BRAZILIAN JOURNAL OF PETROLEUM AND GAS | v. 6 n. 3 | p.

105-113 | 2012 | ISSN 1982-0593

CEMENT SLURRIES OF OIL WELLS UNDER HIGH TEMPERATURE AND

PRESSURE: THE EFFECTS OF THE USE OF CERAMIC WASTE AND SILICA
FLOUR

a a a b c b
Souza, P. P. 1; Soares, R. A.; Anjos, M. A.; Freitas, J. O.; Martinelli, A. E.; Melo, D. F.

a
Universidade Federal do Rio Grande do Norte, Cement Laboratory, Rio Grande do Norte, Brazil
b
Universidade Federal do Rio Grande do Norte, Chemistry Institute, Rio Grande do Norte, Brazil
c
Universidade Federal do Rio Grande do Norte, Department of Materials Engineering, Rio Grande do Norte, Brazil

ABSTRACT
This study evaluates the behavior of a ceramic waste material in partial and total substitution of a mineral
additive, commonly used in oil well cement slurries, when exposed to high temperatures and pressures.
The samples were submitted to a cycle of low temperature (38°C) for 28 days, followed by exposure to
280ºC and 6.5MPa (1000 psi) for 3 days. The evaluation was made by compression testing and X-ray
diffraction (XRD). The results showed that cement pastes containing ceramic waste, when combined with
silica flour, produced hydrated products of low Ca/Si ratios which maintained the compressive strength at
satisfactory levels.

KEYWORDS
ceramic waste; silica flour; high temperature; high pressure; strength retrogression

1
To whom all correspondence should be addressed.
Address: Universidade Federal do Rio Grande do Norte, Instituto de Química, Laboratório de Cimentos, Campus Universitário –
Natal - Rio Grande do Norte - Brazil - CEP 59072-970
Telephone: +55 84 8718-2725 | E-mail: pdpsouza@hotmail.com
doi:10.5419/bjpg2012-0009

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1. INTRODUCTION smaller amount of Gyrolite, promoting little

changes in cement strength (Nelson, 1990).
Due to the high viscosity of heavy oils it is
necessary to use special techniques to boost the oil The silica used as a mineral additive in
from the reservoir and bring it to the surface. cementitious products can be originated from
Among the techniques for recovering heavy oil, the several sources such as microsilica, also called or
methods that promote thermal heating of the silica fume, a very finely spheres of non-crystalline
reservoir receive special emphasis for its properties silica, a byproduct of electric furnaces used for
of reducing oil viscosity, thus facilitating its obtaining silicon and silicon alloys (Taylor, 1990);
removal. Steam injection is one of the most used fly ashes, ashes separated from the flue gas of a
thermal recovering techniques because of its high power station burning pulverized coal with the
technology, which yield high recovery factors chemical composition depending on the minerals
(Queiroz et al., 2005). associated with the coal (Taylor, 1990);
metakaolin, a high reactivity metastable phase
However, when subjected to high temperatures originated from the calcination of the mineral
and pressures, the physical and chemical behavior kaolinite at 700-800 oC used as a pozzolanic
of Portland-based cement changes significantly. If material (Shvarzman et al., 2003). There are also
the materials are not handled properly during the many researches indicating the possibility of using
formulation stage, they can lose mechanical other sources of silica for cement-based products
strength and increase permeability. These changes such as rice husk ash (Jauberthie et al., 2000),
may lead to isolation loss and, consequently, sugar cane biomass ash (Aigbodion et al., 2010),
provide a high risk to the continuation of activities ceramic roof tile wastes (Lavat et al., 2009), natural
(Griffith et al., 2004). zeolite tuffs (Snellings et al., 2010) and cracking
catalyst fluid (Paya et al., 2003).
The calcium silicate hydrate (C-S-H) is the main
phase, formed during the Portland cement Currently, the only material used to prevent or
hydration. It is the primary responsible for the reduce harmful reactions caused by high
mechanical strength of the hardened cement and temperatures is silica flour, a commercial additive
the excellent physical and chemical stability at made of finely divided SiO2. The use of alternative
temperatures up to 110 oC. At higher sources of silica in place of commercial additives
temperatures, there is a formation of high proves to be very attractive from both economic
calcium/silicon (Ca/Si) ratio crystalline silicate and environmental standpoints. From an economic
hydrates, such as C3S-H1.5 (C3S hydrate or Jaffeite) point of view, these materials have low added
and C2S-H (α-C2S hydrate). These hydrates are value, which would reduce production costs. From
deleterious to the mechanical properties of the an as the environmental perspective it would be
resulting slurry (Jupe et al., 2007). This able of promoting the recovery and recycling of
phenomenon is known as cement strength waste material, representing the most attractive
retrogression (Nelson, 1990). solution for problems of treatment and final
disposal (Menezes et al., 2009). This study
Nevertheless, studies (Anjos et al., 2011; Eilers evaluated the effects of the use of silica flour and a
and Root, 1976; Herianto and Fathaddin, 2005; ceramic waste in the chemical and physical
Rogers et al., 2006) show that cement strength behaviors of cement slurries subjected to high
retrogression can be avoided by adding 30-40% of temperatures and pressures.
silica based-materials to the mixture. This quantity
of silica is sufficient to consume large amounts of
calcium hydroxide and reduce the Ca/Si ratio of C-
S-H phases from 1.5 to 1.0. In the presence of silica 2. EXPERIMENTAL PROCEDURES
and at a temperature of about 110 oC, a phase
known as Tobermorite is formed in lieu of the high 2.1 Materials
Ca/Si ratio phases, preserving the mixture’s
mechanical strength and permeability properties. The cement slurries were produced using a
Increasing the temperature to about 150 oC, Portland cement with similar proprieties to the
Tobermorite usually produces Xonotlite and a class G cement used in oil-well’s cementation. The
ceramic waste used was generated during a surface

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Table 1. Chemical composition of the mineral additives (Wt.%).

Composition Silica flour Ceramic Waste

SiO2 95.70 62.01
Al2O3 2.00 21.77
Fe2O3 0.20 0.75
CaO - 1.18
MgO - 7.16
SO3 1.80 2.12
Na2O - -
K2O - 4.07

polishing process. This process provides desirable The silica flour selected is a commercial product
properties such as waterproofness, cleanability, commonly used for cementing operations in high-
stain resistance, mechanical strength and abrasion temperature oil wells. The chemical properties of
resistance to a certain class of ceramic tile, along those materials were determined or estimated by
with an improved aesthetic appeal (Kummer et al., energy-dispersive X-ray fluorescence (XRF) as
2007). During this process, the ceramic’s body is shown in Table 1.
reduced up to 90% of its original mass (Wiggers et
al., 2007). A single Brazilian company is responsible The high concentration of silicon in the ceramic
for about 30 tons of waste daily, which is disposed waste, 62.01%, is essential for such application,
entirely in landfills (Souza, 2007). The product since to form low Ca/Si ratio phases in the cement
produced is incorporated into the water to assist in it is necessary to add materials with high
the polishing process. Subsequently, the residue is concentration of this element. A high
submitted to a physiochemical treatment for its concentration of aluminum, 21.77%, can lead to
removal, and the treated water returns to the additional improvements. The conversion of
process. The waste will remain in the storage yard Tobermorite into Xonotlite that occurs around
until reaching its final destination (Souza, 2007). 150oC in cement slurries with silica-based materials
The material used in the study was collected from a can create shrinkage and cracks in the hardened
storage yard. cement, resulting in unsafe operation. However,
the presence of some aluminum atoms can replace
others of silicon in that phase, causing an
insignificant amount of shrinkage in the hardened
paste (Jupe et al., 2007).

The characterization of the phases presented by

the mineral additives is shown in Fig. 1. The figures
were fixed using the X-ray diffraction technique,
having CuKα as the radiation source, with voltage
of 30 kV and current of 30 mA. The data were
collected in the goniometer velocity of 0.02° 2θ
degree by step with counting time of 1.0 second by
step, from 10 to 80° 2θ degrees. The XRD analysis
revealed that the ceramic waste consisted in its
higher proportion of silica in the form of quartz,
and small amounts of mullite. The peaks are similar
to those of silica flour, but with lower intensities,
which represent a lower degree of crystallinity of
the waste over silica flour.

The particle size distribution of the ceramic

waste and the silica flour (Figure 2) was fixed
Figure 1. XRD of silica flour and the ceramic waste. trough a laser granulometer in liquid environment.

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The study evaluated formulations containing

only ceramic waste (CW) and others containing
blends of ceramic waste and silica flour (SF) in
different concentrations. The slurries specific
weights were fixed at 1.87 g/cm3, because it is the
most used specific weight in cementing operations
with special Portland cement (SPC). For
comparative purposes it was used a formulation
containing cement and water (RFNC), and another
with 40% silica flour (40SF), because this is the
usual concentration used for cementing operations
in high temperature oil wells. The Table 2 presents
Figure 2. Particle size distribution curves of cement the components’ concentrations and their
and mineral additives. respective masses for each formulation adopted.

The ceramic waste was the one with the lowest The cement-slurry mixtures were carried out in
average particle size, 5.13 μm, against 24.73 μm a mixer in accordance with API SPEC 10 (American
from the cement and 8.26 μm from the silica flour. Petroleum Institute, 2000-a). The experiment
The particle size distribution is a good feature molded cubic test-samples with edges of 5.0cm.
because the smaller the particle size of the mineral The samples were submitted to a hydrating process
additive, the greater will be the area available for (cure) in a thermal bath at 38oC for 28 days. This
reactions. Also, mineral additive particles do not temperature was chosen to be near to downhole
react chemically and can fill existing gaps, reducing temperatures of oil wells that use the steam
the porosity and permeability, thus increasing the injection technique for oil recovery. This technique
compressive strength of cement paste (Mehta and is used in wells up to 800m depth, approximately,
Monteiro, 1994). because to greater depths the injected steam loses
effectiveness.
2.2 Cement slurries formulation
After this step, a sample of each formulation
To determine the mass of the components of a was collected for compressive testing. Others
given oil well cement slurry, initially, the specific samples were placed in a pressurized chamber and
weight or water/cement ratio and concentration of subjected to 3 additional days of cure under high
additives solid and liquid are fixed. Then, the mass temperature (280oC) and pressure (6.5MPa). Then,
of the components is determined. The calculations the samples were tested mechanically. All samples
of the components mass were made according to were also analyzed by X-ray diffraction using CuKα
the recommendations of the API RP 10 practices radiation, a voltage of 30 kV, and a current of 30
(American Petroleum Institute, 2000-b). mA. The data collected from 10 to 60o 2θ degrees.

Table 2. Components concentrations and masses.

Content (%) Composition (g) Water/cement
Formulation
CW SF SPC Water CW SF factor (W/C)
RFNC --- --- 765.75 353.16 --- --- 0.46
40SF --- 40 560.24 337.24 --- 224.10 0.60
10CW 10 --- 705.11 343.23 70.51 --- 0.49
20CW 20 --- 653.69 334.63 130.74 --- 0.51
30CW 30 --- 609.25 327.19 182.78 --- 0.54
20CW-30SF 20 30 529.10 322.77 105.82 158.73 0.61
25CW-25SF 25 25 530.35 320.52 132.59 132.59 0.60
30CW-20SF 30 20 531.36 318.86 159.41 106.27 0.60
*CW – Ceramic Waste; SF – Silica Flour; SPC – Especial Portland Cement

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o
Figure 3. Compressive strength – 28 days, 38 C.

3. RESULTS AND DISCUSSION 34.10, and 47.12 2θ degrees) of all slurries with any
addition had lower intensities than those of the
Initially, it was verified the influence of the reference slurry. This reduction confirms the
ceramic waste and the silica flour in the samples existence of a pozzolanic reaction between calcium
just subjected to the simple cure (38oC for 28 days) hydroxide (Ca(OH)2), formed during hydration of
to serve as reference for subsequent comparison C3S and C2S phases of Portland cement and the
with patterns of those undergoing high addition rich in silica.
temperatures and pressures. Figure 3 shows the
mechanical properties of those samples. The
cement slurries that contained only ceramic waste
presented compressive strength directly
proportional to its concentration. The formulation
containing silica flour (40SF) also presented a little
increase in compressive strength. The blended
samples, ceramic waste and silica flour, showed
slight reductions when compared with the
reference formulation.

The X-ray diffractogram displayed in Figure 4

shows the reference slurry is formed by calcium
hydroxide (Portlandite), a calcium silicate hydrate,
Ettringite, and a calcium silica-aluminate hydrate
known as Gismondine. The formulations containing
ceramic waste, silica flour, and the blends of both
presented similar hydration products to the
reference sample. Differently, these formulations
had peaks of crystalline silica that did not react, as
can be seen mainly in the peaks located at 20.91 Figure 4. XRD spectra: samples cured at 28 days,
and 26.60o. This result was expected considering o
30 C. Where: P- Portlandite Ca(OH)2; E- Ettringite
that the addition used is rich in that phase. Ca6.Al2.SO4.3(OH)12.26H2O; G- Gismondine
Moreover, the Portlandite peaks (mainly 18.04, Ca.Al2.Si2.O8.4H2O; CSH- Ca1.5.SiO3.5.xH2O; SiO2 -
Silica.

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Figure 5. Compressive strength comparison between Figure 7. Compressive strength comparison

o
the samples just cured (28 days at 38 C) and those o
between the samples just cured (28 days at 38 C)
subjected to the steam injection simulation (28 days and those subjected to the steam injection
o o
at 38 C + 3 days at 280 C and 6.5MPa) – reference o o
simulation (28 days at 38 C + 3 days at 280 C and
sample and ceramic waste-doped samples. 6.5MPa) – silica flour-doped sample and blends-
doped samples.

results show that all formulations suffered strength

retrogression after subjected to the high
temperature cycle. The pastes presented strength
loss directly proportional to the amount of waste
added, reaching a loss of more than 85% for the
one containing 30% of addition, resulting in a
compressive strength of only 6.84MPa.

Formation conditions and stability of the

hydrated calcium silicates in cement pastes
submitted to high temperatures and pressures are
highly relevant to determining strength and
durability. The presence of large amounts of
Portlandite (calcium hydroxide) and calcium silicate
hydrate phases with higher than 1 Ca/Si ratio in
hydrated pastes are considered deleterious
because they lead to high permeability and low
compressive strength (Luke, 2004). The elevated
strength reduction of the reference slurry and of
those with addition of ceramic waste can be
explained by their X-ray diffractogram (Figure 6).
Figure 6. XRD spectra: samples cured for 28 days at The reference sample diffractogram shows that the
o o
38 C + 3 days at 280 C and 6.5MPa. Where: P- phases formed after the initial cure were replaced
Portlandite Ca(OH)2; R- Reinhardbraunsite by the phases Reinhardbraunsite
Ca5.(SiO4)2.(OH)2, H- Hillebrandite Ca2.(SiO3).(OH)2 (Ca5.(SiO4)2.(OH)2), Hillebrandite (Ca2.(SiO3).(OH)2),
and CSH- Ca2.SiO4.H2O. and a sort of CSH (Ca2.SiO4.H2O), which have Ca/Si
ratios of 2.5, 2.0 and 2.0, respectively. The 10CW,
20CW, and 30CW samples presented the same
The Figures 5 and 7 compare the compressive
hydration products as the reference.
strength among the samples cured and those
subjected to the steam injection simulation. The The additive used was formed by over 60% of
Figure 5 compares the reference paste with the silicon and, unexpectedly, the experiment did not
ones with addition of just ceramic waste. The observe the formation of any hydrated phase with

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The XRD spectra of the 40SF and the blended

samples are shown in Figure 8. The 40SF slurry is
formed by the phases Xonotlite (Ca6.Si6.O17.(OH)2),
Rosenhahnite (Ca3.(Si3O8.(OH)2)), and Tobermorite
(Ca5.Si6.(O, OH, F)18.5H2O), which exhibit Ca/Si ratio
of 1.0, 1.0, and 0.83, respectively. At last, the
Portlandite phase was totally consumed.

Similarly, the Portlandite of the blended slurries

was consumed. The blended slurries presented
only the phases Xonotlite and Tobermorite. The
complete consumption of Portlandite phase and
the formation of silica-rich phases are responsible
for maintaining the compressive strength of those
pastes at high levels. When the anhydrous mixture
presents relations CaO/SiO2 and CaO/(SiO + Al2O3)
equal to or lower than 1, and the hydrating
temperature is higher than 110oC, there is the
conversion of hydrate calcium silicate (little
crystalline C-S-H) to silica-rich phases as hydrate
calcium silicates, like Xonotlite and Tobermorite.
Figure 8. XRD spectra: samples cured for 28 days at These hydrate products are responsible for the
o o
38 C + 3 days at 280 C and 6.5MPa. Where: X - maintenance of compressive strength in acceptable
Xonotlite - Ca6.Si6.O17.(OH)2; T - Tobermorite - levels (Anjos et al., 2010).
Ca5.Si6.(O,OH,F)18.5H2O and R - Rosenhahnite -
Ca3.(Si3O8.(OH)2.

4. CONCLUSIONS

Ca/Si ratios equal to or lesser than 1.0 in any The ceramic waste presented characteristics of
cement paste with addition of ceramic waste. Thus, the pozzolanic material used in the characterization
the elevated Ca/Si ratio of the hydrated products by X-ray diffraction. The samples containing
formed is responsible for the drastic reduction in incremental additions of the additive, cured at 38°C
compressive strength observed after the steam for 28 days, exhibited a consumption of calcium
injection simulation. hydroxide in the presence of the additive. The
waste’s reactivity was confirmed through
Moreover, all blended pastes, ceramic waste compressive testing of the samples, which showed
and silica flour, showed low strength loss (Figure that compressive strength is directly proportional
7). Particularly, 25CW-25SF and 30CW-20SF to the presence of waste.
suffered losses of 18.75 and 25.12%, causing the
compressive strength to remain at 21.06 and All formulations suffered strength retrogression
20.06MPa, respectively. These values were after the steam injection simulation, if compared to
superior to the sample containing 40% silica flour, the post initial cure strength. The formulations with
which had a loss of 10.32% after the simulation, the addition of ceramic waste presented the
maintaining its strength at 28.25MPa. greatest losses, reaching 85%, phenomenon that
was justified by the presence of C-S-H phases with
Cement pastes used in oil wells need to present Ca/Si ratios equal to or greater than 2.0. However,
a compressive strength of at least 17 MPa. Such the formulations 25CW-25SF and 30CW-20SF, as
strength levels can bear the mechanical stresses well as the cement slurry containing 40% silica
generated in the wells. Therefore, based solely on flour, maintained the strength at satisfactory levels
the compressive strength, it is possible to classify (above 17MPa). This was justified mainly by the
the samples 25CW-25SF and 30CW-20SF with total consumption of Portlandite and the presence
having potential for use in oil wells subjected to of phases with Ca/Si ratios equal to or smaller than
thermal recovery by steam injection (Smith, 1980). 1.0.

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Through the experiments, it was possible to Griffith, J. E.; Lende, G.; Ravi, K.; Saasen, A.;
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reduction of just over 5% of cement mass, while bond strengths of geothermal well cement.
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