is about 47% higher than that of WLM. The
higher strengths of 7d, 28d and AFC of SLM are attributed to the
addition of the sticky rice solgel, which is in line with the exper-
imental results of Peng et al. [24] and Zhao et al. [2]. Comparing the
increase of 7d, 28d compressive strength of SLM with that of com-
pressive strength of the SLM after 6 freezethaw cycles, we can
infer that the addition of the sticky rice solgel enhances the dura-
bility of the lime mortar. The mechanism of the addition of sticky
rice solgel will be discussed in Section 3.5.
3.3. Textural morphology and pore size distribution
As shown in Fig. 4, the irregular, angular crystals (calcite and/or
portlandite and/or dolomite) are precipitated on the surface of the
soil grains in WLM and SLM. Generally, the sticky rice solgel, serv-
ing as a templet (nucleation sites), should facilitate the formation
of submicron calcite crystal [6], which would lead to the more
homogeneous and compact microstructure of SLM. However, as
explained in Section 3.1, the sticky rice solgel does not facilitate
the formation of sub-micron calcite crystals, and SEM images in
Fig. 4 show not much difference between the texture of WLM
(Fig. 4a and b) and texture of SLM (Fig. 4c and d).
Fig. 5 presents the pore size distributions of WLM and SLM
derived from MIP measurement. As can be found from the figure,
the addition of sticky rice solgel gives rise to the reduced critical
pore throat (120 nm) and lower porosity of SLM. Thus SLM has a
finer pore size than WLM. The difference in the pore size distribu-
tion is consistent with the experimental results from Refs. [1,24], in
which the water permeability of SLM is lower than that of WLM. It
 R. Yang et al. / Construction and Building Materials 125 (2016) 974980 977

Table 2
Measured physical properties and mechanical strength.

Sample OWCa Dry density Compressive strength MPa

% Kg:m 3 7d 28 d AFCb

WLM 22.4 1560 2.02 5.01 2.57

SLM 21.5 1660 2.74 5.92 3.78
a
OWC represents optimum water content.
b
AFC represents uniaxial compressive strength of 28-day cured sample after 6 freezethaw cycles.

(a) WLM, magnified by 10,000 (b) WLM, magnified by 2,000

(c) SLM, magnified by 10,000 (d) SLM, magnified by 2,000

Fig. 4. SEM images of WLM and SLM

can also be found that the volume of pores larger than 100 lm
accounts for ca. 10% of the porosity, these pores are either the air
voids introduced during the sample preparation or the large pores
formed by the sand grains. It should be noted that the pore size
ranging from 0.2 nm to 2 nm, corresponding to the intraparticle
pores (interlayer) within clay aggregates, could not be detected
by MIP as the minimum diameter detected by MIP is 3 nm [25].
3.4. Surface fractal dimension analysis
The surface fractal dimension quantifies the degree of the irreg-
ularity of the surface. The rougher is the surface, the greater is its
surface fractal dimension [26]. The surface fractal dimensions of
WLM and SLM are determined by Zhangs model based on the
MIP data [30,31]. The model is derived from dimension analysis
and the thermodynamic consideration, i.e. the balance between
the surface energy of mercury in pores and the external work
needed for mercury intrusion [30]. Zhangs model established a
relationship between the intruded work W n and intruded mercury
volume V n as [30,31]:

 !
Wn V n1=3
log Ds log C 1
r 2n rn
P
where the intrusion work W n ni1 Pi DV i , Pi and DV i are the
applied pressure and intruded pore volume at step i; V n and r n
are the intruded volume and pore radius at nth stage of mercury
intrusion process, Ds is the surface fractal dimension, C is a constant.
Fig. 6 shows the surface fractal dimensions of WLM and SLM. In
the figure, when the pore diameter D > 100 lm, the surface fractal
dimensions for WLM and SLM are 4.02 and 3.86, which have no
978 R. Yang et al. / Construction and Building Materials 125 (2016) 974980
(a)
Fig. 5. Pore size distribution of lime mortars from MIP, (a) Differential pore size distribution; (b) Cumulative curves.
(a) WLM
Fig. 6. The surface fractal dimensions for WLM and SLM.
physical sense since Ds must range from 2 and 3 [26]. As aforemen-
tioned, this is probably due to the different pore configurations:
pores in this range (larger than 100 lm) are either air voids intro-
duced during sample preparation or large pores formed by the
sand grains. When the pore diameter D < 17 nm, the data points
of WLM and SLM (the circle points in Fig. 6) are scattered, this
may be due to the large deformation of WLM and SLM and/or to
the collapse of pore walls under high mercury pressure, as argued
by Fadeev et al. [32] and Mahamud et al. [33]. However, when
17 nm < D < 100 lm, the pore structure of WLM and SLM is self-
similar and the determined surface fractal dimensions for SLM
and WLM are respectively 2.95 (with correlation coefficient
99.5%) and 2.92 (with correlation coefficient 99.1%).
The surface fractals of WLM and SLM are close to the magnitude
of the surface fractal dimensions of clay (Ds 2:95) and silt loam
(Ds 2:91) determined by Rieu et al. [12]. The surface fractal
dimensions of WLM and SLM are also similar to that of calcite
sandstone (Ds 2:93) [31]. As proposed by Bartoli et al. [27] and
Pachepsky et al. [28,29], higher fractal surface dimension indicates
more bonds between soil particles, which means that a higher Ds
leads to a higher strength; furthermore, the Ds value increases lin-
early with the content of carbohydrates [27]. Therefore, the higher
surface fractal dimension of SLM indicates the higher strength,
which is consistent with the experimental results of uniaxial com-
(b)
(b) SLM
pressive strength shown in Table 2. Moreover, the surface fractal
dimensions of WLM and SLM indicate the validity range of pore
diameters of soils during MIP test is from 100 lm to 17 nm.
3.5. Microscopic mechanism of the strength
The effect of sticky rice solgel on the bonding strength of SLM
at micro scale is discussed in this section. The sticky rice solgel is
mainly composed of starch gel which consists of amylose and
branched amylopectin, both of which are cross-linked together
and form integral junction zone [34]. Hence, it is expected that
the sticky rice solgel is a binder to cohere the soil grains together.
As shown in Fig. 7, both amylose and amylopectin tend to form
lamellar arrays of hexagonally packed double helices [35]. The sur-
face of starch is negatively charged, where an electrical double
layer is attached [35]. Cation exchange occurs and Ca2 is adsorbed
on the surface of starch [36]. When the carbon dioxide (CO2 ) is
introduced from the atmosphere, the starch surface is manifested
itself as a calcite nucleation site during the carbonation process
(see Fig. 7). Calcite crystals precipitate on the surface of starch
and form an inorganicorganic composite, and this process is ter-
med as biomineralization [35,37]. It should be noted that the gel
pores of starch gel can also act as nucleation site as argued by Parv-
inzadeh Gashti et al. [35], which is not depicted in Fig. 7. The size of
 R. Yang et al. / Construction and Building Materials 125 (2016) 974980 979

Fig. 7. Schematic illustration of formation of calcite crystals in starch, the chains represent the calcite and/or portlandite crystals at micron scale, and the ellipsoids are the
calcite crystals at submicron scale, modified from Parvinzadeh Gashti et al. [35].

the calcite crystals is significantly affected by the crystallization energy during fracture and crack development and consequently
environment during carbonation process. As observed by Yang increase the compressive strength and fracture property of SLM.
et al. [1] and Zeng et al. [6], the size of the calcite crystal in sticky Recalling that the surface fractal dimension of WLM (2.92) is lower
rice solgel (submicrons) is smaller than that formed in distilled than that of SLM (2.95), that may be related to the local pore
water (microns). This may be attributed to the inhibitor effect of network formed within crystal precipitation of SLM (see Fig. 8);
the sticky rice solgel due to its high viscosity [38]. however, the pore network within crystal + starch precipitation
Both WLM and SLM are cohesive granular materials, in which of SLM is so fine that mercury can not penetrate.
the precipitations at the contact points of soil grains substantially
influence the strength of materials (see Fig. 8). As proposed by
Mitchell et al. [36], an electrical double layer is adsorbed on the 4. Concluding remarks
negatively charged soil grain surface, Ca2 exchanges with other
This work presents a comparison study on the behaviors of the
cations (e.g., K ) within the electrical double layer. This makes
lime mortar mixed with distilled water (WLM) and lime mortar
the soil grain surface the nucleation site of calcite crystals. How-
mixed with sticky rice solgel (SLM). The 7-d, 28-d uniaxial com-
ever, as shown in Fig. 8, only the precipitated calcite crystals in
pressive strength and uniaxial compressive strength after 6
contacts of soil grains will effectively enhance the bonding
freezethaw cycles of SLM are higher than those of WLM, which
strength [39].
confirms the favorable effect of sticky rice solgel in improving
As illustrated in the Fig. 8, the packing of these calcite and port-
the mechanical behavior of lime mortar. The mercury intrusion
landite crystals in WLM would be less compact owing to the larger
porosimetry (MIP) analysis demonstrates that the addition of the
size of the crystals; nevertheless, with the addition of the sticky
sticky rice solgel leads to a finer pore structure for lime mortar.
rice solgel, the portlandite crystals, the smaller calcite crystals,
Surface fractal dimension analysis based on the MIP data shows
and the starch forms an organicinorganic composite, leading to
that when pore diameter is larger than 100 lm or smaller than
the higher coherence of the soil particles and a more compact tex-
17 nm, both WLM and SLM are non-fractal; however when pore
ture. The more compact texture induced by the addition of sticky
diameter is between 100 lm and 17 nm, the surface fractal dimen-
rice solgel is partially responsible for the elevated compressive
sions of WLM and SLM are 2.92 and 2.95, respectively; the higher
strength of SLM shown in Table 2. Another reason for the higher
surface fractal dimension indicates the enhanced bonding strength
compressive strength of SLM is that the sticky rice solgel acts as
of soil grains within SLM. The latter is related to the more compact
a kind of binder within SLM, which can significantly dissipate
texture of inorganicorganic composites, and the dissipative effect

Fig. 8. Schematic illustration of mechanism of bonding strength at soil grain contacts within WLM (left) and SLM (right).
980 R. Yang et al. / Construction and Building Materials 125 (2016) 974980
of binder during fracture and crack development owing to the
addition of sticky rice solgel.
Acknowledgments
We thank Dr. Xiangming Kong for helpful discussions. Further-
more, we would like to acknowledge Dr. Jihui Zhao for the assis-
tance with the analysis of XRD patterns. The present study was
supported by the Tsinghua University Research Project Grant No.
2014Z01004.
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