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Rheological Properties
Rheological Properties
Rheological Properties
RHEOLOGICAL PROPERTIES
Therefore a Newtonian fluid exhibits a linear relationship between shear stress & shear
rate and hence viscosity is independent of the applied shear conditions as shown in
figure.
(Newtonian Fluid flow behaviour)
The viscosity of a Newtonian fluid is dependent only on temperature but not on shear
rate and time. e.g. Water, Milk, Sugar solution, Mineral Oil etc. are the common
example of Newtonian fluid.
Most cases, the relationship between shear stress () and shear rate () is not linear and
these fluids are called as Non-Newtonian Fluid.
Non-Newtonian Fluids
A Non-Newtonian fluid is a fluid in which the viscosity changes with the applied strain
rate. As result, non-Newtonian fluids may not have a well-defined viscosity.
Non-Newtonian fluids are either time dependent or time independent.
Non-Newtonian Fluids, Time Dependent
It is further classified as rheopectic and thixopectic non-Newtonian fluids.
Rheopecty or Rheopexy: The fluid in which the viscosity increases with shear strain is
called rheopecty or rheopexy fluid. Example: lubricants.
Thixotropy: The fluid in which the viscosity decreases with time at constant shear
strain is called rheopecty or rheopexy fluid. Example: gypsum pastes, printer inks etc.
Rheopectic Thixotropic
Pseudoplastic Fluids: Shear thinning fluids are also called Pseudoplastic. e.g.
Paint, Shampoo, Slurries, Polymer Melts, Ketch up, etc.
The - and - relationship for pseudoplastic fluids is shown below in Figure
Plot of shear stress versus shear rate for Plot of shear viscosity versus shear
Pseudoplastic fluids rate for pseudoplastic fluids
Plot of shear stress versus shear rate for Plot of shear viscosity versus shear
rate for dilatant fluids dilatant fluids
c) Bingham Plastic: Exhibits so-called yield value i.e. a critical shear stress must be
applied to cause the fluid flow.
Bingham Fluids / Plastic: These fluids are believed to have an internal structure,
which resists the flow of fluid at lower shear stress. Therefore, a certain shear stress
value needs to be applied to help the fluid flow.
Examples: - Tomato Paste, Tooth Paste, Hand Cream, Grease, etc.
The characteristic shear stress for a given Bingham Plastic fluid is called Yield Stress.
1. Capillary Type
2. Rotational Type
3. Torque Rheometer
These instruments are laboratory tool often used to predict processing behaviour and to
simulate realistic use conditions. Some of the typical applications include determining
melt flow behaviour, polymers degradation time at varying shear rates, rheological
properties, pigment dispersion, characterizing different formulations, and observing the
effects of changing ingredients and temperatures.
The melt-flow rate (MFR) or melt volume-flow rate (MVR) test measures the flow of a
molten polymer through an extrusion plastometer under specific temperature and load
conditions.
Significance:
The reported melt index values help to distinguish between the different grades of a
polymer. A high molecular weight material is more resistant to flow than a low
molecular-weight material.
It can also be useful for other purposes like studying the relative thermal effect with
respect to barrel residence time on plastics.
Test Methods: ASTM D 1238, ISO 1133, DIN 53735
Specimen Dimension: The test specimen should be in the form of powder, granules,
strips or film or moulded slugs.
Conditioning: The test specimen should be conditioned at 232°C and 505% relative
humidity for 48 hrs prior to the test.
Test Apparatus: The extrusion plastometer consists of a vertical cylinder with a small
die of 2 mm at the bottom and a removable piston at the top. A charge of material is
placed in the cylinder and preheated for several minutes. The piston is placed on top of
the molten polymer and its weight forces the polymer through the die and on to a
collecting plate. The time interval for the test ranges from 15 seconds to 6 minutes in
order to accommodate the different viscosities of plastics. Temperatures used are 220,
250 and 300°C. Loads used are 1.2, 5 and 10 kg. The amount of polymer collected after
a specific interval is weighed and normalized to the number of grams that would have
been extruded in 10 minutes: melt flow rate is expressed in grams per reference time.
Apparatus for determination of MFI
Test Procedure:
Set the temperature according to the chart given in Table.
Place the thermometer on the hold provided.
The set temperature stabilizes for 5 min then fills the material using tool without any
air gap. Then apply the load over the piston. Allow some time for material to melt and
soften and purge the material upto the lower mark of the piston.
The rate of extrusion is measured by cutting off the extrudate at suitable intervals.
These cuts are taken when the piston head is between 50 mm and 20 mm the upper
end of the die (i. e. between the scribed lines on the piston).
At least three cut-off samples are weighed and average mass is calculated. MFI is
calculated as the amount extruded in 600 seconds. The results are reported,
specifying the temperature and applied load.
Table: Temperature and load for MFI test as a Case Study
Material Temperature Load, Kg
Acetal (Homo &
190 2.16/1.05
Copolymer)
PMMA 230 1.2/3.8
ABS 200 and 230 5.0 and 3.8
Cellolose esters 190 and 210 0.325/2.16/21.6
Nylon66 275 0.325
Nylon6 235 1.0/2.16/5.0
PCTFE 265 12.5
PE 125 0.325/2.16
190 0.325/2.16/10/2.16
310 12.5
PC 300 1.2
PP 230 2.16
PS or HIPS 190 5.0
200 5.0
230 1.2/3.8
Polyterepthalate 210 2.16
250 2.16
285 2.16
PPS 315 5.0
Calculations: Then start the stopwatch and start cutting off the extrudate depending
upon the flow for example, 30 Sec., 1 min, 3 min, or 6 min intervals and tabulate the
weight of the extrudate.
Flow rate = (m/t) x 600
Where m = mass extruded, t = time of piston travel for length L. (sec), 600 =
conversion factor to convert in sec.
Factors Influencing:
Preheat Time: If the cylinder is not preheated for a specified length of time, there is
usually some non-uniformity in temperature along the walls of the cylinder even
though the temperature indicated on the thermometer is close to the set point. This
causes the flow rate to vary considerably.
Moisture. Moisture in the material causes bubbles to appear in the extrudate. The
weight of the extrudate is significantly influenced by the presence of the moisture
bubbles.
Packing. The sample resin in the cylinder must be packed properly by pushing the
rod with substantial force to allow the air entrapped between the resins pellets to
escape. Once the piston is lowered, the cylinder is sealed of air can escape. This
causes variation in the test results.
Volume of Sample: Change in sample volume causes the heat transfer from the
cylinder to the material.
Test Apparatus:
The capillary rheometer consists of an electrically heated cylinder, a pressure ram,
temperature controller, timer and interchangeable capillaries. The plunger can be
moved at a constant velocity that translates to a constant shear rate. The forces to
move the plunger at this speed is recorded which determines the shear stress.
Alternately, a weight or constant pressure can be applied to the plunger which
generates a constant shear stress and the velocity of the plunger is determined by
cutting and weighing the output. Shear rate can be calculated by knowing the melt
densities.
Test Procedures:
Select test temperature, shear rates and shear stress in accordance with material
specification
Recommended test temperatures of different thermoplastics are given in table.
Replace the die and piston in the barrel and allow the assembled apparatus to reach
thermal equilibrium.
The sample material is placed in the barrel of the extrusion assembly, brought to
temperature and forced out through a capillary. The charging of materials should be
done within 2 min.
Place the piston movement until the full melt time reached. Reactivate the piston to
start extrusion. After reached steady state operation, record the force and record the
data by:
Run a constant rate test (or a constant shear stress test)
Run a multiple rate of multiple stress level test
Calculations: Shear stress, shear rate and apparent melt viscosities are calculated as
follows:
Fr
( Pa)
2 R 2l
Where, = shear stress (psi); F = Load on the ram (lbs); r = radius of capillary orifice
(in); R= radius of the barrel (in); l = length of capillary oriface (in).
4Q
( s 1 ) 3
r
Where, = shear rate (sec ); Q = flow rate (in3/sec.)
-1
Shear stress
Apparent melt viscosity (poise) ( Pa.s 1 )
Shear rate
Factors Influencing:
Capillary Calibration: The apparent viscosity varies with the fourth power of r, it is
desirable to know this value within 0.00762 mm.
Piston friction: The frictional force is negligible compared to the pressure drop through
the capillary. The frictional force should be subtracted from force reading.
Polymer back flow: The clearance between the plunger and the barrel may permit a
small amount of melt to flow along with the piston instead of flowing through the
capillary. Due to this the true shear rate needs to be lower than that calculated from the
piston velocity. Measuring the rate of capillary extruded and comparing this with the
actual piston displacement rate, taking into account the change in fluid density, enable
us to determine the shear rate.
Melt compressibility: As the hydrostatic pressure diminishes along with the capillary,
the fluid density decreases and the flow rate increases. This results in an increase in
shear rate.
Determining True Shear Stress: To obtain true shear stress, perform the following
procedure: using a minimum of two dies having same entrance angle and same
diameter (D) of different capillary length (L). At least one L/D ratio should be less than
16 and one should be more than 16. Obtain the true shear stress using the following
equation:
( P Pc ) D ( F Fc ) D
4L 4 LAB
Where, = Ture shear stress
P = Melt pressure
Pc = the intercept between shear rate
D = dia meter
L = Die length
Ab = Cross section area
Fc = Bagley plot
For Newtonian fluid, the basic equations for the cone and plate rheometer are:
3 M
2 R 3
dv
dr
3M
2 R 3
R = Radius distance of the sample in cone and plate
= Angle in radian which cone makes with the flat plate
M = Torque required to rotate the cone relative to the plate of an angular frequency of
Co-axial Viscometer
It consists of two cylinders, one within the other (cup and bob) with the sample between
them (Figure 13). The first practical rotational viscometer consisted of a rotating cup
with an inner cylinder supported by torsion wire. The relationship between viscosity,
angular and torque for a Newtonian fluid in a concentric cylinder viscometer is given
below:
M 1 1 kM
2 2
4 h Ri Ro
Where, M is the torque on the inner cylinder, h is the length of the inner cylinder, is
the relative angular velocity of the cylinder in radius per seconds R i the radius of the
inner cylinder wall, Ro the radius of the outer cylinder wall and k an instrument constant.
The shear rate can be given by
2 / r 2 Ri 2 Ro 2 Where r is any given radius.
Ro
2
Ri
2
The shear stress is given by: M 2
2 r h
Co-axial Viscometer
The viscosity of Newtonian liquid may be determined from the above equation or from
slope of a shear stress –shear rate plot. Non-Newtonian fluid gives intercepts and
curves with such plots.
Definition: The viscosity defined as the flow behaviour of plastisol under low shear.
This viscosity relates to the conditions encountered in pouring, casting, molding and
dipping process. The Brookfield instrument is a commercially used rotating spindle type
viscometer
Significance: The suitability of a dispersion resin for given application process is
dependent upon its viscosity characteristics. The test standard for viscosity
measurement of plastisols / organosols, epoxy resin and emulsion etc
Test Methods: ASTM D-2393, ASTM D 1824 and ISO 2555.
Test specimen: The specimen should be in liquid form.
Procedure:
1) Select the spindle in middle or upper portion of viscometer dial at the highest
rotational speed to be used. Insert the spindle approximately at 45° angle. Move the
sample so as to center the spindle, adjust the depth to the immersion mark.
2) Start the viscometer at its lowest speed. Allow it to run 2 min. record the scale
reading during the next rotation.
3) Placing it in a constant temperature bath at the specified test temperature
preconditions the sample. The proper spindle size is allowed to rotate in the sample
for 30 sec. The instrument is stopped through the use of a clutch and the reading is
taken from the dial. The test is repeated until a constant reading is obtained.
4) Record the sample temperature at the conclusion of viscosity reading.
Calculation: Calculate the viscosity using the factors provided with the viscometer
Test Apparatus:
3. Because of lot-to-lot variations in the quality of plasticizer, and basic lead carbonate,
it is recommended that the laboratory maintain a large enough inventory of these
additives to establish control standards. A standard powder-mix curve should also
be generated using standard additives and kept on file for comparison purposes.
Temperature : 88 1°C
Mixer Speed : 63 1 rpm
Material Weight : 380g 10g
Thermosetting Materials
The ability of the material to flow is measured by filling a mold with the plastics materials
under a specified condition of applied temperature and pressure with a controlled
charge mass. The flow tests are used as a quality control test and as an acceptance
criterion for incoming raw materials.
Factor Affecting Flow:
1) Resin Type: All resins flow differently because of basic differences in the structure of
the polymer e.g. melamine formaldehyde exhibit longer flow than urea
formaldehyde.
2) Type of filler: The small particle size filler e.g. wood floor, mica, and minerals creates
less turbulence and less frictional drag during mold filling. The size of the glass fibre
and long fiber can adversely affect the flow.
3) Storage Time: All resins have a natural tendency to polymerize in storage, causing
partial precure, which reduces flow.
Phenolics: 165 1 °C
Melamine: 155 1 °C
Urea: 150 1 °C
Epoxy: 150 1 °C
Diallyl phthalates: 150 1 °C
Alkyd: 150 1 °C
2. Take the weight and begin the test with proper load to close the mold to the fin
thickness specified for the type of material. The load can be applied to the mold
is as given below:
Total Load Molding Pressure (MPa)
1112 4.6
1601 6.6
1124 9.0
1686 13.6
2248 18.0
3372 21.2
4496 36.3
11120 45.4
If a 2248 N load applied to make initial cup and required fin thickness is obtained, the
next lower load 1686N is applied as indicated above. If the mold close to the required
thickness again then next 1124 N load applied. If the mold then does not close, the
‘molding index’ is close to 1686 N load.
3. The time of flow in seconds shell be measured from that the hydraulic gage
indicates an applied load of 454 kg to the instant that the fin has reached 0.20 mm I
thickness for material with an izod impact strength of 27 J/m of notch.
Procedure:
1) Heat the mold and transfer the plunger 1503°C.
2) The plunger preferably is equipped with sealing grooves. These must be cleaned
freee of compounds before checking and before each molding
3) Using a force gage adjust the transfer pressure to 6.99 MPa.
4) Weight out the compound to the nearest 0.1 g as previous determined to yield a 3 to
3.5 mm-molded cull.
5) Place the compound in the transfer pot activate the transfer cycle immediate. Cure
the compound as recommended for easy removal.
6) Open mold and remove the cured material. Read the spiral floe length directly from
molded specimen at the point of farthest continuously flow to nearest 0.25 in.