Construction and Building Materials xxx (2016) xxxxxx

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Construction and Building Materials

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

An analysis of the steam curing and autoclaving process parameters

for reactive powder concretes
Tomasz Zdeb
Cracow University of Technology, Warszawska 24, 31-155 Cracow, Poland

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 The optimum RPC steaming and

autoclaving parameters were
determined.
 The efficiency of steel fibres
depending on RPC curing conditions
was investigated.
 The changes in microstructure of RPC
cured at elevated temperature were
described.

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

Article history: The two different methods of thermal treatment were used when curing reactive powder concretes (RPC),
Received 26 February 2016 namely low-pressure steam curing and autoclaving. The properties of obtained material were referred to
Received in revised form 13 October 2016 those of materials cured in water at a temperature of 20 C. The main aim of this study is to verify
Accepted 6 November 2016
mechanical properties of RPC without fibres, at variable steaming and autoclaving parameters. The fol-
Available online xxxx
lowing factors were taken into account: preset time, target temperature and holding time. At the same
time by using the techniques of SEM and MIP, changes in microstructure of composites cured at an
Keywords:
increasing temperature and different time were observed. After establishing the most favourable heat
Reactive powder concrete
Steam curing
treatment parameters, their effect on the efficiency of steel fibres of 6 mm long added at amount of 2%
Autoclaving by volume was analysed. Compressive strength and three-point flexural strength were tested along with
Mechanical properties deformability evaluation. The factor having the strongest effect on mechanical properties of RPC under
Microstructure examination was the target temperature of steaming and autoclaving. RPC curing conditions had also
a significant impact on post-critical strains in composites containing dispersed reinforcement.
2016 Elsevier Ltd. All rights reserved.

1. Introduction autoclaving processes of RPC, in order to establish their optimal

In recent years many work has been done to improve reactive
powder concrete properties by application of sophisticated treat-
ment during setting of this cementitious and high performance
composite. The impact of selected heat treatment parameters on
RPC properties was studied by [13] as well as the effect of com-
pression [4] and vacuuming [5] of concrete mixture was evaluated.
This comprehensive research is focused on both steaming and
E-mail address: tzdeb@pk.edu.pl
parameters.
The steaming process (S) carried out at a temperature not
exceeding 100 C, thus at steam pressure below 1 bar, at first place
is aimed at accelerating the binder hydration processes that in turn
may lead to reaching high material strength in a relatively short
time. However, improperly selected steaming parameters, and at
first place preset time may lead to some adverse phenomena,
for example DEF type corrosion [6]. Improperly controlled curing
of a material at elevated temperature may reduce strength
parameters due to another reason. The products of calcium silicate

http://dx.doi.org/10.1016/j.conbuildmat.2016.11.026
0950-0618/ 2016 Elsevier Ltd. All rights reserved.

Please cite this article in press as: T. Zdeb, An analysis of the steam curing and autoclaving process parameters for reactive powder concretes, Constr. Build.
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2 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx

hydration, naturally formed, are characterised of strongly devel- Table 1

oped specific surface area that is reduced by increasing tempera- Chemical, physical and mechanical properties of RPC components.

ture. This in turn may cause their poorer adhesion to composite Cement Silica Quartz Quartz
aggregate grains [7]. RPC steaming cycles used by various research- fume powder sand
ers are highly differentiated. Both preset time changing from few Chemical composition [%]
hours 06 [8,9] and reaches even few days 37 [2], as well as mate- SiO2 22.98 94.06 99.0 98.5
rial holding time at the maximum temperature from 9 to 96 h Al2O3 4.41 0.74 0.3 0.8
Fe2O3 2.10 0.78 0.05 0.03
[9,10] are varied. However, the low-pressure steaming tempera- CaO 65.58 0.06 <0.1
ture in the vast majority of publications is 90 C. MgO 1.06 0.49 <0.1
The properly selected autoclaving cycle parameters (A), a Na2Oe 0.51 1.43 0.2
hydrothermal treatment carried out at a temperature above SO3 3.32 0.63
Cl- 0.009
100 C and pressure higher than 1 bar, like steaming cause a rapid
increase in mechanical properties, and also reduction in porosity, Mineral composition [%]
C3S 59.1
shrinkage and an increase in resistance to chemical aggression.
C2S 18.0
The autoclaving process eliminates, among other things, the occur- C3A 8.1
rence of secondary ettringite. This results from the fact that a sig- C4AF 6.4
nificant amount of Al3+ and SO2- 4 ions are built in the structure of Physical and mechanical properties
hydrated calcium silicates during hydrothermal treatment [11 Specific surface [m2/g] 0.41 22.4 0.8 0.04
14]. Additional advantages resulting from autoclaving cementi- Density [g/cm3] 3.10 2.23 2.65 2.65
tious materials, including RPC, are related to changes in its struc- Initial setting time [min] 130
Final setting time [min] 220
ture consisting primarily in the appearance of crystalline forms Compressive strength after 35
of hydrated calcium silicates. The type of formed ordered C-S-H 2 days [MPa]
structures depends on many factors, among other things, on tem- Compressive strength after 71
perature, pressure, C/S ratios for substrates or guest ions that sta- 28 days [MPa]
bilize some phases. In autoclaved cementitious materials
tobermorite and xonotlite of very well investigated and described
structures [1012] occur as the most common phases. The occur- (SF), and polycarboxylate based superplasticizer were used. Brass
rence of both phases in autoclaved RPC materials was confirmed coated steel fibres of 6 mm in length and 0.175 mm in diameter
by a number of researchers [1518]. However, it should be noted of 2200 MPa in tensile strength, density of 7.76 g/cm3 and modulus
that there are some unfavourable CaO/SiO2 proportions at which of elasticity of 210 GPa were used. Steel fibres were incorporated to
crystallization of hydrated calcium silicates leads to formation of concrete mixture during second stage of the research, i.e. once all
such phases as a-C2SH or truscotite causing the deterioration of the curing parameters at elevated temperature were established.
mechanical properties of cementitious materials [11]. There is a According to [20,21], in order to ensure the highest packing
very wide range of RPC autoclaving parameters used. Target tem- density for dry composite ingredients when choosing micro-
perature varies from 160 up to 400 C, while treatment at 400 C aggregate proportions the optimum grain size distribution curve
is performed outside the autoclave, causing an increase in pressure proposed by Funk and Dinger was applied [22]. As the result of
inside the material characterized of very tight structure. However, analysis carried out quartz sand was mixed with quartz powder
holding time reported in the literature varies between 8 and 24 h at the ratio of 30/70%. Detailed information on chemical, physical
[8,12,19]. and mechanical properties of all grained components is shown in
So far many studies pertaining mechanical properties of RPC detail in Table 1, while corresponding grain-size distribution is
cured in various hydrothermal conditions, i.e. in standard wet presented in Fig. 1. The RPC composition is specified in Table 2.
environment at 20 C, during low-pressure steaming (S) or auto-
claving (A) were carried out. It is difficult to compare material
properties described in publications due to differentiated treat- 2.2. Experimental procedures
ment parameters at elevated temperatures, and in addition these
materials are of different composition in terms of binder content Preparation of concrete mixture started from preliminary
and fibre content and length. The completed research program pre- mixing of all dry concrete components for 1.5 min, and then 75%
sented below consists in its first part in choosing the most favour- of assumed water amount was added and with an admixture intro-
able parameters of low-pressure steaming and autoclaving for RPC duced earlier mixing was continued for 1.5 min. The mixing
without fibres. In the second part of this research a comparative
study of compressive strength and material response during bend-
ing test for a material containing steel fibres, steam cured and
autoclaved with optimized parameters and a material cured in
water at 20 C for 28 days was made.

2. Experimental study

2.1. Materials

To obtain reactive powder concrete the ordinary Portland

cement (OPC) of 52.5 strength class according to EN 197-1 charac-
terized of essential properties for RPC composites, i.e. low alkaline
content, high silicate modulus exceeding 3.5 and relatively low
specific surface area was used. In addition, quartz sand of
0/0.5 mm in grain size, quartz powder (0/0.2 mm), silica fume Fig. 1. Grain-size distribution for RPC components.

Please cite this article in press as: T. Zdeb, An analysis of the steam curing and autoclaving process parameters for reactive powder concretes, Constr. Build.
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 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx 3

Table 2
Composition of RPC matrix in kg/m3.

Cement 903
Silica fume 181
Quartz powder 0/0.20 mm 312
Quartz sand 0/0.50 mm 729
Water 217
Superplasticizer 19
Water to binder ratio 0.20

process was then stopped for 2 min to ensure appropriate cement-

water contact, and finally, to add the remaining amount of water
with superplasticizer and mix it so that the entire process lasts
not longer than 8 min. In the second part of this study, where an
effect of heat treatment on efficiency of dispersed reinforcement
is verified, fibres were added one minute before the end of mixing
process at amount of 2% by volume. Such time was sufficient to
obtain an uniform fibre distribution in the mixture.
The prepared mixtures were moulded in bars of 40  40 
160 mm in size. The filled moulds were stored at a chamber (see
Fig. 2) and subject to hydrothermal treatment. Specifically for this
research designed and performed chamber had internal dimen-
sions: 110 mm in diameter and 220 mm in height which enabled
treatment of 3 hardened specimens without mould or 2 concrete
mixtures in the mould. The pressure during steaming (Tmax 6 90 C)
was 1 bar, while autoclaving (100 C 6 Tmax 6 250 C) its value was
determined by water vapour pressure at each fixed temperature
and varied from 1 to 40 bar.
Among all parameters of hydrothermal treatment (see Fig. 3)
the most significant ones were selected. Initially, an effect of preset
time t1 on RPC mechanical properties at fixed Tmax and t3 was
established. During determining the parameter t1 the highest tem-
peratures assumed for steaming (90 C) and autoclaving (250 C)
were applied. This results from the well-known relationship that
preset time should extended with increasing target temperature.
Thus, the specified time t1 will be safe also for other temperatures.
Second step was devoted to determination of an impact of target
temperature Tmax at fixed other parameters t1 and t3 on mechanical
properties of RPC. Finally, in the third step holding time t3 at t1 and
Tmax set previously was verified. During all the steps both heating
and cooling rates were controlled and fixed in all cases at 20 C/h,
as well as initial temperature Tini was 20 C. The temperature ver-
sus time curves for all cases under investigations are presented in
detail in Table 3.
Once all the parameters of steaming and autoclaving were
established, second part of the research was carried out. This time
steel fibres were incorporated to the composite in amount 2% by
Fig. 3. General temperature vs. time graph for any heat treatment process.
volume in order to compare material response during compression
and bending after steaming and autoclaving with optimized
parameters. As a reference material RPC with fibres cured in water
at 20 C for 28 days was applied.
Due to a known homogeneity of RPC composite structure, thus
also the obtained results of mechanical properties testing, each
time flexural strength was determined based on the results
obtained from 3 bars of 40  40  160 mm in size, and then after
cutting six cubes of 40  40  40 mm in size from the remaining
halves, compressive strength was determined. Generally, mechan-
ical properties after steaming were tested 48 h from forming, while
for autoclaving just after the material was cooled down to room
temperature. Mechanical properties were tested on the Zwick/
Roell Z100 and Z1600 universal testing machines, enabling
research to be continued by controlling deformation increment
over time and additionally equipped with a precise extensometer
capable to measure deflection with accuracy to 0.1 lm.
Microstructure observations were made by using the Zeiss
EVO10 M scanning microscope, while pore-size distribution with
the Quantachrome Pore Master 60 porosimeter, enabling identifi-
cation of pores of diameters within the range of 3.750.25 mm.
3. Results and discussion
3.1. Mechanical properties of RPC without fibres
3.1.1. An effect of preset time t1
Regardless of the stage of this experiment the results of
mechanical tests were of very high homogeneity. The maximum

Fig. 2. Scheme of the curing system and picture of the steel chamber and mould.

Please cite this article in press as: T. Zdeb, An analysis of the steam curing and autoclaving process parameters for reactive powder concretes, Constr. Build.
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4 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx

Table 3
Variable parameters of the steaming and autoclaving process (discussed in the text).

Stage t1 [h] t3 [h] S Tmax [C] A Tmax [C]

1 0 12 90 250
3
6
12
24
2 Most favourable t1 for S and A 12 20 100
30 130
50 160
70 180
90 220
250
3 Most favourable t1 for S and A 6 Most favourable Tmax for S and A
12
24
48

value of the coefficient of variability did not exceed 10% and 15%,
for compressive and flexural strength, respectively.
It was decided to choose the longest preset time as 24 h because
as presented in [2], longer t1 factor like 37 days do not bring about
significant changes in RPC mechanical properties. The results of
experiments presented in Fig. 4 confirm that the most favourable
RPC mechanical properties when steaming at 90 C are reached
after preset time t1 = 6 h. Both shorter and extended time cause a
reduction in compressive strength by 13% and even up to 40% for
flexural strength. For autoclaving at 250 C the effect of preset time
was negligible. Compressive strength changed by 3%, while flexural
strength by 12%, when comparing extreme values. As mentioned
above, one of the crucial factors deciding on grained composite
mechanical properties is the matrix adhesion, i.e. between C-S-H
phase and quartz micro-aggregate as an inclusion. As reported in
[11] already at a temperature about 100 C the traces of silica dis-
solution appear. In addition, a relatively slow rate of temperature
increase during heat treatment equal to 20 C/h is sufficient to pro-
duce an adequate amount of amorphous hydrated calcium silicates
(see Fig. 9). Thus one can conclude that despite the lack of preset
phase (t1 = 0 h), mechanical properties of autoclaved RPC were
not reduced. When summarizing, for steaming and autoclaving it
has been decided to apply preset time t1 = 6 h for further analysis
in this study.
3.1.2. An effect of target temperature Tmax
The improvement of strength in RPC cured at elevated temper-
ature is caused by several factors. One of the most important is an
increased pozzolanic reactivity of silica components. This applies
both to amorphous and crystalline raw materials [11,19,23].
This in turn transforms to an increased production of C-S-H,
that reduces the porosity of composites. In addition, since the

Fig. 4. Compressive strength (a) and flexural strength (b) for steamed and autoclaved materials depending on preset time t1.

Fig. 5. Compressive strength (a) and flexural strength (b) of steamed and autoclaved materials as a function of target temperature Tmax.

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 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx 5

Fig. 6. Compressive strength (a) and flexural strength (b) of steamed and autoclaved materials as a function of holding time t3.

Fig. 7. a) measuring system for recording the force deflection relationship during three point bending tests, b) representative force-deflection curves for RPC cured under
various conditions.

coefficient of thermal expansion is very close to concrete shrink-
age, a temperature increase fosters reduction of internal strains
resulting from the shrinkage [24]. This of utmost importance for
cementitious composites of a high binder content.
Both compressive strength and flexural strength were changed
linearly depending of target temperature used, that is also con-
firmed by test results obtained by [25]. The lowest compressive
strength was recorded for a material cured at 20 C and was
98 MPa, while after steaming at 90 C it increased up to 207 MPa.
Based on this linear relationship it can be computed that an
increase in steaming temperature by 10 C within the range under
consideration, causes an increase in strength by about 16 MPa. For
flexural strength the obtained values ranged from 8.4 to 13.8 MPa,
and an increase in strength per each 10 C was 0.7 MPa.
When a temperature of 100 C is exceeded during heat treat-
ment, i.e. during autoclaving, a reduced increase in these proper-
ties is observed with increasing target temperature. Although
extreme values obtained just after autoclaving, depending on tem-
perature were 187 MPa and even 252 MPa for the lowest (100 C)
and highest temperature (250 C), correspondingly, for each 10 C
an increase in strength is only 4.3 MPa. Thus, an increase in target
temperature during autoclaving causes its continuous and practi-
cally linear increase, but it is almost four times lower in compar-
ison to steaming. Similar phenomenon was observed also for
flexural strength. For extreme temperatures it varies between
12.3 and 19.1 MPa. In this case the strength increase rate compared
to low-pressure steaming was almost two times lower per each
10 C and was 0.5 MPa (see Fig. 5). Regardless of possible crystal-
lization of a-C2SH, stable at 180 C, no reduction in RPC composite
mechanical parameters was observed. The presence of pozzolana
at amount of 20% per cement weight reduces the probability of
occurrence of this compound. EDS point analysis indicated that
the average value of CaO/SiO2 is about 1.2. Thus, it should be
assumed that in autoclaved RPC, among many possible crystalline
forms of hydrated calcium silicates [17,18], most often tobermorite
(C5S6H5) and xonotlite (C6S6H) will be found, having an advanta-
geous effect on material mechanical properties [3,26].
When summarizing, both for RPC steaming and autoclaving the
best mechanical properties showed the materials cured at highest
temperatures. Therefore, at the next stage of this study when an

Fig. 8. Stress (a) and toughness (b) at characteristic points of force-deflection curve for RPC cured under different thermal conditions.

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6 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx

Fig. 9. RPC cured with a) steaming at Tmax = 90 C and b) autoclaving at Tmax = 250 C, without presetting (t1 = 0 h) description in the text.

appropriate holding time was established Tmax = 90 C for steaming Table 4

and Tmax = 250 C for autoclaving were adopted. Mechanical properties of RPC with steel fibres of 6 mm in length at amount of 2% by
volume, exposed to various curing conditions.

Units Water Steaming Autoclaving

3.1.3. An effect of holding time t3 20 C 90 C 250 C
Based on the results presented in Fig. 6 it should be thought that fcm rmax MPa 178 212 265
holding time above 12 h during steaming brings no essential LOP fLOP MPa 20.5 20.5 24.5
advantages in improving RPC strength. A weak tendency to dLOP mm 0.068 0.061 0.138
increase compressive strength observed also by [25], when holding TLOP N
m 0.142 0.155 0.626
between 12 and 48 h was only 4%. However, flexural strength rose MOR fMOR MPa 15.5 24.7 27.3
by 16%. dMOR mm 0.129 0.160 0.187
Similarly to steaming, during autoclaving holding time ranging TMOR N
m 0.530 0.922 1.076
from 12 to 48 h brought no essential changes in composite d5 fd5 MPa 15.6 24.6 20.8
mechanical properties. Although compressive strength increased dd5 mm 0.206 0.180 0.408
Td5 N
m 0.974 1.104 2.966
slightly after 24 h by 5%, holding time t3 extended to 48 h caused
even a drop of compressive strength by 7%. Flexural strength d10 fd10 MPa 14.0 22.1 13.8
dd10 mm 0.381 0.337 0.762
remained almost unchanged at a level of 19 MPa within the entire
Td10 N
m 1.926 2.432 5.148
range of t3. Similar tendency to reduce compressive strength after
d20 fd20 MPa 9.2 16.9 5.0
too long holding time was observed by [3]. This effect is connected
dd20 mm 0.723 0.635 1.447
with the conversion of C-S-H amorphous phase of large specific Td20 N
m 3.315 4.482 5.148
surface into crystalline forms of hydrated calcium silicates show-
L/600 fL/600 MPa 16.0 24.6 26.4
ing a lowered adhesion to quartz crystals. In addition, hydrated cal- dL/600 mm 0.200 0.200 0.200
cium silicates undergo partial dehydration at 250 C, that also can TL/600 N
m 1.090 1.415 1.343
participate in increasing material porosity, and in consequence in L/150 fL/150 MPa 8.2 14.9 13.0
decreasing its strength. dL/150 mm 0.800 0.800 0.800
TL/150 N
m 3.553 5.410 5.390

3.2. Mechanical properties of RPC with fibres

Mechanical properties were determined after heat treatment at
the best parameters set for steaming: t1 = 6 h, Tmax = 90 C, t3 = 12 h
and autoclaving: t1 = 6 h, Tmax = 250 C, t3 = 6 h. The results were
compared to those of a material which was water cured at 20 C
for 28 days. Besides of principal properties, i.e. compressive
strength (fc) and flexural strength (ff),the parameters related to
composite deformation during bending test based on the recorded
force-deflection curve like as in [27] according to standards [28,29]
were determined. Thus such parameters as residual strength (f),
deflection (d), and toughness (T) were determined for characteris-
tic points of the forcedeflection curve. The following characteris-
tic points describing the deformation of material with fibres were
determined: LOP (limit of proportionality assigned to first crack
of the matrix), MOR (modulus of rapture assigned to the point
when material softening is observed after LOP), and deflections
L/600, L/150, d5 = 3dLOP, d10 = 5.5dLOP, d20 = 10.5dLOP. The testing
machine with the tested sample is shown in Fig. 7a, while typical
force-deflections curves are presented in Fig. 7b. The computed
averaged mechanical parameters are listed in Table 4.
The results obtained both in compression and flexural bending
tests revealed an advantageous effect of heat treatment. Compres-
sive strength is higher by 20% and more than 40% compared to a
water cured material for steaming and autoclaving, respectively.
When 6 mm long steel fibres at amount of 2% by volume were
used, no significant effect on compressive strength was recorded.
The improvement in this feature was below its natural variability.
For flexural strength both heat treatment and the presence of fibres
enhanced this feature. Steaming increased flexural strength by
20%, while autoclaving by more than 30% compared to 28-day
strength of a material with fibres cured in water at 20 C. Thus,
the obtained results do not confirm a reverse tendency to weaken-
ing fibre adhesion to the matrix described by [26]. In turn, the
introducing a dispersed reinforcement into a steamed material
increased this strength by 80%, and by 40% in autoclaved material.
With increasing temperature the values of stress fLOP and
deflection dLOP increase. This indicates both an increase in matrix
strength as well as better collaboration with dispersed reinforce-
ment before first crack occurs. Then, energy to be provided to crack

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 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx
matrix TLOP, compared to that of water cured material, is by 10%
higher for steaming, and even more than four times higher for
autoclaving.
A very interesting relationship between stresses at points LOP
and MOR was observed (see Fig. 8). In both cases of curing at ele-
vated temperature, i.e. steaming and autoclaving, the value of
stress fMOR is higher than fLOP. This means that the same amount
of fibres like in a water cured material can carry higher loads,
undoubtedly due to higher adhesion to the matrix. This is also
reflected in values of TMOR.
The coefficients fd5, fd10, fd20, and fL/150 characterise residual
material strength at higher beam deflections, as they are relatively
low at autoclaved material. This can be probably explained by the
fact that during such heat treatment the material becomes more
brittle. Thus, fibres stretched during bending cause larger damage
to the matrix, while weakening anchoring of still active fibres.
However, the value of toughness obtained for relative points d5,
d10, d20, increases after heat treatment, especially autoclaving,
due to variable values of dLOP, with respect to which these coeffi-
cient are computed. An analysis of toughness at absolute deflection
of the beam, i.e. L/600 = 0.2 mm and L/150 = 0.8 mm shows that
heat treatment increases also energy required to reach an adequate
deflection, compared to a water cured material. However, when
comparing TL/600 and TL/150, assigned to materials subjected to
steaming and autoclaving, one can say, that they are very close.
3.3. Microstructure of tested RPCs
All concretes made with reactive powders cured under appro-
priately controlled steaming and autoclaving conditions are char-
acterised of better mechanical parameters. This can be explained,
inter alia, by increased pozzolanic activity of inert composite
Fig. 10. Microstructure of RPC autoclaved at: a) Tmax = 130 C, b) Tmax = 160 C, c) Tmax = 180 C, d) Tmax = 250 C description in the text.
Please cite this article in press as: T. Zdeb, An analysis of the steam curing and autoclaving process parameters for reactive powder concretes, Constr. Build.
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7
components, i.e. crystalline silica [23]. As shown in Fig. 9b a quartz
grain was partially dissolved, thus a topochemical reaction
between SiO2 and Ca(OH)2 is observed, thus improving inclusion-
matrix adhesion. Also the presence of alkaline ions coming from
cement will have a great effect on destruction of the silica crystal
lattice [6], while increasing the matrix-inclusion contact surface
area. The observed values of compressive strength as well as ten-
sile strength, especially for autoclaved materials are very high
and exceed even 250 MPa and 20 MPa, correspondingly.
An effect of individual heat treatment parameters can be
observed in microstructural photos presented below. Preset time
t1, was found to be significant for steamed composites. Too short
preset time causes that the amount of chemically bonded water
is very small, and a temperature rise entails free water removal.
Microstructure of such materials is distinguished by a lot of short
cracks that reduce mechanical properties and durability deteriora-
tion (see Fig. 9a). For autoclaving this effect was not observed (see
Fig 9b). A relatively slow temperature increase rate of 20 C/h was
sufficient to create an appropriate amount of C-S-H amorphous
phase of very high specific surface area showing a very good adhe-
sion to quartz micro-aggregate. Moreover, when holding the mate-
rial at Tmax = 250 C, the structure was sealed with additional
amount of C-S-H phase due to increased pozzolanic activity of sil-
ica ingredients and deposition of crystalline hydrated calcium sili-
cates in material defects, i.e. in cracks and pores.
The image of pores in RPC autoclaved at lower temperatures
partially filled with crystals, mainly tobermorite, and at higher
temperatures, i.e. above 180 C, where phases of both tobermorite
and xonotlite appeared, is presented in Fig. 10. These observations
allow us to conclude that with increasing temperature Tmax the
length of whiskers of deposited hydrated calcium silicates also
increases. While at a temperature of 130 C no crystals were
8 T. Zdeb / Construction and Building Materials xxx (2016) xxxxxx
Fig. 11. Distribution of pores in RPC cured in water at Tmax = 20 C, steamed at
Tmax = 90 C and autoclaved at Tmax = 250 C.
observed, its length was about 7 lm at 160 C. Further temperature
rise to 180 C lengthened them to 17 lm, while in the range from
220 C to 250 C the measured length was practically the same
(approx. 20 lm). It should be also added that holding time t3 was
identical in all cases described above and was fixed at 12 h. No
effect of parameter t3, within the range of 6 h to 48 h on qualitative
changes in microstructure of steamed and autoclaved materials
was observed.
The porosimetry measurements revealed that during steaming
at 90 C the total porosity remains practically unchanged (see
Fig. 11) compared to porosity of RPC cured in water for 28 days.
However, an advantageous effect of steaming is visible by reduc-
tion in macropores of size above 100 nm. In steamed concretes a
tendency to increased amount of capillary and gel pores in the
range of 3.7 nm to 100 nm compared to those naturally cured is
visible. After autoclaving a reduced porosity both macropores, cap-
illary as well as gel pores are detected. This probably results not
only from an increase in pozzolanic activity of ingredients, but also
tobermorite and xonotlite crystals appearing in material voids. The
total porosity of autoclaved material compared to a naturally cured
concrete was reduced by approx. 20%.
4. Conclusions
An analysis of an influence of steaming and autoclaving param-
eters on the selected properties of RPC allowed their more favour-
able values to be established.
 For steaming preset time plays an important role and should be
verified depending on binder used due to different setting
times. In the case of cement used in this study, time t1 should
be 6 h. For autoclaving this parameter was insignificant for
mechanical properties, however for practical reasons it seems
that a possibility of autoclaving after demoulding is a significant
facilitation, thus time t1 before ramp time may be related to bin-
der setting time.
 Both for steaming and autoclaving temperature Tmax has a sig-
nificant effect on mechanical properties of RPC tested just after
heat treatment. For steaming an increase in temperature by
10 C increases compressive strength and flexural strength of
concretes without fibres by 16 MPa and 0.7 MPa, respectively
while by 4 MPa and 0.5 MPa for autoclaving. Also temperature
of heat treatment play a great role for microstructure by
increasing micro-aggregate reactivity, thus increasing also
inclusion-matrix adhesion. In addition, crystallization of
hydrated calcium silicates at a temperature of about 160 C is
Please cite this article in press as: T. Zdeb, An analysis of the steam curing and autoclaving process parameters for reactive powder concretes, Constr. Build.
Mater. (2016), http://dx.doi.org/10.1016/j.conbuildmat.2016.11.026
observed. These crystals deposit in material defects, as con-
firmed by porosity measurements. Further temperature rise
increased the length of whiskers in deposited tobermorite and
xonotlite.
 RPC holding time at the maximum temperature during steam
curing for more than 12 h brought no significant advantages
in terms of mechanical properties, while it seems that holding
time of 6 h is sufficient for autoclaving.
 The employed method of RPC curing was found to be important
not only for strength of the matrix itself, but also for behaviour
of dispersed reinforcement analysed primarily during flexural
tests. It was revealed that at a steel fibre share of 2% by volume,
after first cracking, i.e. at LOP point, a water cured material
showed only a continuous weakening with increasing deflection
of the beam. Both for steaming and autoclaving these materials
showed an increase in post-critical stresses assigned exclusively
to the interaction between the matrix and fibres.
Acknowledgments
The results and paper preparation were supported with the
funds of Cracow University of Technology within the framework
of the L1/242/2015/DS research project. The author would like also
to thank Professor Jacek Sliwinski from Cracow University of Tech-
nology for his invaluable comments to this paper.
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