POWDER FLOW

• Four commonly reported methods for testing

powder flow are (1) angle of repose, (2)
compressibility index or Hausner ratio, (3) flow
rate through an orifice, and (4) shear cell. In
addition, numerous variations of each of these
basic methods are available. Given the
number of test methods and variations,
standardizing the test methodology, where
possible, would be advantageous.
 ANGLE OF REPOSE
• Angle of repose is a characteristic related to interparticulate
friction or resistance to movement between particles.
• The most common methods for determining the static
angle of repose can be classified on the basis of the
following two important experimental variables:
• 1. The height of the “funnel” through which the powder
passes may be fixed relative to the base, or the height may
be varied as the pile forms.
• 2. The base upon which the pile forms may be of fixed
diameter or the diameter of the powder cone may be
allowed to vary as the pile forms.
 Variations in Angle of Repose Methods
• Drained angle of repose is determined by allowing an excess
quantity of material positioned above a fixed diameter base to
“drain” from the container. Formation of a cone of powder on
the fixed diameter base allows determination of the drained
angle of repose.
• Dynamic angle of repose is determined by filling a cylinder (with
a clear, flat cover on one end) and rotating it at a specified
speed. The dynamic angle of repose is the angle (relative to the
horizontal) formed by the flowing powder. The internal angle of
kinetic friction is defined by the plane separating those particles
sliding down the top layer of the powder and those particles
that are rotating with the drum (with roughened surface).
 Angle of Repose General Scale of
Flowability
• There are examples in the literature of
formulations with an angle of repose in the
range of 40 to 50 that were manufactured
satisfactorily. When the angle of repose
exceeds 50, the flow is rarely acceptable for
manufacturing purposes.
 Experimental Considerations for Angle of
Repose
• Angle of repose is not an intrinsic property of the powder; i.e., it is
very much dependent upon the method used to form the cone of
powder. The following important considerations are raised in the
existing literature:
• The peak of the cone of powder can be distorted by the impact of
powder from above. By carefully building the powder cone, the
distortion caused by impact can be minimized.
• The nature of the base upon which the powder cone is formed
influences the angle of repose. It is recommended that the powder
cone be formed on a “common base,” which can be achieved by
forming the cone of powder on a layer of powder. This can be done
by using a base of fixed diameter with a protruding outer edge to
retain a layer of powder upon which the cone is formed.
 Recommended Procedure for Angle of
Repose
• Form the angle of repose on a fixed base with a retaining lip to
retain a layer of powder on the base. The base should be free
of vibration. Vary the height of the funnel to carefully build up
a symmetrical cone of powder. Care should be taken to prevent
vibration as the funnel is moved. The funnel height should be
maintained approximately 2–4 cm from the top of the powder
pile as it is being formed in order to minimize the impact of
falling powder on the tip of the cone. If a symmetrical cone of
powder cannot be successfully or reproducibly prepared, this
method is not appropriate. Determine the angle of repose by
measuring the height of the cone of powder and calculating
the angle of repose, , from the following equation:
 FLOW THROUGH AN ORIFICE
• The flow rate through an orifice is generally
measured as the mass per time flowing from
any of a number of types of containers
(cylinders, funnels, hoppers). Measurement of
the flow rate can be in discrete increments or
continuous.
Basic Methods for Flow Through an Orifice
• There are a variety of methods described in the literature. The most
common method for determining the flow rate through an orifice can be
classified on the basis of three important experimental variables:
• 1. The type of container used to contain the powder. Common containers
are cylinders, funnels, and hoppers from production equipment.
• 2. The size and shape of the orifice used. The orifice diameter and shape
are critical factors in determining powder flow rate.
• 3. The method of measuring powder flow rate. Flow rate can be measured
continuously using an electronic balance with some sort of recording
device (strip chart recorder, computer). It can also be measured in discrete
samples (for example, the time it takes for 100 g of powder to pass
through the orifice to the nearest tenth of a second or the amount of
powder passing through the orifice in 10 seconds to the nearest tenth of a
gram).
Variations in Methods for Flow Through an
Orifice
• Either mass flow rate or volume flow rate can be
determined. Mass flow rate is the easier of the
methods, but it biases the results in favor of high-
density materials. Because die fill is volumetric,
determining volume flow rate may be preferable. A
vibrator is occasionally attached to facilitate flow from
the container; however, this appears to complicate
interpretation of the results. A moving orifice device has
been proposed to more closely simulate rotary press
conditions. The minimum diameter orifice through
which powder flows can also be identified.
 Experimental Considerations for Flow
Through an Orifice
Flow rate through an orifice is not an intrinsic
property of the powder. It very much depends
on the methodology used. Several important
considerations affecting these methods are
discussed in the existing literature:
• The diameter and shape of the orifice
• The type of container material (metal, glass,
plastic)
• The diameter and height of the powder bed.
Recommended Procedure for Flow Through
an Orifice
• Flow rate through an orifice can be used only for materials that have some capacity to flow. It is not
useful for cohesive materials. Provided that the height of the powder bed (the “head” of the powder)
is much greater than the diameter of the orifice, the flow rate is virtually independent of the powder
head. Use a cylinder as the container because the cylinder material should have little effect on flow.
This configuration results in flow rate being determined by the movement of powder over powder
rather than powder along the wall of the container. Powder flow rate often increases when the height
of the powder column is less than two times the diameter of the column. The orifice should be circular
and the cylinder should be free of vibration. General guidelines for dimensions of the cylinder are as
follows:
• Diameter of opening > 6 times the diameter of the particles
• Diameter of the cylinder > 2 times the diameter of the opening
• Use of a hopper as the container may be appropriate and representative of flow in a production
situation. It is not advisable to use a funnel, particularly one with a stem, because flow rate will be
determined by the size and length of the stem as well as the friction between the stem and the
powder. A truncated cone may be appropriate, but flow will be influenced by the powder-wall friction
coefficient, making selection of an appropriate construction material an important consideration.
• For the opening in the cylinder, use a flat-faced bottom plate with the option to vary orifice diameter to
provide maximum flexibility and to better ensure a powder-over-powder flow pattern. Rate
measurement can be either discrete or continuous. Continuous measurement using an electronic
balance can more effectively detect momentary flow rate variations.
 SHEAR CELL METHODS
• One type of shear cell is the cylindrical shear cell that is split horizontally, forming a shear plane between
the lower stationary base and the upper moveable portion of the shear cell ring. After powder bed
consolidation in the shear cell (using a well-defined procedure), the force necessary to shear the powder
bed by moving the upper ring is determined. Annular shear cell designs offer some advantages over the
cylindrical shear cell design, including the need for less material. A disadvantage, however, is that
because of its design, the powder bed is not sheared as uniformly; i.e., material on the outside of the
annulus is sheared more than material in the inner region. A third type of shear cell (plate-type) consists
of a thin sandwich of powder between a lower stationary rough surface and an upper rough surface that
is moveable.
• All of the shear cell methods have their advantages and disadvantages, but a detailed review is beyond
the scope of this chapter. As with the other methods for characterizing powder flow, many variations are
described in the literature. A significant advantage of shear cell methodology in general is a greater
degree of experimental control. The methodology is rather time-consuming and requires significant
amounts of material and a well-trained operator.
• The many existing shear cell configurations and test methods provide a wealth of data and can be used
very effectively to characterize powder flow. They are also helpful in the design of equipment such as
hoppers and bins. Because of the diversity of available equipment and experimental procedures, no
specific recommendations regarding methodology are presented in this chapter. It is recommended that
the results of powder flow characterization using shear cell methodology include a complete description
of equipment and methodology used.