SEM and Rock Failure

Reservoir Rock Properties Laboratory

PE 3221-003 Wednesday 1:30 – 4:30

Group 5

May 03, 2017

Group Member Position Rating % Signature

Cirilo Mauricio Manager/Editor 100

Apolinario Malungo Technician 100

William Coulter Researcher 100

David Lagunes Scribe 100

Fabio Vicente Analyst 100

Academic Integrity Statement

On my honor, I affirm that I have neither given nor received any inappropriate aid on the
completion of this exercise.

Signed: (Manager) Date:

PE 3221-003 05/03/2017 SEM and Rock Failure Group 5

Abstract

SEM test was conducted in order to see the distribution of minerals in a sample. The

image captured from this test shows dispersed shale growth on grains. Moreover, thin section

images Enlighted us about the pore to grain ratio. The porosity estimate ranged from 18.7±1.0 to

28.1±1.0%.

Furthermore, a uniaxial mechanical test was conducted by loading a dry sample having

2.91 ± 0.0021 inches in length and 1.50 ±0.0016 inches in diameter in order to determine its

failure angle, calculate failure strength and static moduli. The failure angle, stress, and strain

were determined to be 17±1˚, 5799±12, and 491.2 µstrain respectively. Young’s, Bulk, and

Shear modulus, as well as Poisson’s ratio were calculated at 0.1, 0.25, 0.5, 0.75, and 0.9 of

ultimate failure strength. Their values ranged from 9.81±0.02 to 11.9±0.03 for Young’s, 3.4±0.2

to 11±3.8 for Bulk, 3.9±0.2 to 6.1±0.2 for Shear, as well as -0.06±0.03 to 0.32±0.06 for

Poisson’s ratio. As load increases, Young’s modulus increases meaning that rigidity increases.

However, compressibility decreases as rigidity increases. The normal and shear stresses at failure

plane were determined sketching Mohr’s circle, and their values were 5303 and 1621 psi

respectively.

Moreover, static moduli were not consistent in comparison to dynamic moduli mostly

because of the difference in strain amplitude and presence of cracks or holes in the sample. The

ratio of Young’s modulus to the failure stress was measured to be 2036±6, a ratio of 1000,

indicating the sample failure at low young’s modulus.

Introduction

The understanding of rock mechanics is crucial when it comes to the production of oil

and gas. Knowledge of strength anisotropy and elastic anisotropy has great practical application

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in stimulation design (Cheng, Q., 2013). The target rocks containing the hydrocarbons are under

a significant amount of pressure and like most materials, have a certain threshold before they

fail.

The Scanning Electron Microscopy (SEM) is a technique that is used to identify the

different types of specimens that a rock is composed of. Also, we can identify the sorting, pore

space, and pore size from these SEM and thin section images. These observations and results can

be used to derive reservoir parameters such as permeability and relate to geological variables

(Clelland, W. D., 1991).

All of this information becomes relevant when performing a rock failure test. As stated

before, different materials have different thresholds before they fail. Rocks are not only

composed of many specimens, they also contain pores. The pores are important because

microcracks around these pores can occur leading to fine grains damaging the equipment. Hence,

to ensure a well's production cycle as long as possible, wellbore integrity becomes very

significant and is attracting more and more attention (Li, Y. et al, 2012). There are many stresses

that a rock can go through, especially underground. However, in this particular rock failure test,

a uniaxial stress (σ11≠ σ22= σ33= 0) test was performed. This test results in the measuring of the

static elastic properties and failure strength of the rock.

Experimental Procedure

Scanning Electron Microscope (SEM)

The SEM consists of a focused ray of high-energy electrons causing a multiples signals at

the sample’s surface (Swapp 2017). These signals result from the interaction between electron

and sample, and they provide information about chemical composition, texture, shapes,

crystalline structure and minerals in the sample (Swapp 2017). Before placing the sample to the

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FEI Quanta electron microscope (Fig. 1C) equipment used in the experiment, it was completely

degreased and dried to remove any chemical contamination and water.

Rock Failure:

The NER Autolab 1500 mechanical testing system (Fig. C2) was used to perform a

uniaxial compression (σ1≠σ2=σ3) test on a dry core sandstone until failure (Ner, 2017). After

measured 10 times, the core dimensions were 2.91 ± 0.0021 inches long and 1.50 ±0.0016 inches

in diameter. The axial and lateral strains were recorded by placing a strain gauge soldered on the

core’s surface while an axial load had been applied to the core at strain rate of 10-6 sec-1.

Connected to a speaker, it was possible to listen how the core responds to the stress. After it fails,

the angle of failure was measured, and the static moduli and failure strength calculated.

Results and Discussion

Thin section images were analyzed using photo editing software to convert a color image

into a RGB stack image with pores and grains black and white. The software then calculated the

ratio of pores to grains in the edited photo. The percentages occupied by pores in the thin

sections is another method of analyzing porosity throughout the sample. Results for each

magnification are displayed in Table 1.

Image Porosity
2.5x 23.7±1.0%
2.5x White Light 22.3±1.0%
5x 20.7±1.0%
5x White Light 24.0±1.0%
10x 24.1±1.0%
10x White Light 18.7±1.0%
20x 28.1±1.0%
20x White Light 18.9±1.0%
Table 1. Porosity values based on the ratio of pores to grains in thin sections.

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SEM captured images reveal important information about the arrangement of minerals in

the sample. Fig. 3C shows dispersed shale growth on grains. The presence of dispersed shale

has huge implications for reservoir characterization because it reduces permeability and porosity

while increasing water saturation (Tiab and Donaldson 2012). Shale grains also impact the

resistivity of the sample and there are different models for predicting resistivity based on the

dispersion of shale in sample.

The sample failure angle measured horizontally was 73 ±1˚ and from axial stress

axis was 17±1˚ (Table 1B). We used the dry sample diameter to find Area (See Eq. 1A in

appendix) in order to calculate effective stresses a (Eq. 2A). The sample Failure Stress was

determined to be 5798.9 psi and this value was retrieved from the maximum strain during test

run, which was 491.2 µstrain.

The static moduli, Poisson’s ratio (υ), Young’s (E), Bulk (K), and Shear modulus (G), are

increasing as a function of applying load because the rigidity of the sample is increasing. These

moduli were determined at 10, 25, 50, 75, and 90% of failure strength using Eq. 3A, 4A, 5A and

6A. At 50% failure, their respective values were 0.25±0.06, 9.81±0.02 Mpsi, 6.5±1.5 Mpsi, and

3.9±0.2 Mpsi. (See Table 2B for values at other percentages of failure). In addition,

Compressibility factor was determined in Mpsi (Eq. 7A).

The Young’s modulus to the failure stress ratio (Eq. 8A) was measured to be 103 ,

meaning that the sample fails at a small fraction of the modulus (Table 3B).

Moreover, Fig. 4C shows the stress-strain relationship and, based on the figure, the axial

strain exhibits the largest increase compared to both lateral and volumetric strains. Dilatancy

begins at nearly 500 psi and when the elastic limit is reached the sample goes to a process of

plastic behavior until it fails.

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Furthermore, we used the failure angle to complete the Mohr’s circle, and measure both

the normal and shear stresses on the failure plane. Fig. 1 shows the normal stresses of 495.7 psi

in y-direction and 5303 psi in x-direction as well as a shear stress of 1621 psi at 17˚ failure angle.

Fig. 1 Mohr’s Circle of Stress and measured angle.

Compared to static moduli, the dynamic moduli are smaller (See Table 4B). However,

the differences between Young’s and Shear moduli are decreasing as effective stresses increase

due to pore closure. For the static measurement, both Young’s modulus and Poisson’s ratio

oscillates as stress increases, but overall Young’s modulus increase.

Summary and Conclusions

Using SEM, we were able to see the shale growth in the minerals, as well as the

mineralogy distribution itself. Thin section images gave us insights on the ratio between pore

size to the grain size, and the estimate of porosity. Using uniaxial compression test, Static moduli

were estimated and compared with previously calculated dynamic moduli. Young’s modulus is

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PE 3221-003 05/03/2017 SEM and Rock Failure Group 5

an indicator of rock’s stiffness. The average of the estimated Young’s modulus (9.81±0.02 to

11.9±0.02 Mpsi) during this test is a proof that we dealt with a hard sandstone. Poisson’s ratio

provides an acceptable prediction of formation strength. Its values ranges from -0.06±0.03 to

0.32±0.06 on this experiment. The failure angle of 17±1˚ provided normal and shear stresses of

5303 and 1620 psi respectively. However, these values are not defined since this was only an

attempt in calculations. More trials need to be performed in order to provide accurate results.

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References

Cheng, Q., Sondergeld, C., and Rai, C., 2013 "Experimental study of rock strength anisotropy

and elastic modulus anisotropy." SEG Technical Program Expanded Abstracts 2013,

2013. doi:10.1190/segam2013-1349.1.

Clelland, W.d., and Fens, T. W. 1991. "Automated Rock Characterization With SEM/Image-

Analysis Techniques." SPE Formation Evaluation 6, no. 04 (1991): 437-43.

doi:10.2118/20920-pa.

Li, Y. Yuan, J. Qi, F. et al., 2012. "Analysis of Cemented Casing Mechanical Failure under

Arbitrary in-situ Stress Field Coupling Effects of Downhole Pressure and Temperature."

IADC/SPE Asia Pacific Drilling Technology Conference and Exhibition, January 2012.

doi:10.2118/155895-ms.

Ner, 2017. AutoLab 1500. New England Research, Inc.

http://www.ner.com/site/systems/autolab-series/autolab-1500.html (Accessed: 01 May

2017).

Swapp S., 2017. Scanning Electron Microscopy (SEM). Integrating Research and Education.

April 10, 2017.

http://serc.carleton.edu/research_education/geochemsheets/techniques/SEM.html.

Tiab, D. and E. C. Donaldson, 2012, 3rd edition, Petrophysics, Gulf Professional Publishing,

Houston, TX, 262 pp.

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Appendix A- Equations

Eq. 1A- Area

𝜋
𝐴𝑟𝑒𝑎 = 4 (d2)

Eq. 2A- Effective Stress

𝐴𝑥𝑖𝑎𝑙 𝐿𝑜𝑎𝑑 𝑃
𝜎= =
𝐴𝑟𝑒𝑎 𝐴

Eq. 3A- Poisson’s Ratio

𝜀𝑟𝑎𝑑𝑖𝑎𝑙
𝑣= (𝐿𝑖𝑛𝑒𝑠𝑡)
𝜀𝑎𝑥𝑖𝑎𝑙

Eq. 4A- Young’s Modulus

𝜎
𝐸= (𝐿𝑖𝑛𝑒𝑠𝑡)
𝜀

Eq. 5A- Bulk Modulus

𝐸
𝐾=
3(1 − 2𝑣)

Eq. 6A- Shear Modulus

𝐸
𝐺=
(2 + 2𝑣)

Eq. 7A- Compressibility

1
𝛽𝑜 =
𝐾

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Eq. 8A- Ratio of Young’s Modulus and Failure Stress

𝐸
𝜎𝑓

Eq. A9- Error

𝐸𝑟𝑟𝑜𝑟 = √(𝐴𝑒𝑟𝑟𝑜𝑟 𝜕𝐴)2 + (𝐵𝑒𝑟𝑟𝑜𝑟 𝜕𝐵)2

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Appendix B-Tables

Number of Diameter Failure angle from Failure angle from

trials Length (in) (in) Area (in^2) horizontal axial stress axis
1 2.909±0.002 1.498±0.002 1.763±0.004 72±1 18±1
2 2.91±0.002 1.496±0.002 1.759±0.004 71±1 19±1
3 2.903±0.002 1.496±0.002 1.759±0.004 73±1 17±1
4 2.909±0.002 1.497±0.002 1.76±0.004 72±1 18±1
5 2.908±0.002 1.497±0.002 1.761±0.004 72±1 18±1
6 2.906±0.002 1.5±0.002 1.766±0.004 74±1 16±1
7 2.907±0.002 1.497±0.002 1.761±0.004 74±1 16±1
8 2.909±0.002 1.501±0.002 1.77±0.004 72±1 18±1
9 2.91±0.002 1.496±0.002 1.759±0.004 72±1 18±1
10 2.908±0.002 1.498±0.002 1.762±0.004 73±1 17±1
Average 2.908±0.002 1.498±0.002 1.762±0.004 73±1 17±1
Table 1B. Area and Failure Angle.

Stress Effective Poisson's Young's Bulk Modulus Shear Modulus Compressibility

Level Stress ratio Modulus (Mpsi) (Mpsi) ((Mpsi)^-1)
(%) (psi) (Mpsi)
10 568±1 -0.06±0.03 11.4±0.02
3.4±0.2 6.1±0.2 0.3±0.01
25 1466±3 0.27±0.08 9.88±0.02 7.2±2.4 3.9±0.2 0.14±0.05
50 2916±6 0.25±0.06 9.81±0.02 6.5±1.5 3.9±0.2 0.15±0.03
75 4303±9 0.23±0.04 11.9±0.02 7.3±1 4.8±0.1 0.14±0.02
90 5209±1 0.32±0.06 11.9±0.03 11±3.8 4.5±0.2 0.09±0.03
Table 2B. Static Moduli measurements, Poisson’s Ratio and Compressibility and their
errors.

Young's
Stress Level Effective Stress Modulos
(%) (psi) (Mpsi) E/𝜎f
10 568±1 11.4±0.02 20028±59
25 1466±3 9.88±0.02 6743±20
50 2916±6 9.81±0.02 3366±10
75 4303±9 11.9±0.02 2755±8
90 5209±11 11.9±0.03 2298±7
100 5799±12 11.81±0.02 2036±6
Table 3B. Ratio between Young’s Modulus and Failure Stress

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Vertical Confining Poisson's ratio Young's Shear Bulk Modulus

sample Pressure (Psi) Modulus Modulus (Mpsi)
(Mpsi) (Mpsi)
508 0.15±0.02 2.64±0.02 1.15±0.01 1.24±0.04
1011 0.07±0.02 3.2±0.2 1.4±0.09 1.5±0.2
1512 0.11±0.02 4.1±0.2 1.88±0.06 1.6±0.3
2012 0.15±0.04 4.2±0.1 2.13±0.06 1.33±0.1
3015 0.12±0.02 4.5±0.2 2.22±0.02 1.6±0.2
5020 0.11±0.03 5.0±0.2 2.47±0.07 1.7±0.2
Table 4B. Dynamic moduli from P and S velocities lab.

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Appendix C- Figures

Fig 1C - FEI Environment Scanning Electron Microscope (ESEM). Images from this

equipment provide information about minerals composition and abundance, shapes and

crystalline structure.

Fig. 2C - Mechanical loading frame of the NER Autolab 1500 used to determine static

elastic moduli and uniaxial failure.

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Fig 3C - SEM Sample mineralogy

6000 Stress Vs Strain

5500
5000
4500
4000
3500
Axial Stress (Psi)

3000 Axial Strain

2500 Volumetric Strain
2000 Lateral Strain
1500
1000
500
0
-200 -100 0 100 200 300 400 500 600
Strain (µm)

Fig. 4C- Relationship between stress and strain. The slope of the axial stress-strain is the

young’s modulus. The ratio of the negative lateral strain is the poisson’s ratio.

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Stress Vs Youngs Modulus

6000
5000
Effective Stress (psi)

4000
3000
2000
1000
0
0 5 10 15
Young's Modulus (Mpsi)

Fig. 5C- Static young’s modulus vs effective stress.

Stress Vs Poisson's Ratio

6000
Effective Stress (psi)

4000

2000

0
-0.1 0 0.1 0.2 0.3 0.4

Poisson's ratio

Fig. 6C- Static Poisson’s ratio and effective stress relationship

Vertical Poisson's Ratio VS Conf.

Pressure
6000
5000
4000
3000
2000
1000
0
0 0.05 0.1 0.15 0.2

Fig. 7C- Dynamic Poisson’s ratio vs Confining Pressure. Values taken from the velocity lab.

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Vertical Youngs' Modulus VS Conf.

Pressure
6000
5000
4000
3000
2000
1000
0
0 1 2 3 4 5 6

Fig. 8C- Dynamic Young’s modulus and Conf. Pressure relationship. It shows a direct

relationship. As pressure increases, Young’s modulus increases.

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