PETROLEUM EXPLORATION AND DEVELOPMENT

Volume 42, Issue 1, February 2015

Online English edition of the Chinese language journal

Cite this article as: PETROL. EXPLOR. DEVELOP., 2015, 42(1): 104–111. RESEARCH PAPER

Mechanical properties of oil well cement stone reinforced

with hybrid fiber of calcium carbonate whisker and carbon
fiber
LI Ming1, LIU Meng1, YANG Yuanyi1, LI Zaoyuan2, GUO Xiaoyang2,*
1. School of Material Science and Engineering, Southwest Petroleum University, Chengdu 610500, China;
2. State Key Laboratory of Oil and Gas Reservoir Geology and Exploitation (Southwest Petroleum University), Chengdu 610500, China

Abstract: To decrease the brittleness of oil well cement stone, the effects of carbon fiber, calcium carbonate whisker and hybrid fiber of
them on mechanical prosperities of the cement stone were studied by experiments. The microstructures and micromechanical behaviors of
the cement stone were investigated using scanning electron microscopy. The strengthening and toughening mechanisms of hybrid fiber
were discussed. The experimental results show that: the compressive, flexural, split tensile strengths of the cement stone can be improved
effectively with each of carbon fiber, calcium carbonate whisker and hybrid fiber; compared with adding a single fiber, the hybrid fiber
can strengthen the cement stone better; the mechanical deformation capacity of the cement stone added the hybrid fiber is significantly
improved, and the cement stone shows obvious toughness. Observing the microstructures and micromechanical behaviors of the cement
stone and analyzing the reinforcement mechanism of hybrid fiber reveal that, the calcium carbonate whisker and carbon fiber have dif-
ferent sizes, morphologies and performances, which can work in different structure levels and loading stages, controlling generation and
development of microcracks and fractures and improving the strength and toughness of the cement stone.

Key words: oil well cement stone; carbon fiber; calcium carbonate whisker; mechanical properties; well cementing

Introduction its poor dispersion in cement slurry can be solved[9]. Calcium

carbonate whisker, a kind of single crystal in whisker shape
After cementing, the cement slurry would cure into cement
much shorter than short fiber, has both the characteristics of
sheath which is required to provide effective zonal isolation,
mineral powder and fibers, and good compatibility with ce-
and protection and support for casing. Long-term cement
ment-based materials, so it is an ideal reinforcing material[10]
sheath integrity is of vital importance for the following drill-
yet to be tried in cement slurry. This study was to evaluate the
ing and oil and gas production[1−2]. Considering the brittle
effect of carbon fiber, calcium carbonate whisker and hybrid
nature of cement based-materials, the operations performed
fiber on the microstructure and mechanical properties of ce-
after cementation such as perforation, fracturing, and produc-
ment stone, and their mechanisms of improving toughness.
tion operations and complex formation stresses on cement
sheath can damage its integrity and bond with the casing or 1 Experimental materials and methods
formation, resulting in the loss of zonal isolation and sus-
1.1 Materials and setup
tained casing pressure adverse to oil and gas production[3−5].
Some studies abroad show that fiber can improve the me- Experimental materials include: G grade oil well cement
chanical properties of cement-based material[6]. Polyester fiber, (Jiahua Cement, Sichuan); dispersants, fluid loss additive,
polypropylene fiber, carbon fiber and various organic fibers sodium carboxymethyl cellulose (Kelong Chemical Co., Ltd.,
currently used in oil industry can improve the toughness of Chengdu); defoamer (Chuan Feng Chemical Co., Ltd,
cement stone to some extent, but they have such disadvan- Chengdu); carbon fiber (Xingke of Carbon Fiber Company,
tages as poor dispersion, poor durability, and high cost[7−8]. As Dalian); calcium carbonate whisker (Runxing Chemical Co.,
a kind of fiber with high strength and high elastic modulus, Ltd, Laizhou). Carbon fiber is columnar and calcium carbon-
carbon fiber will toughen oil well cement stone significantly if ate whisker is a needle-like crystal of aragonite-type, their

Received date: 10 Feb. 2014; Revised date: 16 Oct. 2014.

* Corresponding author. E-mail: [email protected]
Foundation item: Supported by the Open Fund of State Key Laboratory of Oil and Gas Reservoir Geology and Exploitation（Southwest Petroleum University）
(PLN1213); National Key Basic Research and Development Program (973 Program), China (2013CB228003).
Copyright © 2015, Research Institute of Petroleum Exploration and Development, PetroChina. Published by Elsevier BV. All rights reserved.
 LI Ming et al. / Petroleum Exploration and Development, 2015, 42(1): 104–111

Table 1 Characteristics of carbon fiber and calcium carbonate whisker

Item Length/μm Diameter/μm Tensile strength/MPa Density/(g·cm−3) Elastic modulus/GPa pH
Carbon fiber 700−1 400 8−20 >3 300 1.76 >220
Calcium carbonate Theoretical strength of
20−80 0.5−2.0 2.80 9.0−9.5
whisker Calcium carbonate crystal

basic parameters are listed in Table 1. flexural strength of cement stone. The results show that under
The experimental setup includes: an electro-hydraulic test- the same conditions flexural strength of cement stone in-
ing machine (YA-300, Haizhi Technology Development Cen- creased at first and then decreased with the increase of carbon
ter, Beijing); a pressure consistometer (OWC-9350A, Shen- fiber length, and the best length of the carbon fiber was 700−
yang Institute of Applied Technology University of Aeronau- 1 400 μm. The reason is that carbon fiber too short cannot
tics and Astronautics); a scanning electron microscope connect crack, and can’t play the role of bridging; carbon fiber
(JSM-6490LV, JEOL in Japan); an electric bending test ma- too long can’t be uniformly dispersed in slurry. Therefore,
chine (PKZ-5000, Instrument Machinery Co., Ltd, Jianyi on chopped carbon fiber 700−1 400 μm long was selected in the
Wuxi ); a tissue masher (JJ-2, Shuangjie Instrument Factory, experiment.
Jiangsu Jintan); a turbidimeter (2100Q, HACH company, Fig. 1 shows the turbidity variations of carbon fiber in
U.S.); triaxial rock mechanics testing system (RTR-1000, CMC solution of different concentrations, it can be seen from
GCTS company, U.S. ). the figure the amount of carbon fiber has a significant effect
1.2 Experimental methods on dispersion; the carbon fiber (0.1%) can disperse in solu-
tions with CMC concentration in between 0.10% and 0.20%
Referring to GB/T 19139-2012[11], according to the experi- when carbon fiber concentration is lower than 0.3%; increas-
mental requirements, slurry with carbon fiber, slurry with ing the amount of CMC can improve the dispersibility of the
calcium carbonate whisker, slurry with carbon fiber and cal- carbon fiber, but when the concentration of CMC is over
cium carbonate whisker, and blank slurry were prepared, 0.20%, the increase of CMC concentration would decrease the
cured and tested. The cement samples 50.8 mm × 50.8 mm × dispersibility of carbon fiber. Therefore, the concentration of
50.8 mm were cured at 30 °C (cement powder must be pre- the CMC solution was set at 0.20%, and carbon fiber concen-
mixed with whisker for the preparation of slurry with whisk-
tration was controlled below 0.3%, to ensure effective disper-
er). In the experiment, carboxymethyl cellulose (CMC) was
sion of carbon fiber, as well as good mobility of cement slurry
used as dispersant to disperse the carbon fiber, turbidimetry
at ambient temperature.
method was used to characterize the dispersion of chopped
The experiments show, compared with pure cement (with
carbon fibers in the dispersion solution. First, according to the
no carbon fiber and CMC), the slurry with CMC was slow in
amount of carbon fiber, water and CMC required in carbon
strength growth, because CMC has some retarding effect, so
fiber cement the different materials were weighed, then car-
about 0.2% of CMC was also added in the blank sample P1 in
bon fiber was added into different CMC solution of different
the experiment (Table 2).
concentrations and the solution was stirred by a variable speed
agitator for 30 min, finally the turbidity of the solution was
measured with a turbidimeter. For the carbon fiber solution
with the same amount of CMC, the higher turbidity means the
better dispersion[12−13].
The compressive strength of cement stone was measured
with a universal hydraulic testing machine; the flexural
strength measured with an electric bending device; the split
tensile strength was measured with the Brazilian experiment
splitting method; then referring to GB/T 50266-99 “test me-
thod standards for engineering rock”[14], stress and strain of
cement were measured with a triaxial rock mechanics testing
Fig. 1 Turbidity variations of carbon fiber in the CMC solution
system (RTR-1000 type) at a static constant speed (2 kN/min)
during cyclic loading, and confining pressure of 20 MPa; fi- Table 2 Formula of each sample of carbon fiber reinforced ce-
nally the microscopic morphology of the cement stone was ment test
observed with scanning electron microscopy.
Serial Fluid loss Dispers- Fresh Carbon
Cement/g
2 Results and discussion No. agent/g ant/g water/g fiber/g
P1 800.0 0
2.1 Impact of carbon fiber on the mechanical properties C1 799.2 0.8
of cement stone 16 6 352
C2 798.4 1.6
Bu et al[15] studied the effects of carbon fiber length on the C3 797.6 2.4

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The mechanical properties of cement with only carbon fiber stone with calcium carbonate whisker only are shown in Table
(curing temperature of 30 °C) are shown in Figs. 2-4, com- 3 and Table 4, and it can be seen that the basic engineering
pressive strength, flexural strength, and splitting tensile property of the cement slurry cannot be reached because of
strength of cement stone with carbon fiber were all lower than the sharp decrease of the mobility of the cement slurry and the
those of the sample (P1) with no carbon fiber after 1 d of cur- down trending of the compressive strength when the amount
ing, because cement hydration was low at 30 °C, carbon fiber of calcium carbonate whisker is more than 15%. Therefore, it
and cement matrix didn’t create enough binding, thus the fiber is concluded that the amount of calcium carbonate whisker
hadn’t enhanced the strength of the cement stone much. But should be less than 15%.
with curing time increased, the mechanical properties of ce- The mechanical properties of the cement stone are shown in
ment improved significantly, strength increased with the in- Fig. 5, Fig. 6 and Fig. 7, and it can be seen that the compres-
crease of carbon fiber amount; when cement curing exceeded
7 d, with the ongoing of hydration, the strength of sample C2
and C3 increased substantially, compared with the sample P1,
the compressive strength, flexural strength and splitting ten-
sile strength of sample C3 at 7 d and 28 d of curing increased
by 17.48%, 28.36%, 30.69% and 22.57%, 29.52%, 41.79%,
respectively.

2.2 The influence of calcium carbonate whisker on the

mechanical properties of cement stone
The formula and the engineering properties of the cement
Fig. 3 Flexural strength of carbon fiber reinforced cement

Fig. 2 The compressive strength of carbon fiber reinforced ce-

ment stone Fig. 4 Tensile strength of carbon fiber reinforced cement

Table 3 Formula of each cement sample with calcium carbonate whisker

Sample Cement/g Calcium carbonate whisker/g Fluid loss agent/g Dispersing agent/g Clear water/g Defoamer/g
P2 100 0 0.5
J1 95 5 0.5
J2 90 10 1.0
2 44 0.2
J3 85 15 1.5
J4 80 20 2.0
J5 75 25 2.5

Table 4 Properties of the cement samples with calcium carbonate whisker

Compressive strength at Flexural strength at Tensile strength at
Sample Density/(g·cm−3) Mobility/cm Free fluid/mL
3d/28d /MPa 3d/28d /MPa 3d/28d /MPa
P2 1.92 21.0 17.1/25.7 6.2/10.5 1.5/3.4
J1 1.89 19.5 13.5/28.4 6.6/10.2 1.5/3.8
J2 1.88 18.0 18.2/35.5 6.3/12.9 1.9/4.1
0
J3 1.87 16.5 19.1/35.4 6.1/11.9 1.7/3.9
J4 1.82 10.0 19.2/32.4 6.0/10.2 1.6/3.4
J5 1.67 6.0 18.6/29.3 5.4/8.9 1.5/3.2

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strength, flexural and splitting tensile strengths of the sample

J2, C3, M and the blank sample at different curing time
(Fig.11) shows that the hybrid fiber doesn't work much better

Fig. 5 Compressive strength of the cement stone with calcium

carbonate whisker

Fig. 8 Compressive strength of the cement stone with hybrid

fiber

Fig. 6 Flexural strength of the cement stone with calcium car-

bonate whisker

Fig. 9 Flexural strength of the cement stone with hybrid fiber

Fig. 7 Tensile strength of the cement stone with calcium car-

bonate whisker

sive, flexural, split tensile strengths of the cement stone were

improved due to the addition of the calcium carbonate
Fig. 10 Tensile strength of the cement stone with hybrid fiber
whisker and increased with the increase of curing time. Com-
pared with the sample P2 without calcium carbonate whisker,
the compressive and flexural strengths of sample J2 increased
by 38.13% and 22.86% after 28 days of curing, and the tensile
strength of sample J1, J2 and J3 increased by 13.43%, 22.39%
and 16.42%, respectively.

2.3 The influence of the hybrid fiber on the mechanical

properties of cement stone

The mechanical properties of the hybrid fiber reinforced

cement sample (M) with 0.3% of carbon fiber and 10% of
calcium carbonate whisker were tested and the results are
shown in Fig. 8, Fig. 9 and Fig. 10, and it can be seen that the
strength of cement stone increases with the increase of curing Fig. 11 Relative change rate of mechanical properties of the
time. Comparing the relative change rate of the compressive cement stone with hybrid fiber
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in reinforcing the compressive strength of cement stone than after reaching the peak, the stress declines slowly, suggesting
a single kind of fiber in the early stage, but with the ongoing good toughness. It can be seen from Fig. 13 and Fig. 14 that in
of hydration process it outperforms the others, resulting in the first stress loading cycle, cement with hybrid fiber has
remarkable improvement in flexural and splitting ten- higher plasticity than the cement with no fiber; in each stress
sile strengths of the cement stone, and the rise of rela- loading cycle, the cement with hybrid fiber has higher total
tive change rate with the increase of curing time. Thus it can strain, plastic strain and elastic strain than the cement with no
be seen that the hybrid fiber has a better effect in reinforcing fiber, indicating that hybrid fiber significantly improved the
the cement stone than a single kind of fiber. mechanical deformation capability of cement stone; after the
The triaxial stress and strain and stress cycling loading test first stress loading cycle, the stress-strain curves of both the
were conducted on sample J2, C3, M and sample P2 and the cement stone with hybrid fiber and without fiber were denser,
results were shown in Fig. 12, Fig. 13 and Fig. 14. The high- suggesting plastic deformation capacity decreased, an indica-
er the peak value of the stress-strain curve, the higher the axial tion the pores inside the cement stone was gradually com-
compressive strength, the slow decline of stress after the peak pacted.
means the cement has higher toughness, while the rapid drop
2.4 Mixing coefficient of hybrid fiber reinforced cement
of stress after the peak is the typical characteristic of
the brittleness materials. In order to analyze the hybrid fiber reinforcement on ce-
Fig. 12 shows that the cement stone with hybrid fiber has a ment stone, the strength enhancement coefficient of cement
much higher peak, indicating high compressive strength, and with fiber relative to cement without fiber is defined as[16−18]:
f
β= (1)
fm
The mixing coefficient of compressive strength of hybrid
fiber reinforced cement is defined as:
β Mc
α Mc = (2)
β Cc β Jc
Mixing coefficient of flexural strength is defined as:
β Mf
α Mf = (3)
β Cf β Jf
The mixing coefficient of split tensile strength is defined
as:
Fig. 12 Triaxial stress-strain experiment β Mt
α Mt = (4)
β Ct β Jt
When the mixing coefficient is more than 1, the mixing ef-
fect is positive, conversely, a mixing coefficient less than 1
means negative mixing effect. Table 5 lists the strength en-
hancement coefficient and mixing coefficient of sample M
and strength enhancement coefficient of sample C1 and J1, it
can be seen that hybrid fiber works much better than a single
kind of fiber in reinforcing cement strength, and shows posi-
tive mixing effect.

2.5 Microstructure analysis of cement stone

Fig. 13 Triaxial cyclic loading test of sample P2 Observation under microscopy shows that needle-like
whiskers embedded in cement paste in the cement with cal-

Table 5 Strength enhancement coefficient of sample C1, J1, M

and mixing coefficient of sample M
Coefficient C1 J1 M
βMc 1.070 1.105 1.486
βMf 1.038 1.109 1.438
βMt 1.093 1.134 1.642
αMc 1.257
αMf 1.249
αMt 1.325
Fig. 14 Triaxial cyclic loading test of sample M
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cium carbonate whisker (Fig. 15). When a crack extends to a enhancement in cement stone strength and toughness[21].
whisker, since the whisker, higher in mechanical strength, After the dispersion treatment, the carbon fiber changed
withstands the external load and bridges the opposite sides of from bundles into single threads (Figs. 18 and 19), and dis-
the crack, the crack would need to consume more power to perses in the cement paste randomly. The crack resistance due
propagate further[19−20]. Because the whisker and cement ma- to bridging and pulling out damage of carbon fiber can result
trix are different in mechanical properties and there is an in- in a wide range of slow stable crack extension before the de-
terface between them, when the shear stress acted on the struction of cement, and create a micro-fracture zone and
whisker is greater than the whisker-matrix interface bond, the crack transition zone at the tip of crack, consuming the dam-
whisker will be pulled out (Fig. 16, point A), the stripping and age energy[22].
rubbing of the whisker and matrix interface will prevent the There are some significant differences between calcium
crack propagation. When a crack extends to the area of cal- carbonate whiskers and carbon fiber in the hybrid fiber rein-
cium carbonate whisker (Fig. 17, point B), the original crack forced cement (Fig. 20). Compared with carbon fiber, the cal-
propagation direction is limited, because of the weakness of cium carbonate whiskers are smaller in size and ratio of length
whisker - cement interface, the crack will extend along the to diameter.
interface, due to the increase of crack propagation path, the
2.6 Mechanism of hybrid fiber reinforced cement stone
energy damaging cement will be consumed, leading to the
Hybrid fiber reinforced cement is different from cement
with one single kind of fiber in mechanical properties and
microstructure, which can be explained by the synergetic ef-
fect and role playing of carbon fiber and calcium carbonate
whisker. Calcium carbonate whisker and carbon fiber have
different sizes and properties, the former in micron scale has
high elastic modulus and low elongation at break, while the
latter in millimeter scale, has relatively large size and fracture
elongation than the calcium carbonate whisker, therefore hy-
brid fiber can reinforce the cement at different structure levels
and loading stages[23−24].
In the initial stage of bearing external load, the cement ma-
Fig. 15 Bridging of calcium carbonate whisker trix, subjecting to low inner stress, forms some smaller mi-

Fig. 16 Pulling out of calcium carbonate whisker Fig. 18 Bridging of carbon fiber

Fig. 17 Deflection of a cement stone crack Fig. 19 Pulling out of carbon fiber

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Fig. 20 Microstructure of hybrid fiber reinforced cement

cro-cracks, the calcium carbonate whisker with smaller size, Different in size, shape and property, calcium carbonate
special needle-like structure and good mechanical properties, whiskers and carbon fiber in hybrid fiber can reinforce the
can effectively hinder the creation of micro-cracks and delay cement stone at different levels and loading stage.
micro-crack propagation by bridging, pulling, micro-crack
deflecting, and so on[25−26]. In the course of pulling of large Nomenclature
amounts of whiskers, the energy causing micro-cracks is con-
sumed, meanwhile the stress concentration at micro-crack tip β—strength enhancement coefficient of fiber reinforced cement
is reduced, and the generation and propagation of sub-micron stone to non-reinforced cement;
cracks are slowed down, thus improving the matrix strength of ƒ—strength of fiber reinforced cement stone, MPa;
first crack. As the load increases, if the micro-cracks gradually ƒm—strength of non-reinforced cement stone, MPa;
grow into larger ones and even regional cracks, the carbon αMc, αMf, αMt—compressive strength, flexural strength, split tensile
fiber larger in size at this point plays a leading role in bridging strength mixing coefficient of hybrid fiber reinforced cement stone;
cracks and limiting the large-scale crack extension. When the βMc, βMf, βMt—compressive strength, flexural strength, split tensile
load acted on the matrix reaches the maximum value, the ce- strength reinforced factor of hybrid fiber reinforced cement stone;
ment stone begins buckling and failure, part of the carbon βCc, βCf, βCt—compressive strength, flexural strength, split tensile
fiber is pulled out due to insufficient binding of the carbon strength reinforced factor of carbon fiber reinforced cement stone;
fiber and cement matrix, and a lot of energy is consumed in βJc, βJf, βJt—compressive strength, flexural strength, split tensile
overcoming the carbon fiber and matrix interfacial friction, strength reinforced factor of calcium carbonate whisker reinforced
thus reducing the damage efficiency effectively, and giving cement stone.
the matrix some toughness against damage[27].
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