Materials and Design 64 (2014) 497–502

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Materials and Design

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Effects of water content, magnesia-to-phosphate molar ratio and age

on pore structure, strength and permeability of magnesium potassium
phosphate cement paste
Hongyan Ma a, Biwan Xu a, Jun Liu b, Huafu Pei a, Zongjin Li a,⇑
a
Department of Civil and Environmental Engineering, The Hong Kong University of Science and Technology, Hong Kong, China
b
Guangdong Provincial Key Laboratory of Durability for Marine Civil Engineering, College of Civil Engineering, Shenzhen University, Shenzhen 518060, China

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

Article history: In this study, the pore structure of magnesium potassium phosphate cement paste is investigated using
Received 26 June 2014 mercury intrusion porosimetry. Several mix proportions, obtained by changing the magnesia-to-phos-
Accepted 31 July 2014 phate molar ratio (M/P) and the water-to-cement mass ratio (W/C) of the material, are involved. It is
Available online 14 August 2014
found that lower W/C and longer material age make the porosity lower and the pore structure finer.
When the W/C is kept constant, both porosity and critical pore diameter are not monotonic functions
Keywords: of M/P, but the M/P of 6 gives the lowest porosity and the smallest critical pore diameter. Also, the
Magnesium potassium phosphate cement
M/P of 6 shows the highest compressive strength and the lowest intrinsic permeability. Based on the
Chemically bonded ceramics
Pore structure
experimental results, empirical models describing the relations between the properties and pore struc-
Compressive strength ture parameters (porosity / and critical pore diameter dc) of MKPC paste are developed. The compressive
2
Intrinsic permeability strength is inversely proportional to /, and the intrinsic permeability is directly proportional to dc /.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction
Magnesia–phosphate cements (MPCs) are low-temperature
high-strength materials formed by through-solution acid–based
reaction between dead burned magnesia and phosphate [1], and
also known as chemically bonded ceramics [2]. MPCs have been
widely utilized in many engineering applications, including repair
and rehabilitation of civil structures [3], treatment of waste water
[4,5], stabilization of toxic matters and nuclear wastes [6–10], den-
tal and bone restorations [11,12], and so on. In civil engineering,
MPCs are frequently used as repair materials for pavements and
structures, as they set very fast and produce high strength patches
with low permeability, little drying shrinkage and good durability
[13–17]. Two types of MPCs appear the most frequently in both
engineering practice and academic research, one uses ADP (ammo-
nium dihydrogen phosphate) while the other uses KDP (potassium
dihydrogen phosphate) as the phosphate components. The former
can be termed as MAPC, and the latter MKPC, as the main reaction
products in the two systems are magnesium ammonium phos-
phate (MAP) hexahydrate and magnesium potassium phosphate
(MKP) hexahydrate, respectively. Compared with MAPC, MKPC
does not generate unpleasant odor when it reacts with water not
⇑ Corresponding author. Tel.: +852 23588751.
E-mail addresses: mhy1103@gmail.com (H. Ma), zongjin@ust.hk (Z. Li).
only, but also the rate of this reaction is easier to be controlled
because KDP has smaller dissociation constant and lower solubility
than ADP. Due to these two advantages, MKPC seems to be more
favored in recent years [3–6,18–20]. As frequently cited
[11,18,21], the chemical reaction between MKPC and water can
be written as
MgO þ KH2 PO4 þ 5H2 O ! MgKPO4  6H2 O ð1Þ
and this can be approximately assumed to be the sole reaction in a
MKPC paste [22].
In the literature, most of the studies on MPCs seemed to directly
focus on the engineering properties of MPCs-based materials, e.g.
setting time, fluidity and strength, to obtain optimized formula
based on locally available raw materials [3,16–20], and a few
investigated the reaction mechanisms of MPCs [23–26]. In the
above-mentioned applications, trial-and-error strategy was nor-
mally used, while the material, to the authors’ knowledge, can still
not been effectively designed so far. To design the material, the
microstructure and its influence on the macroscopic engineering
properties have to be fully studied. Pore structure is an effective
representation of the microstructure, and the mechanical proper-
ties as well as transport properties of a porous material are
strongly related to its pore structure. Therefore, it is imperative
to study the pore structure of MPCs-based materials, for better
understanding their performance.

http://dx.doi.org/10.1016/j.matdes.2014.07.073
0261-3069/Ó 2014 Elsevier Ltd. All rights reserved.
498 H. Ma et al. / Materials and Design 64 (2014) 497–502

In the present study, the pore structure of MKPC paste is firstly
examined by MIP (mercury intrusion porosimetry), in terms of
porosity, pore size distribution and critical pore diameter, to see
how the pore structure is affected by key material parameters,
including W/C (the water-to-cement mass ratio), M/P (the magne-
sia-to-phosphate molar ratio) and the material age. Furthermore,
the evolutions of compressive strength and intrinsic permeability
of MKPC paste following increasing ages are measured, and their
relations with the pore structure are finally obtained in light of
mathematical fittings.
2. Materials and experiments
In experiments, MKPC pastes were made from dead burnt mag-
nesia powder (calcined under 1500 °C for 5 h) with a purity of
95.1%, powder KDP (chemical reagent) and deionized water. The
magnesia powder was supplied by Jinan Magnesia-Carbon Brick
Plant Co. Ltd., Shandong, China, and the KDP by Guangzhou Chem-
ical Reagent Factory, Guangdong, China. Mix proportions involved
in the experiments, in terms of W/C and M/P, are listed in Table 1.
In the table, the mixed pastes were named by character strings, of
which the former half indicates the W/C and the latter half indi-
cates the M/P. For example, W15M04 indicates a paste with the
W/C of 0.15 and the M/P of 4. In the mix proportions, W/C ranges
from 0.15 to 0.5, and M/P from 4 to 12. For specimen preparation,
powders were first weighted according to the M/P and dry-mixed,
then mixed with a specific mass of water as calculated from the
W/C. Note that the cement included magnesia and KDP only, and
retarder was not used, as the initial set times of all the listed mix-
tures were longer than 10 min due to the relatively low reactivity
of the heavily calcined magnesia. The mixing procedure involved
firstly dry-mixing the powders for 1 min and then further mixing
them with water for 3 min, in a vertical-axis planetary mixer.
The mixed fresh pastes were cast into plastic tubes with the
diameter of 2 cm and then sealed by plastic sheets. The specimens
were de-molded and sealed in airtight plastic bags after 12 h, and
placed at 25 ± 1 °C. At the ages of 3, 7 and 28 days, specimens were
taken out of the bags. After skin removed, the central portions of
the specimens were sawn into small cuboids with the smallest
dimensions of 3–5 mm. The obtained cuboids were then vacuum-
dried to constant weight, and used as samples for pore structure
measurement by MIP, as recommended by Ma [27]. The total
porosity intruded by mercury was used as an index of porosity,
although it is normally slightly lower than the true porosity [28].
The pore size distribution was obtained in light of the well-known
Washburn equation, i.e.
4c cos h
d¼
P corresponds to the critical pore diameter, and the secondary one
where d is the equivalent pore diameter, c is the surface tension of
mercury, h is the contact angle between the mercury and the pore
surface, and P is the applied pressure. As recommended in the liter-
ature [27], 480 mN/m and 130° can be adopted for c and h, respec-
tively, and thus d in lm can be obtained as a function of P in MPa.
The critical pore diameter, corresponding to the steepest point on a
cumulative porosity curve or the highest point on a logarithmic
differential porosity curve [27,29], was also determined as an index
of the pore structure connectivity. It has been proven that the
critical pore diameter has strong relations with both diffusivity
and permeability of a porous material [30,31].
The fresh pastes were also cast into cubic molds, with the side
length of 40 mm, for the purpose of compressive strength mea-
surement. Disk-shaped specimens were also prepared to deter-
mine the intrinsic permeability. All specimens were cured under
the same conditions as mentioned above. At the ages of 3, 7 and
28 days, compressive strengths were tested according to ASTM
C109, on a MTS 815 ROCK Mechanics machine [32], and the gas
permeability coefficients were also tested according to the method
used by Shi et al. [33] using nitrogen gas. The gas permeability
coefficient was then transformed to intrinsic permeability of the
material as
lk
j¼ ð3Þ
qg
where j (m2) is the intrinsic permeability of the material, which is
fluid independent, and k (m/s) is the nitrogen gas permeability
coefficient. Besides, g (m/s2) denotes the gravitational acceleration,
q (kg/m3) and l (Pas) denote the density and dynamic viscosity of
nitrogen gas, respectively. It is worth noting that all tests were
repeated for three times, and the average values are reported in
the present paper.
3. Results
3.1. Pore structure of MKPC paste
3.1.1. Influence of material age
Employing MIP results, the pore structure can be illustrated by
two tools, i.e. the cumulative porosity curve describing the relation
between the porosity and the logarithmic pore diameter, and the
logarithmic differential porosity curve showing the slope changing
of the cumulative porosity curve. The pore structure evolutions of
aged MKPC pastes are shown in Fig. 1, which takes the paste
W15M04 as an example. Comparing the cumulative porosity
curves (black), it can be seen that the porosity decreases continu-
ously with increasing ages. This is a certain result of the continuous
reaction between the cement components and water, which gener-
ates more and more solid phase. In addition, the cumulative poros-
ity curves slightly move toward the small pore size direction,
showing the refinement of the pore structure. On each logarithmic
ð2Þ porosity curve (red), two peaks can be identified. The primary one
may be attributed to the consumed KDP particles in the chemical
reaction as shown in Eq. (1).
In MIP results, the pore size distribution curves can only be used
for the purpose of qualitative comparison [28,34], as shown above.
While the pore structures can be described quantitatively only in

Table 1
Mix proportions, porosities and critical pore diameters of MKPC pastes.

Paste name Mix proportion Porosity (%) Critical diameter (lm)

W/C M/P 3d 7d 28 d 3d 7d 28 d
W15M04 0.15 4 10.69 9.43 8.02 1.36 1.21 0.66
W20M04 0.20 4 11.61 10.13 8.18 1.92 1.46 1.34
W20M06 0.20 6 8.68 7.40 6.31 1.19 0.49 0.33
W20M08 0.20 8 9.83 9.04 7.92 1.32 0.73 0.53
W20M12 0.20 12 15.62 14.29 13.98 2.84 2.57 1.96
W50M04 0.50 4 38.67 33.93 32.36 3.36 3.12 2.96
 H. Ma et al. / Materials and Design 64 (2014) 497–502 499

Fig. 1. Pore structure evolution of MKPC paste following increasing ages. Fig. 3. Comparison of the pore structures of MKPC pastes with the same W/C but
different M/P at the age of 3 days.

terms of porosity and critical pore diameter (as an index of the

pore network connectivity) [35]. The porosities and critical pore
diameters of all test MKPC pastes are collected in Table 1. It can
be seen that, with increasing ages, the critical pore diameter
becomes smaller. In the case of W15M04, it decreases from
1.36 lm at the age of 3 days to 0.66 lm at the age of 28 days, indi-
cating an increasing of tortuosity or a decreasing of connectivity of
the pore network. This trend holds in all test pastes.

3.1.2. Influence of W/C

Pore structures, expressed by the cumulative porosity curves, of
MKPC pastes with the same M/P of 4, but different W/C, are com-
pared at the age of 28 days, as shown in Fig. 2. When the M/P is
kept constant, the higher the W/C, the higher the porosity and
the coarser the pore structure, at the same age. In the three pastes,
W50M04 gives the largest porosity (32.36%) and critical pore Fig. 4. The relation between critical pore diameter and porosity of MKPC pastes.
diameter (2.96 lm). Although the porosity of W15M04 (8.02%) at
the age of 28 days is only slightly lower than that of W20M04
with the M/P of 6 gives the lowest porosity, which is followed by 8,
(8.18%), its critical pore diameter (0.66 lm) is much smaller than
4 and 12 in an ascending order. Critical pore diameters follow a
that of W20M04 (1.34 lm). This is also not out of expectation, as
similar trend to that of porosities. Actually, these trends are not
higher W/C provides more space for the accommodation of the
only valid at the age of 3 days, but hold at all other test ages, as
reaction products, and normally leads to higher porosity and larger
shown in Table 1.
connectivity [36].

3.1.4. Relation between porosity and critical pore diameter

3.1.3. Influence of M/P
The influence of M/P on the pore structure of MKPC paste is
investigated on the basis of constant W/C (0.20). Pore structures
of pastes with the W/C of 0.2 but different M/P, at the age of 3 days,
are compared in Fig. 3. According to this comparison, the porosity
of MKPC paste is not a monotonic function of the M/P, but the paste
Porosities and critical pore diameters of all the test MKPC pastes
at all test ages are listed in Table 1. Looking over the data, it seems
that the lower the porosity, the smaller the critical pore diameter.
In Fig. 4, the critical pore diameters are plotted versus the corre-
sponding porosities. When the W/C is relatively low (0.15 and
0.20), the relation between critical pore diameter and porosity
can be described as a linear function, namely
dc ¼ 0:26  /  1:29 ð4Þ
where dc (lm) denotes the critical pore diameter, and / (%) the
porosity. However, when the W/C is high (0.50), data points deviate
severely from the line, and should be described by another function,
which is not written up due to the limited points.

3.2. Relation between compressive strength and pore structure

The compressive strengths of the MKPC pastes tested at 3, 7 and

Fig. 2. Comparison of the pore structures of MKPC pastes with the same M/P but
different W/C.
28 days are plotted against age in Fig. 5. It can be seen that, the
compressive strength of a MKPC paste increases following age, in
a decelerating way. When the M/P is kept constant, higher W/C
leads to lower compressive strength, at the same age. When the
W/C is kept constant, the M/P of 6 gives the highest compressive
strength, which is followed by 8, 4 and 12 in a descending order.
Although material strength is normally attributed more to the solid
500 H. Ma et al. / Materials and Design 64 (2014) 497–502
Fig. 5. Compressive strength evolutions of the MKPC pastes.
phase, the pore phase can significantly affect the strength as it
breaks the connectivity of the solid phase [37–40]. All these trends
are consistent with those of porosities, i.e. the higher the porosity,
the lower the compressive strength, and vice versa. Since in the
pore structure parameters, porosity has the strongest relation with
compressive strength [41–43], a unique relation between com-
pressive strength and porosity is possible to be found.
The compressive strengths shown in Fig. 5 are plotted against
the corresponding porosities collected in Table 1, as shown in
Fig. 6. It is obvious that the compressive strength decreases follow-
ing the increasing porosities in an inversely proportional way, and
through curve fitting, the relation can be obtained as
f c ¼ 434=/ þ 4:29
where fc is the compressive strength in MPa, and the coefficient of
determination R2 equals 0.948.
3.3. Relation between intrinsic permeability and pore structure
The evolutions of intrinsic permeability of MKPC pastes are
shown in Fig. 7. Contrary to the evolution of compressive
strength, the intrinsic permeability decreases following increasing
ages in a decelerating manner, due to the filling of pores and the
refinement of the pore structure. When the M/P is kept constant,
higher W/C means higher permeability at the same age. When the
W/C is kept constant, the M/P of 6 gives the lowest permeability,
which is followed by 8, 4 and 12 in an ascending order. By a sim-
ple comparison, one may conclude that the higher the compres-
sive strength, the lower the intrinsic permeability. However,
unlike compressive strength which varies from 10 MPa to
Fig. 6. The relation between compressive strength and porosity of MKPC paste.
Fig. 7. Intrinsic permeability evolutions of the MKPC pastes.
70 MPa as shown in Fig. 5, the intrinsic permeability varies from
3  1018 m2 to 2  1015 m2, as shown in Fig. 7, covering 3
orders of magnitude. As proven by researchers [42–47], transport
properties of a porous material are determined by not only poros-
ity, but also the way in which the pores are connected.
Katz–Thompson equation [30] is a simple model relating the
intrinsic permeability of a porous medium to its pore structure,
and has been validated for many times. It can be expressed as
2
dc
j¼ ð6Þ
226  F
where 226 is an analytical constant based on cylindrical pore shape
assumption, and F denotes the formation factor which is unitless.
ð5Þ
Since the formation factor can be related to the porosity as [48]
sD
F¼ ð7Þ
/
where sD is the diffusion tortuosity which is also unitless, Eq. (6)
can be re-written as
2
dc /
j¼ ð8Þ
226  sD
Combining some parameters, an equation which is consistent
with the simple form given by Garboczi [45] can be derived as
j ¼ b  d2c / ð9Þ
where b is a unitless parameter taking into account the pore phase
connectivity, being 1 for straight and non-intersecting tubes while
smaller in other cases. As will be shown, b can approximately be
treated as a constant for this material, thus it can be considered that
Fig. 8. The relation between intrinsic permeability and pore structure of MKPC
paste.
 H. Ma et al. / Materials and Design 64 (2014) 497–502
Initial
Fig. 9. Sketch of the microstructure evolution of MKPC paste. Red, white, green, blue and black in the sketch represent unreacted magnesia, unreacted KDP, reaction product,
water and air void, respectively, and pores include water and air void. (For interpretation of the references to color in this figure legend, the reader is referred to the web
version of this article.)
2 2
the permeability is determined by dc /. The dc / is thus termed as
‘‘permeability determiner’’ in this paper. In Fig. 8, the intrinsic per-
meability values shown in Fig. 7 are plotted against the permeabil-
2
ity determiner dc /. Using Eq. (9) to fit the data sets, b can be
obtained as 3.09  104, with a coefficient of determination R2 as
high as 0.967. As shown in Fig. 4, a unique relation between dc
and / does not exist, thus Eq. (9) cannot be further simplified to a
mono-variable equation.
4. Discussion
In the reaction between MPC and water, phosphate is dissolved
continuously in water, and the reaction occurs on the wetted sur-
face of magnesia particles. The reaction products grow around
magnesia particles and connect with each other, developing the
cementitious matrix [25]. According to this mechanism, pores orig-
inally occupied by water will decrease undoubtedly in size and vol-
ume following the reaction process. However, when phosphate
particles are consumed partially or completely, relatively large
voids will be left. This hypothesis is sketched in Fig. 9, in light of
an algorithm developed for the microstructure simulation of MKPC
paste [22]. As shown in Fig. 1, in a specific paste, the volume frac-
tions of small pores decrease with increasing ages, but those of
pores larger than several microns do not decrease obviously. This
phenomenon could be attributed to the voids formed due to the
consumption of KDP, as shown in Fig. 9.
It has been found that when the W/C is constant, the properties,
including porosity, critical pore diameter, compressive strength
and permeability, are all not monotonic functions of M/P. Similar
phenomena were also reported by others [3,17,19], who found that
the compressive strength and flexural strength are not monotonic
functions of M/P. The optimized M/P in terms of strengths distrib-
uted in the range from 4 to 8, perhaps depending on the chemical
composition of the magnesia. The reason of this phenomenon is
still not clear. Future study on the reaction kinetics of MKPC and
water may help to understand it.
A central work of designing a MKPC-based material is to predict
its properties based on the proportioning parameters or micro-
structure parameters. Eqs. (5) and (9) provide the ways of predict-
ing properties from the pore structure, but valid property–time
relation models may be more straightforward and convenient to
use for design purpose. This is another reason why the reaction
kinetics, which describe the time-dependency of the degree of
reaction, should be emphasized in future works. It is worth noting
that Eq. (5) is physically meaningless, but a purely empirical
model. In the case of Portland cement based materials, the com-
pressive strength is directly proportional to the so-called gel-space
ratio [41], which indicates the filling ratio of space by cement
501
Low degree of reaction High degree of reaction
hydration products, and has a clear physical meaning. Once the
reaction kinetics of MKPC paste are solved, the degree of reaction
will be considered to define a parameter similar with the gel-space
ratio, and a physically meaningful model will be developed to pre-
dict the compressive strength, as well as other mechanical proper-
ties. Strictly speaking, both the diffusion tortuosity sD in Eq. (8) and
the connectivity parameter b in Eq. (9) are pore-structure-depen-
dent parameters, rather than constants. However, as proven in a
numerical study, their values vary only in very limited ranges for
a specific type of porous medium [44]. Therefore, considering b
as a constant will not bring significant errors, which can be proven
somewhat by the fitting shown in Fig. 8.
5. Conclusions
The pore structure of MKPC paste is firstly investigated in this
study, and then its influences on the compressive strength and
intrinsic permeability are analyzed. Through this study, several
conclusions can be drawn as follows:
(1) Lower W/C and longer age make the porosity lower while
the pore structure finer, which is totally a consequence of
being expected and not surprising.
(2) When the W/C is kept constant, both porosity and critical pore
diameter are not monotonic functions of M/P, but the M/P of 6
gives the lowest porosity and the smallest critical pore diam-
eter. The M/P of 6 also shows the highest compressive
strength and the lowest intrinsic permeability. An optimum
M/P of MKPC-based material should depends on the chemical
composition of the dead burnt magnesia used as raw mate-
rial. Why such an optimum M/P exists cannot be explained
until the reaction kinetics of this material are revealed.
(3) The compressive strength increases, while the intrinsic per-
meability decreases following increasing ages. Generally,
higher porosity leads to lower compressive strength, while
lower porosity and smaller critical pore diameter result in
lower intrinsic permeability.
(4) Two empirical models are developed to describe the relations
between the properties and pore structure of MKPC paste,
according to which, the compressive strength is inversely
proportional to porosity (/), and the intrinsic permeability
2
is directly proportional to a permeability determiner (dc /).
Acknowledgement
The financial support from the Hong Kong Research Grants
Council under 615810 is gratefully acknowledged.
502 H. Ma et al. / Materials and Design 64 (2014) 497–502

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