Construction and Building Materials 123 (2016) 274–280

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Construction and Building Materials

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

Waterproof properties of thermal insulation mortar containing vitrified

microsphere
Jianqing Gong ⇑, Zurong Duan, Kaiqiang Sun, Min Xiao
College of Civil Engineering, Hunan University, Changsha 410082, China

h i g h l i g h t s

Effect of the content of vitrified microsphere on the waterproof properties.

Effect of hydrophobically-modified aggregate on the waterproof properties.

Effect of hydrophobically-modified cementing material on the waterproof properties.

Comparison of two methods of hydrophobically-modified.

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

Article history: The waterproof indicators including water absorption, impermeability and wettability were evaluated in
Received 17 November 2015 this paper. First, the optimum vitrified microsphere (VM) content was determined according to the fun-
Received in revised form 11 April 2016 damental performance, water absorption and impermeability of the thermal insulation mortar. The influ-
Accepted 26 April 2016
ence of water to cement ratio (w/c) on consistency of the mortar was then investigated. The results
Available online 13 July 2016
indicated that when w/c was 1.4, the mortar was favorable in terms of workability, strength and durabil-
ity. The test results showed that the hydrophobic treatment of VM surface was beneficial to the reduction
Keywords:
of water absorption. Two hydrophobic treatment methods, i.e., coating with organosilicon hydrophobic
Thermal insulation mortar
Vitrified microsphere
agent (OHA) on VM or blended OHA with cement were compared. According to the testing results of
Water absorption water absorption, the water level decline and water seepage depth, blending OHA with cement was more
Impermeability effective to improve the waterproof performance of the thermal insulation mortar.
Wettability Ó 2016 Published by Elsevier Ltd.

1. Introduction
Unlike the traditional heat insulation lightweight aggregate
involved in architecture engineering, i.e., expanded perlite and
polystyrene particles, vitrified microsphere (VM) is characterized
by relatively higher strength and better fire resistance. Due to its
favorable overall performance, the VM thermal insulation mortar
has attracted increasing attention [1–3]. The researches related
to the VM thermal insulation mortar primarily focused on mechan-
ical properties, thermal characteristics, and fire resistance. S.P.
McBride et al. [4] studied the mechanical properties of lightweight
concrete using VM. The results indicated that the high content of
VM significantly lowered the density and strength of concrete. Li
et al. [5] analyzed the mix proportion and mechanism of VM ther-
mal insulation mortar and the results demonstrated that the VM
content was responsible for the reduction of thermal conductivity
⇑ Corresponding author.
E-mail address: gongjianqing@hnu.edu.cn (J. Gong).
and compressive strength. Md. Akhtar Hossain [6] found that in the
absence of a superplasticizer, when the temperature was less than
200 °C, both the compressive strength and tensile strength of the
cement mortar containing fly ash increased as the temperature
increased, and the cement mortar was optimally resistant to high
temperature when fly ash replaced 50% of the cement. Derek
Kramar and Vivek Bindiganavile [7] explored the effects of the
dry density of lightweight mortar using expanded VM on its
mechanical properties. Fang et al. [8] revealed the correlations
among the dry density, compressive strength and thermal conduc-
tivity of the thermal insulation mortar. Recently, the fire resistance
of thermal insulation mortar containing VM has been attracted
increasing attention [9].
As indicated above, thermal insulation mortar containing VM is
generally characterized by favorable thermal insulation and rela-
tively high strength when compared to thermal insulation mortar
made with other types of traditional lightweight aggregate. How-
ever, there have been few studies carried out on its waterproof
properties. Actually, the hydrophilicity of VM and cement and

http://dx.doi.org/10.1016/j.conbuildmat.2016.04.107
0950-0618/Ó 2016 Published by Elsevier Ltd.
 J. Gong et al. / Construction and Building Materials 123 (2016) 274–280 275

the porous structure of VM affect negatively the waterproof perfor- Table 2

mance of the thermal insulation mortar. Consequently, high water Performance of the vitrified microspheres.

absorption and permeability can often be observed, which is dev- Bulk Thermal Size Cylinder Water Volumetric
astating for the exterior thermal insulation wall [10,11]. Water density conductivity compressive absorption floating
exists in thermal insulation mortar in the phase of solid, liquid or strength
(kg/m3) (W/mK) (mm) (kPa) (%) (%)
gas, and the existence and migration of these three forms of water
can seriously weaken the thermal insulation system, which then 90–110 0.037 0.5–1.5 188 39.5 93

manifests as such problems as freezing, leakage, and water vapor

diffusion [12–17]. When a leak occurs in an external thermal insu-
lation system, the decline of thermal insulation can often be
observed. Additionally, in case of temperature rise or even fire,
the migration of water vapor that is intended to be restrained by
the thermal insulation mortar, can produce enormous stress inside
the mortar, thus resulting in the mortar cracking or even falling. In
winter, in process of freezing, the 9% volume expansion produces
considerable tensile stress in the thermal insulation mortar, thus
causing the entire thermal insulation system to crack or even fall
off. In addition, water can serve as a carrier that triggers the chain
reaction of a thermal insulation system, e.g., the chemical and
physical erosion. Therefore, improving the waterproof perfor-
mance of VM thermal insulation mortar can help improve the sta-
bility and durability of its thermal insulation in the presence of
moisture [18].
This paper mainly aims to study the waterproof performance of
the thermal insulation mortar containing VM. First, the thermal
insulation mortar was prepared which could meet the physical
and mechanical requirements of the specification. Then, the water
absorption, impermeability and wettability were researched.
Methods to improve the waterproof performance of the thermal
insulation mortar, coating organosilicon hydrophobic agent
(OHA) with VM, or blending OHA with the cement was compared.
2. Experimental program
2.1. Raw materials
The raw materials involved in this study is listed in Table 1. The vitrified micro-
sphere was employed as the major thermal insulation component. Organosilicon
hydrophobic agent was used to improve the impermeability, reduce the water
absorption and wettability, and thus contribute to the moisture resistance of the
thermal insulation mortar. The properties of VM and OHA are illustrated in
Tables 2 and 3, respectively.
2.2. Testing methods
The fundamental properties, e.g., dry density, compressive strength and thermal
conductivity of the thermal insulation mortar were tested. The three major water-
proof indicators, i.e., water absorption, impermeability and wettability were
evaluated.
2.2.1. Dry density
Six 70.7 mm  70.7 mm  70.7 mm specimens in a group were made and cured
in molds at (23 ± 2) °C and (50 ± 10)% relative humidity for three days. Subse-
quently, the molds were removed, and the specimens were cured for additional
25 days. Then, the cubic specimens were placed at (105 ± 5) °C and dried to a con-
stant weight. The dry density of each specimen was tested and the average value
was calculated as specified in GB/T 5486.3-2001 [19].
Table 1
Raw materials involved in the experimental program.
Raw materials Abbreviation form
Vitrified microsphere VM
Ordinary Portland cement PO
Polypropylene fiber PF
Redispersible emulsion powder REP
Organosilicon hydrophobic agent OHA
Hydroxypropyl methyl cellulose ether HMCE
Table 3
Main parameters of the water repellent agent.
Product Active Appearance Dilution Wetting angle after
name ingredient ratio hydrophobic modification
BLA101 Surface- Colorless, 1:4 100°–130°
modified transparent
siloxane liquid
2.2.2. Compressive strength
Three 70.7 mm  70.7 mm  70.7 mm specimens in a group were made and
cured in molds at (23 ± 2) °C and (50 ± 10)% relative humidity for three days. The
molds were then removed and the specimens were cured in standard condition
(with relative humidity of 95% and temperature of 20 ± 2 °C) for additional 25 days).
The compressive strength of the thermal insulation mortar was then tested as spec-
ified in GB/T 5486.3-2001 [19].
2.2.3. Thermal conductivity
Three 300 mm  300 mm  30 mm specimens were prepared in a group. The
curing condition was the same as described for compressive strength test. The ther-
mal conductivity was tested according to the method in GB/T 10294-2008 [20].
2.2.4. Water absorption
Three 70.7 mm  70.7 mm  70.7 mm cubes were made and cured for 28 days.
Then, the cubes were dried at (105 ± 0.5) °C for (48 ± 0.5) h, and the mass (m0) was
measured. Each cube was then soaked in water. After being soaked for (48 ± 0.5) h,
the cube was taken out and wiped with a wrung-out wet cloth to achieve saturated
surface dry condition, and its mass (m1) was measured. The water absorption of
each test cube was calculated according to formula (1). Then, the average of the
three test cubes’ results was calculated as the water absorption of the mortar.
m1  m0
Wx ¼  100% ð1Þ
m0
2.2.5. Impermeability
The impermeability affects the durability of the thermal insulation mortar sig-
nificantly. Two indexes to evaluate the impermeability of the thermal insulation
mortar was proposed in reference [21], i.e., water level decline (h0) and water seep-
age depth (h1) within two hours (2 h) (Figs. 1 and 2). The specimens
(70.7 mm  70.7 mm  70.7 mm) were prepared. The curing condition and testing
steps were as following:
(1) The cube that had been cured for 28 days was put in an oven at a temper-
ature of (105 ± 0.5) °C and dried to a constant weight.
(2) The dried cube was placed onto a test bench with its non-shaped surface
facing upwards. An organic glass tube (diameter of 2 cm) with butter
applied to its bottom was erected on the surface of the test cube and then
sealed with hot melted wax. It is necessary to ensure that the sealing
around the tube is firm and that the liquid wax does not enter into the tube
from the bottom, as is shown in Fig. 1.
(3) (200 ± 1) mm of water was poured into the tube within 10 s, and then, the
initial water level was recorded. The water level was recorded at specific
intervals throughout the test for a total of 2 h, and then, the final water level
was recorded. If all of the water in the tube had leaked out before 2 h, this
step would be stopped and step 4 would be initiated. The untreated thermal
insulation mortar had high water absorption. Therefore, the water should
be poured quickly into the tube. It is advised to weigh the amount of water
required to fill the 200 mm-high water column before pouring the water
into the tube.
(4) The organic glass tube was removed, and a blade was used to scrape the
wax and butter from the test cube’s surface. A hacksaw blade was used to
saw the test cube through the center of the installed organic glass tube,
and then, the depth of the water seepage into the test tube was determined,
as is shown in Fig. 2.
276 J. Gong et al. / Construction and Building Materials 123 (2016) 274–280
Fig. 1. Diagram of water level decline for 2 h.
Fig. 2. Diagram of water seepage depth for 2 h.
2.2.6. Consistency
To explore the influence of w/c on consistency of the thermal insulation mortar,
a w/c of 1.3, 1.4, 1.5, 1.6 and 1.7 were varied. The test was carried out as specified in
the Standard for Test Method of Performance on Building Mortar (JGJ70-2009).
2.2.7. Wettability
To exam the limitation of OHA on wettability of the thermal insulation mortar,
contact angle with or without OHA treatment was measured and compared. The
testing procedures are as follow: a water drop was placed onto the surface of the
thermal insulation mortar and then the photo was taken by using a digital camera.
After that, the photo was used to analyze the contact angle.
2.3. Hydrophobic modification of VM
The hydrophilicity and high accessible pores often result in the high water
absorption of the VM, thus weaken the waterproof performance of the thermal
insulation mortar. It is beneficial to soak the VM in OHA solution to transform
the hydrophilicity to hydrophobicity of the surface.
To prepare OHA solution, the OHA-Solvent ratio was kept as 1:8, 1:16 and 1:24,
respectively. VM were sprayed with the three OHA dilutions, respectively. Then,
each group of VM sprayed with a particular dilution was divided into two parts
(thus making six total groups, two identical groups for each dilution). Next, since
the groups of VM sprayed with OHA were divided into two parts, the first part
was placed directly into an oven at a temperature of 80 °C and dried. The remaining
part of each group was dried at room temperature for 72 h and then placed into an
oven at a temperature of 80 °C and dried to a constant weight. Afterwards, tests, i.e.,
water absorption of the dried VM, contact angles of the corresponding thermal
insulation mortar was conducted.
3. Results and discussion
3.1. Influence of VM content on fundamental properties
The mass ratio of PO:REP:HMCE:PF:water was kept as
1:0.03:0.007:0.003:1.5 in this part. The VM content was 25%,
30%, 35%, 40%, 45%, 50%, and 55%, respectively.
The fundamental properties of the thermal insulation mortar
made with different VM contents are shown in Figs. 3 and 4,
respectively. As shown in Figs. 3 and 4, the dry density, compres-
sive strength, and thermal conductivity of the thermal insulation
mortar decreased significantly as VM content increased.
3.2. Influence of VM content on water absorption and impermeability
In contrast, the water absorption of the thermal insulation mor-
tar increased as the VM content increased (see Fig. 5). Likewise, as
shown in Fig. 6, both h0 and h1 for 2 h increased as the VM content
increased. Both h0 and h1 for 2 h increased gradually as the VM
content increased from 25% to 40%. However, after the VM content
exceeded 40%, both factors began to increase rapidly.
A mortar’s impermeability is closely related to its compactness.
Densified mortar usually indicates favorable impermeability.
Therefore, to improve its impermeability, the thermal insulation
mortar is required to have enough cementing materials to com-
pletely coat VM and fill the pores so as to increase the mortar’s
compactness. As was previously mentioned, both h0 and h1 for
2 h changed suddenly when VM content reached 40% (see Fig. 6).
Because the amount of cementing materials decreases with the
increasing of VM content, when VM content exceeded 40%, the
cementing material content is relatively small, the amount of
cementing materials can not completely encased in aggregate
and fill pore, rapid increase of h0 and h1 for 2 h could be observed
which indicated significant reduction of the impermeability.
When VM content was kept as 40%, the compressive strength,
dry density, and thermal conductivity of the VM thermal insulation
mortar were 1.34 MPa, 468 kg/m3, and 0.0933 W/(mK), respec-
tively. The VM content was kept constant as 40% in the subsequent
mix proportion.
3.3. Effect of water-cement ratio on consistency
The relationship between the w/c and the consistency of the
mortar is illustrated in Table 4. When the w/c was 1.4, the thermal
Fig. 3. Effect of different VM contents on dry density and compressive strength.

Fig. 4. Effect of different VM contents on thermal conductivity.
Fig. 5. Effect of different VM contents on water absorption.
Fig. 6. Effect of different VM contents on water level decline and water seepage
depth for 2 h.
Table 4
Effects of the water-cement ratio on the consistency of the thermal insulation mortar
containing vitrified microspheres.
Water-cement ratio
Sinking depth (cm)
J. Gong et al. / Construction and Building Materials 123 (2016) 274–280 277
insulation mortar with a sinking depth of 5.3 cm could be obtained
which could meet the requirements for ordinary operations includ-
ing mixing, transportation, placing and finishing. Due to the
adverse effect of higher w/c on strength and durability of the ther-
mal insulation mortar, w/c of 1.4 was determined as the optimum
in the subsequent tests.
3.4. Effect of hydrophobic treatment of VM on water absorption
The water absorption of VM with or without OHA treatment is
shown in Table 5. As shown in Table 5, the water absorption of the
untreated VM was as high as 39.5%, whereas the water absorption
of the OHA-treated VM declined significantly. Obvious reduction of
water absorption could be observed in No. 5#, No. 6# and No. 7#,
approximately 60% lower than that of the untreated VM.
No. 2# and 5# had high OHA concentration and the lowest water
absorption of the VM; however, the reduction of the water absorp-
tion was negligible when compared with the other four OHA con-
centrations (with a less than 3% difference). The small difference in
the water absorption among the VM treated with different water
repellent agent concentrations also indicated that these three
water repellent agent concentrations were already sufficient for
preventing water from entering the accessible pores of the VM.
The water repellent agent deposited on VM surface and con-
tributed to the improved hydrophobicity, however, excess water
repellent agent would be washed away in application due to the
infirm bonding with VM.
The water absorption of the VM dried in Batch No. 2 were lower
than those dried in Batch No. 1, thus indicating that the second
drying method contributed more to the improvement of the
hydrophobic modification effects. In addition, in the controlled
experiments in which the same water repellent agent concentra-
tions were used to treat the VM (experiments 2# and 5#, 3# and
6#, and 4# and 7#), the turbidities of the water collected in the
measuring cylinders differed greatly, and the water collected in
Experiment 2# was more turbid than that collected in Experiment
5#, the water collected in Experiment 3# more turbid than that col-
lected in Experiment 6#, and finally, the water collected in Exper-
iment 4# more turbid than that collected in Experiment 7#. From
these results, it becomes apparent that drying the VM coated with
the OHA at room temperature facilitated the steady attachment of
the OHA to the surface of the VM as well as contributed to the
improvement in the utilization efficiency of the OHA.
To sum the results, the use of the OHA to treat the VM could
hydrophobically modify the aggregate surface, but the water repel-
lent agent concentration had an insignificant effect on the water
absorption of VM. To reduce the cost, the VM that were selected
for subsequent experiments were sprayed with OHA with a con-
centration of 1:24, then dried at room temperature, and finally
put into an oven at a temperature of 80 °C and dried to a constant
weight.
Table 5
Water absorptions of the vitrified microspheres before and after hydrophobic
treatment.
Experiment Dilution ratio of the water Batch No. of drying Water
No. repellent absorption (%)
1# Untreated Dried to constant 39.5
weight
2# 1:8 1 18.5
3# 1:16 1 19.3
4# 1:24 1 20.8
5# 1:8 2 16.5
1.3 1.4 1.5 1.6 1.7
6# 1:16 2 16.8
3.1 5.3 8.1 9.6 11.4 7# 1:24 2 17.6
278 J. Gong et al. / Construction and Building Materials 123 (2016) 274–280

Fig. 7. Contact angles of the thermal insulation mortar: a. Untreated; b. Coating OHA with VM; c. Blending OHA with cement.

Fig. 8. SEM pictures of the thermal insulation mortar: a. Untreated VM; b. VM Coating with OHA; c. Untreated thermal insulation mortar; d. Thermal insulation mortar
containing modified VM; e. Thermal insulation mortar blending OHA with cement.

3.5. Influence of hydrophobic treatment of VM/PO on water absorption

Table 6 and impermeability
Influence of OHA treatment on water absorption and impermeability.

Group 1 2 3 The mix proportion of PO:VM:REP:HMCE:PF was controlled as

Without treatment VM treated PO treated 1:0.65:0.03:0.007:0.003:1.4 in this part. Three groups of VM ther-
with OHA with OHA with OHA mal insulation mortar were prepared. The first group was
Water absorption (%) 29.4 22.7 13.9 untreated. In the second group, after being dried at room temper-
Water level Decline in 51.0 46.0 4.0 ature, the VM was put into an oven at a temperature of 80 °C, dried
2 h (mm) to a constant weight, and then sprayed with the OHA. In the third
Water seepage depth in 26.5 29.0 8.0 group, 1.2% OHA was blended with the cementing material. The
2 h (mm)
test results are shown in Table 6.
 J. Gong et al. / Construction and Building Materials 123 (2016) 274–280
As shown in Table 6, the water absorptions of the thermal insu-
lation mortars coating OHA on VM surface or blending OHA with
cement decreased compared to that of the unmodified reference.
This was because the hydrophobic treatment of the aggregate
decreased the compactness of the mortar, and thus, there were
more pores present in the mortar, which absorbed considerable
moisture, thereby reducing the decrease in the water absorption
of the mortar caused by the hydrophobic treatment of the aggre-
gate. In addition, compared to the thermal insulation mortar con-
taining the hydrophobically-modified aggregate, the thermal
insulation mortar containing the hydrophobically-modified
cementing material had obvious decreased water absorption,
decline in water level for 2 h, and depth of water seepage for 2 h.
This was because the active functional groups (such as hydroxyls
generated from the hydrolysis of the hydrophilic functional groups
of the silane released from the OHA, which has high water solubil-
ity, into the mixing water after being dissolved in water) reacted
with the surface active groups in the hydration products of the
cementing material, such as hydroxyls, to form hydrogen bonds
or covalent bonds so as to enable the silane to attach to the surface
or to the inside pore walls of the hydrates of the cementing mate-
rial. The hydrophobic organic functional groups of the silane faced
the outside of the pore walls, resulting in the formation of a stable
hydrophobic film on the surface of the cement mortar and pores.
The molecular structure of the hydrophobic film primarily con-
sisted of SiAC bonds and SiAO bonds with high bond energy.
Therefore, the hydrophobic film had a compact structure that
was uneasily to be damaged and was also strongly resistant to high
temperature, oxidation, and erosion. In addition, the hydrophobic
film with a large molecular volume could effectively prevent the
hydrates of the cementing material from coming into direct con-
tact with the water, thus changing the hydrophilic properties of
the mortar itself. The process in which the OHA reacted with the
cementing material to form the hydrophobic film is shown in for-
mula (2). This hydrophobic planar siloxane molecular film with
small surface tension can be firmly attached to the cement-based
material, thereby rendering its surface and inner pore walls highly
hydrophobic.
R R R R
Irreversible polycondensation
OH Si OH OH Si OHOH Si OH
OH OH OH
Hydrates of cementing material
In addition, the contact angles of the original thermal insulation
mortar, treated with OHA on VM surface and blended OHA with
cement were tested, respectively. As shown in Fig. 7, the contact
angles of the hydrophobically-treated thermal insulation mortar
increased considerably compared to that of the untreated thermal
insulation mortar, indicating significant reduction of the wettabil-
ity. Additionally, the thermal insulation mortar blended OHA with
cement was superior to that of coating OHA on VM surface.
As shown in Fig. 8, SEM photos were taken to observe the differ-
ence of VM, hydrophobically-treated VM, thermal insulation mortar
and hydrophobically-treated thermal insulation mortar,
respectively.
Unlike VM without processing by OHA in Fig. 8a, the
hydrophobically-modified VM (see Fig. 8b) was coated with a
279
waterproof film on the surface, which consequently resulted in
the significant reduction of the water absorption. As shown in
Fig. 8c and d, however, there was not a significant difference
between the microstructure of the thermal insulation mortar trea-
ted with OHA or not. Fig. 8e is the SEM picture of the thermal insu-
lation mortar containing the cementing material mixed with OHA.
As demonstrated in Fig. 8(e), the hydrates were characterized by
smooth surface and densified structure, indicating that the addi-
tion of OHA to the mortar could consume the hydroxyls in the
hydrates, thereby resulting in mature hydration of the cementing
material, tighter lapping of its crystals, and increased compactness
of its hydrates [22–25]. The removal of the large, discontinuous
crystals in the presence of OHA decreased the adverse effect on
the cement mortar strength. The above-mentioned microstructural
characteristics could aid in significantly improving the imperme-
ability, the chemical erosion and freeze-thawing resistance of the
thermal insulation mortar [26].
4. Conclusions
As the VM content increased, the dry density, compressive
strength, and thermal conductivity of the thermal insulation mor-
tar decreased, whereas the water absorption, decline in water level
for 2 h, and depth of water seepage for 2 h increased. The thermal
insulation mortar with a VM content of 40% was optimum in terms
of impermeability and the corresponding thermal insulation mor-
tar could meet the fundamental requirements.
Compared to the unmodified aggregate, the hydrophobic treat-
ment with water repellent agent resulted in the significant reduc-
tion of water absorption. However, the difference of the water
repellent agent concentration made insignificant influence on the
water absorption of vitrified microspheres.
The two methods, i.e., coating water repellent agent on vitrified
microspheres surface or blending water repellent agent with
cement, are efficient in reducing the water absorption, permeabil-
ity and wettability. In addition, blending water repellent agent
with cement is more favorable and recommended.
R R
O Si O Si O Si O
ð2Þ
O O O
Hydrates of cementing material
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