Chapter5

Fracturing Fluid and

Proppant Characterization
Vernon G. Constien
Dowel1 Schlumberger
5-1INTRODUCTION

Representative data on fracturing fluids and propping agents are necessary for optimum fracturing
design. Complete characterization o f a fluid and proppant system should include the following:

l rheology of clean and proppant-laden fluids,

fluid-loss rates to formation
proppant transport,
damage to proppant pack and rock matrix
compatibilities with additives, possible contaminants, and formation fluids, and physical
properties of proppants.

Although efforts have been made to develop industrywide standardized methods for characterizing
fracturing fluid performance (API RP39, 1983; Prudhomme, 1984, ,1985, 1986), generally these
efforts have not kept pace with new fluid chemistry developments. As a result, some diversity in
testing methods exists between the various laboratories. Because of the complex chemical nature
of many fracturing fluids, their physical properties are dependent on their environment of shear,
temperature, formation permeability, additives, and contaminants. It is important that the
experimental techniques which are used to determine fluid properties for design purposes
accurately reflect treatment conditions. Because the method of testing can significantly bias the
measured fluid properties, the fluid data and the method of evaluation should be considered when
selecting fluids for specific treatment applications. The information in the following sections outlines
basic principles and describes current testing methods. Examples of fracturing-fluid property data
are presented in Appendix B, and additional details on testing procedures are found in Appendix C.

5-2 RHEOLOGY

Rheology is the science of the deformation and flow of matter. For fracturing fluids, the important
variable is the apparent viscosity of the fluid as a function of shear, temperature, and time. These
relationships are commonly determined for clean fluids in a rotational concentric cylinder, a
capillary, or pipe rheometers. Because of the difficulties in evaluating the rheology of fluids
containing proppant, very little laboratory rheological testing of the proppant-laden fluids is done.

5-2.1 Basic Relationships of Flow

A brief discussion of terms and fluid models is presented. Chapter 3 contains additional details on
rheological models.

Shear in laminar flow can be thought of as a process in which infinitely thin, parallel planes slide
over each other (Fig. 5-l). Shear rate, T, is defined as the velocity difference between the planes
divided by the distance between the planes:
The usual rate of shear reported in viscometric experiments is the value at the wall of the
instrument. Shear stress, r, is the shearing force per unit area of surface:

In most measurements the shear stress is determined by measuring the torque exerted on a
measurement bob or by the pressure drop across a tube. Details of these techniques are discussed
in Appendix C.

5-2.2 Fluid Behavior

Newtonian behavior implies that fluids have a constant viscosity at all shear rates. Water, low-
viscosity oils, and gases are examples of fluids which exhibit this behavior. Fracturing fluids have
predominantly non-Newtonian behavior. This means that the apparent viscosity of the fluid is
dependent on the shear that the fluid is experiencing at the moment of interest. Fig. 5-2 illustrates
the apparent viscosity of a typical fracturing fluid over a wide range of shear. The importance of this
presentation is that a unique fluid composition may have considerably different apparent
viscosities, depending on the shear that is exerted on the fluid. This non-Newtonian behavior plays
a significant role in the friction pressure in the tubing and fractures, and in the proppant-transport
abilities of the fluid.

Rheological characterization of a non-Newtonian fluid requires that the response of the fluid to
changes in shear rate is determined and related to a model so that the apparent viscosity can be
calculated under different conditions of flow.

5-2.3 The Power Law Model

In Chapter 3, basic expressions of different fluid models were presented. The power law is the most
commonly used model to represent fracturing-fluid behavior.

where rw is the wall shear stress (lbf/fP or KPa), T is the wall shear rate (set-*), K is the consistency
index (lbf.secn/ft2 or KPa.@), and n is the flow behavior index (dimensionless).

This simple relationship holds for most fracturing fluids over the range of applicable shear rates; it
can be used to predict fluid viscosity as a function of shear rate for non-Newtonian fluids (Fig. 5-3).
As can be seen from Eq. 5-4, a log-log plot of r,+ vs f yields a straight line. The slope is equal to the
behavior index (jr); the intercept atf = 1.0 set- is equal to the consistency (K). Fracturing fluid data
are usually determined on concentric cylinder viscometers and are reported in terms of the power
law parameters II and K. The flow behavior index n is equal to n . However, K is dependent on the
geometry of the measuring device and is sometimes referred to as K,, (K is dependent on the
viscometer geometry). Savins (1958) studied the relationships between the power law fluid
equation and three specific geometries (pipe, annulus or slot, and concentric cylinder). Table 5-l
contains the correcting equations that can be used to translate properties obtained from concentric
cylinder viscometers to other geometries of interest. These equations can be used in reverse; in
other words, if data from pipe or capillary viscometers are available, they can be translated to other
geometries as well. Finally, an equation to calculate the apparent viscosity at a specific shear rate
using n and k is included.
5-3 SHEAR AND TEMPERATURE EFFECTS ON FLUID PROPERTIES

During hydraulic fracturing treatments, fluids experience wide variations in shear and temperature.
High shear is experienced by the fluid during pumping through the tubular and perforation tunnels.
Once in the fracture, the shear on the fluid is significantly less, but fluid temperature increases until
it eventually reaches formation temperature. Examples of a typical shear and temperature history
for a fluid predicted for a specific set of conditions by the KGD fracturing model (Table 5-2) are
shown in Fig. 5-4 and Fig. 5-5. The shear rate experienced by a specific volume of fluid decreases
with time. The formation temperature experienced by the fluid entering the fracture is highest at
the beginning of the treatment and decreases thereafter. As a result, the distance the fluid travels
down the fracture, before it reaches maximum temperature, increases with total fluid volume
pumped. These examples are presented to illustrate typical trends in shear and temperature
encountered by fluid. Changing treatment conditions or fracturing model can significantly change
the predicted values.

Measurement of fracturing-fluid rheological and leakoff properties under conditions which

approach realistic shear and temperature conditions can be an expensive and time consuming
problem. The extent to which field conditions must be simulated depends on the composition of
the fluid and the intended use of the data. For example, fluids which do not show time/shear effects
on their properties require less elaborate equipment and testing procedures and scaleup easier to
field conditions than fluids which have strong shear history dependence. Also, if the intent is to
study the effect of shear and temperature on the fluid and to optimize fluid composition for
maximum stability, different testing methods may be required than might be appropriate for
generating rheological data strictly for use in fracture design purposes. In actual practice, fluid
rheology data that have been generated on laboratory instruments during composition optimization
usually are reported in fluid-property data tables which are then used for fracture design purposes.
When these data are used for fluid selection and design, it becomes extremely important to
understand how the data were generated and how well they relate to field conditions.

An especially difficult problem of relating laboratory measurements to field performance occurs in

the case of aqueous crosslinked fluids. Crosslinking agents are frequently added to fracturing fluids
to enhance rheological properties. Crosslinking agents increase the effective molecular weight by
binding polymer chains, resulting in high fluid viscosities at relatively low polymer concentrations .
In nonflowing conditions, aqueous fracturing fluids can be crosslinked to such an extent that they
will retain the shape of the container in which they were prepared. However, under flowing
conditions, there are limits to the size of the three-dimensional polymer network which can be
formed. As the shear stress on the polymer network is increased, a point is reached where additional
growth is not possible because the bonding energy between polymer and crosslinker is exceeded.
For crosslinking agents, such as berates, which form reversible bonds with the polymer and which
do not rapidly deactivate with time, the structure will re-form and grow as soon as the shear

stress on the fluid is decreasedM. any other typeso f crosslinkers,

such as certain titanate or zirconate chelates, are

active for a relatively short time frame (minutes) after they

are added to the fracturing fluid. The maximum apparent

viscosity that can be obtained from fluids with a nonequilibrium

crosslinker is highly affected by the level of

shear or mixing energy which is applied to the fluid during

the time the crosslinker is active.

Becauseo f the sensitivity of the rheology of crosslinked

fluids to their shearh istory, considerablee fforts haveb een

made to better simulate typical field conditions of shear

and temperature during laboratory optimization and

characterization of these fluids. Conway et al. (1980)

demonstratedth e effect that sheard uring crosslinking can

haveo n the resultanta pparentv iscosityo f crosslinkedg uar

or HPG by subjecting fluids containing three different

crosslinkerst o constants heard uring the crosslinkingr eaction

(Fig. 5-6). Following this work, several new instrumentsa

nd techniquesw ere developedto betterd efines hear

history andt emperatiree ffectso n crosslinkedf luids (Table.

5-3).

A common theme found among these techniques is the

importance of maintaining the fluid under flowing conditions

from the time the crosslinker is added until the

test is complete. A typical test procedure involves

subjecting the fluid to a high shear environment to simulate

flow down the tubing or casing followed by a reduced

shear rate and increased temperature to simulate fracture

conditions. Crosslinkers are added to the fluid during the

high shear conditioning. The equipment for conducting

these experiments varies from small laboratory devices

(Fig. 5-7 and Fig. 5-8) to large pressurized flow loops

(Fig. 5-9). These instruments generally produce reproducible

results as long as crosslinkers are carefully metered

into the fluid under controlled shear conditions. The use

of narrow gaps or small-diameter capillary viscometers

also was found to help reproducibility (Prudhomme,

1986).

An example of shear history effects on HPG crosslinked

with titanium acetylacetonateis shown in Figure 5-10.

Gardner and Eikerts (1983) studied this fluid using a circula

ing flow loop with tubing inside diameters of 0.464

and 0.334 in. Fluid was circulated at rates to simulate flow

in 2.441~in-ID tubing at 3.3 or 9.0 BPM for various times

before flow rates were reduced to simulate a fracture shear

of 150 set-, and heating was applied to raise the fluid

temperature to 200 OF. The same fluid was studied

(Prudhomme, 1986) using the apparatus shown in Fig.

5-7 which had O.O8%n.-ID tubing to simulate tubing shear

of 675 set- for four different times before flowing into

several FANN 50 units for fracture simulations at 170

set- l and 175 OF. Although equipment and conditions

were different for these tests, both experiments showed

this fluid to be very sensitive to shear during crosslinking;

progressivelylo wer fracturev iscositiesw ere obtained

with increasing time at shear in the tubing. Similar trends

were reported by Gardner and Eikerts (1983) and Craigie

(1983) for other fast crosslinking systems.

The use of tubing shear history simulation has had a

significant impact on the chemistry of crosslinked fracturing

fluids. Fluids containingf ast-reactingo rganometallit

crosslinkers were found to undergo shear degradation

during the tubing shear simulation, resulting in lower viscosities

under fracture conditions of shear and temperature.

To reduce the amount of shear degradation, delayed

crosslinking fluids were invented. These fluids crosslink

in the fracture under conditions of lower shear, and they

produce higher final viscosities.

While the practice of laboratory evaluation of fracturing

fluids using a high shear conditioning period has led

to the development of more stable fracturing fluids, questions

have remained on the accuracy at which laboratory

rheology data on crosslinked fluids can be scaled to field

equipment and flow rates. Of particular concern are the

effects of crosslinking in large-diameter tubing and under

turbulent flow conditions.

Craigie (1983) addressedth e problem of scaleb y conducting

a large-scales imulationo f his laboratoryt est. This

experiment used 4,000 ft of 0.866-in.-diameter mbing

(Fig. 5-11). Garduer and Eikerts (1983) and Shah and Watters

(1986) added crosslinkers under turbulent flow conditions

iu closed-loopp ipe viscometers( Fig. 5-12). Results

from these experiments were reported to compare favorably

with field results.

5-3.1 Characterization Of Fluid Microstructure

Shear rheology measurements provide the power law

parameters n and K. -This information is necessary for

optimizing fluid stability and viscosity, and for predicting

laminar flow behavior in fracturing treatments. Additional

information concerning the microstructure of the

fluid is possible using dynamic oscillatory rheological

measurementsD. ynamic oscillatory measurementsm ay

be used to evaluate the viscous, linear elastic, and nonlinear

elastic (normal force) properties of polymeric fluids.

The linear elastic properties (kuown as the elastic storage

modulus aud the viscous loss modulus) are sensitive to

changes in polymer structure which may not be observed

with steadys hearm easurementsT. hesem easurementasr e

especially useful to study properties which simple, steady,

shear viscosity measurementsc annot detect. For example,

Prudhomme (1986) used dynamic oscillatory measurements

to determine that there were differences in the

extent of hydration of guar mixed by two different

methods, although their steady shear viscosity measurements

were the same. Similarly, Knoll (1985) studied the

differences in crosslink density and wall-slip tendencies

of fluids which had been dynamically mixed. Several other

studies have used dynamic mechanical testing to obtain

information on such properties as crossliriking kinetics,

and the effectso f elasticity on proppant suspensionc apabilities

and flow properties (Clark, 1979; Acharya, 1984

and 1986; Menjivar, 1984; and Prudhomme, 1985).

5-4 FOAM FFUCTURING FLUIDS

The apparent viscosities of nitrogen or carbon dioxide

foam fracturing fluids are dependent on the quality

(internal phasev ohune), texture (bubble-sized istribution),

and rheological properties of the continuous phase. The

presenceo f a separatec, ompressiblep hasem akesc haracterization

and prediction of rheological behavior for these

fluids even more difficult than single-phase fracturing

fluids. Foamsh aveb eenc haracterizedu sing severadl ifferent

rheological models, and a wide variety of experimental

methods. The majority of rheological characterizations

has been conducted on high-pressure circulating (Reidenbath

et al., 1986) or single-pass (Cawiezel and Niles,

1987; Phillips et al., 1987) viscometers.

In an extensive study of nitrogen and carboi-&oxide

base foam fracturing fluids, Reidenbach et al. (1986) developed

a model for the calculation of the rheological

properties based on foam quality (I), yield point (T&,

and liquid phase n and K.

where rYp is related to foam quality and gas composition.

The consistencyc oefficient for foam, Kkoam, was found

to be dependent on the liquid-phase consistency coefficient

(K) and quality (I) by

Some typical values for r,,, , Cl, and K' are given for

nitrogen and carbon dioxide foams in Tables 5-4 and 5-5,

respectively.

In general, foams do not thin with increasing temperature

as rapidly as single-phase fluids. Also, higher polymer

concentrationms ay not improve fluid stability asm uch

as the type and concentration of surfactant.

5-5 SLURFtY RHEOLOGY

Fluids containing proppant account from 20 % to 80 % of

the total volume of a fracturing treatment, yet very little

rheological data exist on these slurries. Determining the

rheological properties of fracturing fluids containing proppant

as a function of fluid composition, flow geometry,

temperature, time, and proppant size, density, and

instruments used to determine rheological properties of

clean fluids is unusable for these studies because their

geometriesw ill not accommodateth e large particles and

concentrations (up to 20 lb of proppant added per gallon

of fracturing fluid). Also, the proppant must be kept in

uniform suspension for the data to have meaning.

Gardner and Eikerts (1982) used a large closed-loop

pipe viscometer to study crosslinked aqueous fracturing

fluids containing proppant in laminar flow. They found

that the apparent viscosity of a crosslinked fracturing fluid

increasedu p to 230% with the additiono f six poundsp roppant

per gallon of fluid (Fig. 5-13). Their data also indicated

that the apparent viscosity at 5 11 set- of the fluid

with proppant was 2.7 tunes that predicted by Ford (1960)

for a Newtonian fluid with an equivalent proppant concentration.

I n a more extensivew ork, Shaha nd Lee (1986)

studied the relationship of friction pressure in both

laminar and turbulent flow to proppant concentration and

size in four different hydroxypropylguar (HPG) base fluids

in different pipe sizes and correlated laboratory predictions

with field measurementsS. haha nd Lees studiesi llustrate

the complexity of characterizing slurry rheology.

The friction pressure of fluids containing proppant was

found to increase significantly with increasing proppant

concentration( Pigs. 5-14 and 5-S). The predicteda mount

of friction pressure increase was strongly related to the

flow rate. The HPG concentration also was found to contribute

to the friction pressure.

Several studies have been made to simulate turbulent

flow. A relationship for the increase in friction pressure

in turbulent flow due to the presence of proppant (Hannah

et al., 1983) is

where& frictionis the friction pressure increase from

solids, pr is the ratio of the apparent slurry viscosity to

the apparent fluid viscosity, and pr is equal to the ratio

of the slurry density to the fluid density.

A subjectw hich hasn ot yet beena dequatelyin vestigated

is the rheology of fracturing fluids containing proppant

under conditions which simulate fracture geometry and

temperatureA. ppropriatee quipment o maket hesec haracterizations

is still lacking; however, devices such as heated

and pressurized helical screw rheometers (Kraynik et al.,

1984) or modified concentric cylinder devices are being

developed which may make these measurements more

practical

5-6 PROPPANT TRANSPORT

during the treatment may result in the formation of a proppant

bank at the bottom of the fracture, and thus increase

the ,risk of proppant bridging and high pumping pressures.

Low settling velocities result in a more evenly distribut-

Propped fracture geometry is determined by the settling ~

ed proppant over the total fracture height and the greatest

potential for productivity improvement. A knowledge of

particle settling velocities as a function of fluid composirates

of the proppant in the fracturing fluid during ,both

tion and treatmentc onditions is necessaryfo r fracture deinjection

and closure. ,High proppant settling velocities

sign and for fluid research leading to compositions ,with

improved proppant transport properties

Most of the studies to characterize proppant transport

properties of fracturing fluids have involved single-particle

fall rates in stagnant fluids: Experiments to determine

settling velocities under flow conditions have involved

large vertical slot models (Schols and Visser, 1974; Sievert

et al., 1981), flow loops with single particles suspended

in a vertical section (Shah, 1986), and rotating concentric

cylinder devices in which particle fall rates could be

observed (Hannah et al., 1978; Harrington et al., 1979;

and Clark and Guler, 1983).

56.1 Predicting Proppant Transport

From Fluid Rheological Data

For Newtonian fluids, fluid viscosity is constant regardless

of the shear rate. In these fluids, the Stokes law