1 Identification of viscoelastic properties with fluid inertia in a parallel plate

2 X effective mechanical system analysis.

with the r
3 Xuesi Gao1 (高学思) and Wook Ryol Hwang1,* (황욱렬)

4 1
School of Mechanical and Aerospace Engineering, Gyeongsang National University, Jinju, 52828,

5 Korea

7 Abstract: Measurement of viscoelastic properties in small amplitude oscillatory shear (SAOS)a

tests

8 can be affected by fluid inertia, especially noticeably at high frequencies. In this study, we introduce an
vs
9 effective mechanical system approach to evaluate
oma m viscoelastic
the effect of fluid inertia on the measured
addres )
10 properties
oman during SAOS tests, employing a parallel plate (PP) geometry. This approach is composed of
measurement cwith
11 systematic mappings
m of m the viscous properties
anoasmsse (polymer viscosity and solvent viscosity), elastic
quantigication atorsional constant
second moment of
12 m 업 rsaorr
properties, and inertial properties of a fluid system onto the damper, the
, spring, and the mass inertia

~ 금 ya
ntarional rag ~ elticienf of a

13 components. In this way, we have

m established an analytical framework for characterizing the
op
iresperively .
oossaerco
e analyfic solunan fy damper
14 ~viscoelastic behavior of a fluid by the effective mechanical system. The
oppa analysis of the frequency
carrat
linear in the presene of flnidinentiae
15 response on the moduli,
언 as obtained by the effective mechanical system, reveals that fluid inertia only

shear modeleus
16 coruW
affects the storage modulus and not the loss modulus. Additionally, we investigate the behavior of the
utre a
17 w gap size, oscillation frequency, and disk radius, while demonstrating a strong
usor
storage modulus with
… asafruncuim ofthe
18 dependence on gap size and frequency. We conducted a comparison자
rorsa of the modulus response
U quan acquired
…
L 없 C
ompanison
.
way made shear
19 from the effective mechanical systems with both the analytical solution of the with solvent viscosity,
rrrpoor o

20 and~
여엮 ak (Oldroyd-B U
numerical simulation results employing two non-linear viscoelastic models model and
8low
21 Giesekus model).
a Thea comparative
염 analyses
m substantiates the
s precision ofo
our approach s
in discerning
없lyavaldape
.
thaccray appooaenn
of this

*
The corresponding author. E-mail: wrhwang@gnu.ac.kr (Wook Ryol Hwang), Fax: +82-55-772-1577, Phone:
+82-55-772-1628

1
 ihe
1 viscoelastic
r omoapooe and inertial properties using the effective mechanical system, with a maximum error of
: 는

2 2.7%.
Λ
3 was rund lessthan
4 I. INTRODUCTION

5 Viscoelastic fluids have diverse applications across several industries, playing a crucial role in

6 enhancing oil recovery (Chen et al. 2021, Hu et al. 2021, van Santvoort and Golombok 2015),

7 improving oil displacement efficiency (Li et al. 2019, Liu et al. 2019, Wu et al. 2021), reducing

8 resistance for water vehicles, and optimizing pipeline transport efficiency (Li et al. 2023,

9 Mohammadtabar et al. 2020, Varshney and Steinberg 2018). Furthermore, in the intermittent slot die

10 coating processes for lithium-ion battery (LIB) slurries, these

crrromfluids exhibit viscoelastic behavior, which
a

frfaglud

mvivnikuncrnnrof
11
crmay a
can adversely affect the uniformity of the coated film
서
(Schmitt et al. 2015). Understanding the
g
12 =
viscoelastic properties of materials inu
industry production
nn is essential for meeting
- production demands

13 effectively,
ropr emphasizing the importance of precise measurement for quantitative assessment.
onsrf e
,

process .

14 a
The Small Amplitude Oscillatory Shear (SAOS) cqtrorucar
test is a rheometric method commonly used
a % 5 밤없pliyed
rheoesical jest
15 to investigate the rheological
여 behavior of ra
viscoelastic fluids,
9 including molten polymers, suspensions,

visrelesnc a

16 and emulsions (Chang et al. 1999, Kogan et al. 2013, Li et al. 2021, Tomaiuolo et al. 2016, Van Aken

17 2001). In SAOS tests,

1 a series of oscillatory frequency sweeps is applied to the sample at a small, fixed
없 lare
18 strain amplitude, typically on the order of 10-2 to 10-1, or even smaller, using a rotational rheometer. The

19 rheometer subsequently converts the measured torque and angular displacement into shear stress and

20 shear strain (or shear rate), thus facilitating the calculation of the storage modulus and the loss modulus

21 components (Barnes et al. 1989).

f
22 qom
However, accurately r
measuring the complex shear modulus can be challenging due to factors
meensurearent

23 such as instrument and sample inertia effects (Ewoldt et al. 2015). Inertial effects due to the instrument

24 may introduce torques that are unconnected to the properties of the sample, particularly in the case of the

25
cmi *
Combined Motor-Transducer (CMT) rheometers,
& where the torque is measured on a moving component
2
 asbyminimigng tu secnd mometf inatia
D …
suc 와

te measured dak wth

by makiy
f crection
f
0
or
al )
inehia Bac 13
2.
mnent 다 …
e
th insaramntl of ( .
.

1 (Läuger and Stettin 2016). The acceleration associated with the oscillatory motion of the fixture induces

2 an erroneous torque on this moving part. As a result, the detected torque encompasses not only the

3 response related with M

the intrinsic properties of the sample but also an extraneous
roon torque from inertial

4 effects, which can compromise the accuracy of the measurement. Inertial effects, especially at higher
없ym
detreriorate
5 frequencies, can significantly affect rheological measurements made with a CMT rheometer and the

6 deviation due to inertial effect is found proportional to the square of the frequency. (Franck 2003,

7 Hudson et al. 2017, Klemuk and Titze 2009, Läuger and Stettin 2016). For materials9 with low elasticity,
임 과
8 instrument inertia can cause measurement bias even at low frequencies (Krieger 1990). Extensive
e 금
9 investigations have been attempted to reduce or crore
get rid of the influence of instrument inertia uffom
ㅅ
on
elimanate
10 measurements. One strategy is to minimize the second moment of inertia of the device, thereby reducing
a
~ ~ ~ ~ ~ ~ ~ ~

11 m
6
the difference between the measured torque and the sample torque. However,
r this method only partially

12 diminishes the influence of instrument inertia on the measurement results. Roughly speaking,
~~ ~ ~ ~ ~

13 decreasing the rotational

m
~ ~ inertia of the instrument by a factor>
~ of 9 will only reduce the deviation related

14 to
□
m ~the inertial effect by a factor of 3. Another strategy involves correction of the measurement data by
m a m

15 using
~… the instrumental moment of inertia (Bae et al. 2013, Baravian et al. 2007, Klemuk and Titze 2009).

16 Modern commercial CMT rheometers take into account the instrument inertia, which is measured and

17
에 ε
compensated prior to sample measurement. In Separate Motor-Transducer (SMT) rheometers,
, the
서
18 torque sensor is decoupled from the strain (or angular displacement) sensor, making them less affected

19 by instrument inertia artifacts. This is because the torque sensor remains stationary during measurement

20 (Franck 2003).
Aithougn
21 Even if instrument inertia is removed or compensated, the inertia of the fluid can still affect
하
업

22 the measurement results (Schrag et al. 1965, Schrag 1977). Fig. 1 presents the complex shear modulus

23 obtained from a SAOS test on a 5%

없 wt Polyethylene Oxide (PEO) solution using a CMT rheometer ( ,
5 wtii

1
샘
24 with PP geometry by changing the gap size. Despite the compensation for instrument inertia in the CMT
뵈
25 rheometer, a noticeable discrepancy in the storage modulus at higher frequencies is still observed for a
dente
26 maararpo
large gap size case. This deviation, which increases with the gap of the parallel
omk plate (PP) geometry. A

Λ
t 3
sige MCR30 이 ,

Antom paar ,

Austria
 fuid inatic is respin ) ibu furthx svepanig
1 dionrmmom
The discrepancy should be attributed to the inertia of the fluid. Numerous studies have been conducted

2 to investigate the effects of fluid inertia on rheological measurements, to either minimize or to account

3 for the influence of fluid inertia on measurement accuracy (Larson 1992, Magda and Larson 1988,

4 McKinley et al. 1996, Turian 1972, Yosick et al. 1998). Schrag

roron (Schrag
m 1977) highlighted that hysteresis

5
conlel
can
심
and he
, lead to measurements bias when oscillating waves propagate at high frequencies over short
Accordiy
fohisgworlc,
6 r
timescales. In PP geometries, fluid inertia causes a delay in the transmission of m
nors the oscillation from the

7 moving plate to the stationary plate. This delay results in phase shift angles to vary across different
nreppseomepryy
r
상

8 spatial points within the fluid, and inconsistencies in these

솎 phase shifts may lead to errors in the modulus
a ; '
AD

C 품
9 values
marsoeobtained from calculations. Schrag (Schrag 1977) conducted extensive analyses on linear
:

e
10 viscoelastic wave propagation, using the analytical solution for both shear rate and phase angle. To
~
-
s
11 maintain the accuracy of viscoelastic measurements within acceptable limits, qrr
Schrag (Schrago
1977)

12 proposed constraints to limit experimental errors due to fluid inertia to within 10%. Additional factors
영 M
vere proposed
13 have been identified
없 that can affect fluid inertia, such as secondary flows (Sdougos et al. 1984), purely
onves riguned
14 elastic instabilities (Shaqfeh 1996), surface tension (Johnston and Ewoldt 2013), free surface films

15 (Sharma et al. 2011), and slip (Buscall 2010). Although these factors are fascinating and persistence,
crn

persistirg
16 they are beyond the scope of frass
this discussion and will not be elaborated here.. In practical applications,
tu
presat
e
pfve 이
17 commercial rheometers employ a diverse range of geometries, such as concentric cylinders (CC), cone-
wsr
be
eqwpped
18 and-plate (CP), parallel-plates (PP), double gap (DG), and various
m other configurations that may rn
feature
Λ~
rheomefricfbow

J
-
nun
기

19 sandblasted, profiled, or serrated surfaces. When one encounters more complex geometries with a large 고

20 amount of liquid, the necessity for analyzing the effects of fluid inertia becomes considerably important. Recionsider

employiry tlenecessity
21 It is widely accepted to analyze mechanical vibrations using
/ mechanical systems
an that 업
of thrs
va va 식
22 incorporate springs,
∞
cam
pn damping, and mass elements. Relationships
impu cmponoyssentence
엷 between torque and angular
brv

suchay
Mr ~
constructed
영
23 displacement aosssomrae
within such a mechanical system can be easily
여 obtained
ouocccrr through simple algebraic
to forsioral osillabwn 6 objet
subjecred f an

24 computations, which involve parameters such as the spring constant, damping

C coefficient, and the
rorsursarsag
: a 쌌
a " tu rha elfecrove 8erant
. ties gncha) forsiwnal drag심 ootapional
25 ciut
second moment of inertia. However, there has been little
a research conducted
맑 on the use of an analogous
corn

26
in ostielcnyefen
futhe Λ
es
amalogyfotre
-

effeerve mechanical system 유

for analyzing oscillations
n of a fluid. For example, Mackay et al. (Mackay
arrt et al. 1992)

Folov " this cnalosy , turelaronship

4
BO
y
 utee
1 presented equations of motion for a damped torsional oscillator, in which an instrument inertia,

2 instrument damping coefficient, sample damping coefficient, and torsional spring constant Q
was
were

3 introduced. Titze et al. (Titze

냔 et al. 2004) presented equations of motion for an oscillating fluid in a PP
C
4 ccro analysis.
rheometer, neglecting fluid inertia, and derived the torque response via~mechanical vibration
jeeltreetive
5 aoron
Klemuk and Titze (Klemuk and Titze 2009) divided the vibrating system into two sections: the rotor

6 and the sample. They formulated separated

. equations of motion for each section and merged them to
Lw
7 derive A
the equationsq of motion for the entire system. However, their study solely focused on
a
singh
8 investigating the effect of motor inertia and did not address the effect of fluid inertia. To the best

9 knowledge of the authors, no approach has conducted to analyze the fluid inertia effect in SAOS tests

10 through the effective mechanical system.

" "

s pemove
.

s brion
pEo
.

5 wtf
fov a
3
h
.

11 this fgve P

r
in
prt
.
.
~

langer PP geomefry
" v. m
mala te 8 igme
.
uthe utre U
12 Figure 1. ao
Response of storage modulus (𝐺′) and loss modulus (𝐺′′) to frequency in SAOS tests.
KZ The
e
13 storage modulus and loss modulus of 5% weight PEO solution were investigated for frequency
romariarprrosmooo
14 rcowitth
dependence. This was done for a parallel plate geometry with a diameter of 50 mm and considering
rosoasoom
15 three different gaps (1, 2, and 3 mm).
221 . 412 .
244
ㅡ
16 In this work, we address the effect of fluid inertia on the measurement of rheological properties

17 by modeling viscoelastic-inertial fluid systems. We focus on SAOS tests conducted with the CMT