Powder Technology, 24 (1979) 159 - 166
@ Ekevier Sequoia S-A., Lausanne -Printed in the Netherlands
Ekactionation and Particle Size Analysis of Fine Powders by Micro Sieve
J. HIDAKA and S. MIWA
Department of Chemical Engineering. Doshisha University.
(Received Se,ltember 30.1979)
SUMMARY
Wet sieving of fine powders, usually con-
sidered the sub-sieve region, is discussed.
The main trouble in a wet sieving operation
is resistance due to surface tension of the
dispersing medium passing through the
sieve; this is the main reason why wet sieving
of fine powders is difficult. A basic concept
in the design of wet sieving equipment is
shown.
Fine powders are fractionated rapidly by
using the sieving equipment which consists
of ultrasonic vibrator, electromagnetic vibra-
tor, and reciprocating pump. Quantitative
data on the particle size analysis of fine pow-
ders in the size range 45 - 5pm are given and
compared with those obtained by other
methods.
INTRODUCTION
In various industrial processes, achieving
the improvement of quality of products by
utilizing improved scientific techniques, high-
ly technical problems, where it is difficult to
achieve desired results by using the existing
techniques for fractionating powders, are in-
creasing.
In particular, the accurate fractionation of
fine powders is of interest in the manufactur-
ing of speciai powder products and the anal-
yzing of powders.
Usually, a water elutriation or sedimenta-
tion process has been used for such purposes,
but the accuracy is not satisfactory_ In order
to fractionate fine powders accurately, it is
necessary to establish the technique of sieving
for fine powders because the sieving is a most
effective method in size classification methods.
159
Kyoto 602 (Japan)
The main reasons why the sieving process
has been little used for fine powders are the
following:
(1) as the sieve opening is finer, its accuracy
is not satisfactory.
(2) it is difficult to make fine particles pass
rapidly through the sieve aperture.
However, since the electroformed sieve,
which has uniform apertures, has been devel-
oped, it has increased the possibiliw of
sieving fine powders. The existing problem is
how to accelerate the velocity of fine particles
through the sieve.
In the sieving of fine powders, a wet sieving
process should be used because dispersion of
the fine particles in liquid is easier. The wet
sieving process has already been widely used
for fractionating the particles whose particle
size is coarser than about 50pm. In this size
range, it is very rare to experience any &oubIes
in the operation; but in a finer size range, an
especially highly skilled technique is required
in order to make fine particles pass through
the sieve.
In this paper, basic concept on the wet
sieving technique of fine powders and particle
size analysis of fine powders with the micro
sieve is discussed_
BASIC CONCEPT ON WET SIEVING OF FINE
POWDERS
The greatest advantage in wet sieving is the
fact that fine particles are in good dispersion
in liquid where electrostatic and other agglom-
erating forces can be reduced. However, the
following difficult problems arise along with
utilizing liquid as dispersing medium:
(1) resistance to fluid flow of sieve consider-
ably increases.
160

(2) resistance due to surface tension of fluid TABLE 1

through sieve arises. Specification of micro sieve

(3) fine particles on the sieve cause resistance

to fluid flow. Dimension of Mesh Wire diameter Void fraction
Thus it is necessary to investigate a quanti- sieve aperture d E
tative relationship between these resistances (Pm) !m)
and the aperture dimensions of the sieve. 53 250 48.6 0.271
45 350 27.6 0.383
a) Resistance to fluid flow of sieue 32 500 18.8 0.397
Resistance to fluid flow of sieve has been 25 635 15.0 0.391
investigated in detail by Armour and Cannon 20 750 13.9 0.347
16 1000 9.4 0.397
[l] , and the following equation is proposed 10 1270 10.0 0.250
by treating the sieve as a very thin packed bed. 5 1500 11.9 0.091

4P,= f (y=“, - (L/D) (1)

where 4P, is pressure drop through the sieve;

f is friction factor (f = 8_61/Re + 0.52); p is
fluid density; U is fluid velocity; and E is void
fraction of the sieve; Re = pu/pa’D, p is a
fluid viscosity; D is the aperture dimension
of sieve; a is surface area per unit volume
of sieve wire; and L is fiuid path length.
One of the authors, Miwa, investigated the
resi.&mce to fluid flow of various sieves and
pointed out that the calculated values horn
eqn. (1) agree well with the experimental
values [ 2]_
In the experimental work described in this
paper, an electroformed micro sieve is used as
described in Fig. 1 and Table 1. The calculated
Fig. 1. The micro sieve.
value from eqn. (l), for a micro sieve, is
shown in Table 2_ As is evident from the table,
for a small velocity of fluid through the sieve,
the resistance to fluid flow of the sieve does
not affect the sieving operation. However,
in a range finer than 10 pm, the resistance
increases noticeably.
5
Fig. 2. Droplet formed under the sieve surface.
b) Resistance due to surface iension
In wet sieving, the suspension flows out
from a sieve aperture under gravity with drop-
Iet formation as shown in Fig. 2. Therefore,
a pressure difference 4P arises between the
inside and the outside of droplet. When the
suspension flows out from the sieve aperture,
work must be done in order to increase the
surface area of the droplets against this pres-
sure difference_ Then the resistance due to-
surface tension can be represented by 4P and
it is necessary to know this pressure differ-
ence when the liquid film formed on the sieve
surface is broken.
Now, when the main radius of curvature of
the droplet, R, is assumed to be half the sieve
aperture, i.e. R = l/2 D, this pressure differ-
ence, AP, is given by the following equation
based on the Laplace equation_
AP = 20/R = 40-/O (2)
where (Tis a surface tension.

TABLE 2
Resistance to fluid Row of micro sieve (for U = 1 cm/set.)

Dimension of sieve aperture @m) 53 45 32 25 20 16 10 5

Pressure difference APr (cm HaO) 2.2 1.3 1.7 2.2 3.6 3.5 8.9 120.2

Fig. 3. Experimental apparatus for the measurement
of resistance &Je to surface tension.
Comprei&
Fig. 4. Liquid film formed on the sieve surface.
Measurement of resistance due to surface
tension
To experimentally confirm eqn. (2) which
expresses the relationship between AP and D,
the pressure difference, AP, of many sieves
with various aperture dimensions was mea-
sured by using an experimental apparatus as
shown in Fig. 3. A sieve of 20 mm i-d. and
30 mm height is attached to the top of a com-
pression tube. To form a liquid film on the
sieve, liquid is spread thinly over it using a
small brush. Then air in the compression tube
is compressed by slowly elevating a water
tank, and the liquid film formed on the sieve
is expanded by compressed air as shown in
Fig. 4. To measure pressure in the tube, a dia-
phragm gauge using an eIectricaI resistance
strain gauge is employed. When the liquid film
formed on the sieve surface is expanded and
is suddenly broken, the pressure in the tube
suddenly drops. The maximum pressure, P, is
measured_ThendYisthedifferencebetween
P, and atmospheric pressure P,.
The sieves used in this experiment are micro
sieves and ones of plain weave made of stain-
less steel. The dimensions of the sieve aper-
ture are determined by measuring the en-
larged image from a projector. The liquid used
is distilIed water (u = 72-6 dyne/cm) and sur-
161
Fig_ 5. Relationship between AP and the dimensions
of the sieve aperture.
factant solution (a = 30.76 dyne/cm). Surface
tension of liquid used is determined by the
JoIy balance.
In this experiment surface tension acts on
both the inside and the outside of the liquid
film formed on the sieve as shown in Fig_ 4.
Therefore eqn. (2) is rewritten as follows:
AP = So/D (3)
The measured values are shown on a
logarithmic graph in Fig. 5 with the calcu-
lated values from eqn. (3) and it is found that
they lie almost on a straight line and the slope
of the line is -1. From this fact, it is confirmed
that the relationship between D and AP is
correctly shown by the equation AP = ka/D
similar to eqn. (3). However, the measured
values are smaller than the calculated values.
The main reasons are the following three: (1)
shape of the sieve aperture is square; when a
liquid film is expanded, its shape is not spher-
ical, therefore stress concentrations arise at
specific points. (2) contamination of the sieve
surface. (3) the assumption that the radius of
main curvature of droplet is half the sieve
aperture dimension.
From the experiment described above, it is
found thatresislzmce due to surface tension
of fluid flow through a micro sieve or a woven
sieve, which has a square hole and plain weave,
can be estimated by the following equation:
AP = 1.20/D; this measured value is approxi-
mately one third of the calculated value from
eqn. (3) based on the Laplace equation. It was
also found that resistance due to surface ten-
162
sion is larger than resistance to fluid flow
through the sieve.
Eventually, in order to efficiently sieve fine
powders, the sieving equipment must satisfy
the following conditions:
(1) to promote the passing of fine particles
through the sieve aperture, the velocity of
the dispersing medium through the sieve must
be high. Fine particles pass through the sieve
rapidly with a dispersing medium.
(2) to reduce the resistance due to surface
tension, as described above, the sieve surface
must be immersed in a fluid in order to pre-
vent resistance due to surface tension.
(3) to reduce the resistance due to fine parti-
cles on the sieve, the particles should be fluid-
ized while sieving_
EXPERIMENTAL
Sieuing equipment for fine powders
The sieving equipment for fine powders is
shown in Fig. 6. This equipment consists of
Fig. 6. Sieving equipmentfor fine powders.
an ultrasonic vibrator, electromagnetic vibra-
tor and reciprocating pump. Ultrasonic vibra-
tion is used for dispersion of fine powders on
the micro sieve and accelerating the sieving
rate. In order to prevent fine particles from
precipitating on the micro sieve and to increase
the velocity of suspension through the sieve,
a reciprocating pump is used. Since alternate
pressure and vacuum is applied to the micro
sieve by the reciprocating pump, particles on
this sieve are fluidized and particles finer than
the sieve aperture are exhausted out of the
equipment. Amplitude of particles and medi-
um, when ultrasonic vibration is applied to
the particles in liquid, is given by the follow-
ing equation derived by Brant [3] _
s-p,-D,2-fs
(4)
9P,
where X,, and X, are the amplitudes of parti-
cles and medium respectively; pP is particle
density; D, is particle size; pa is viscosity of
air; f, is frequency of ultrasonic vibration.
The ratio X,/X, calculated by eqn. (4) is
shown in Fig. ‘7. It is found that as particle
size becomes coarser, the vibration of parti-
cles becomes inactive, therefore a? entire
set of sieves is vibrated by using an electro-
magnetic vibrator_
Far!icle size Dp (pm)
Fig. 7. Relationship between frequency of ultrasonic
wave and vibration of particles_
One or a stack of several micro sieves are
tightly mounted on an ultrasonic vibrator_ An
O-ring is used to obtain a liquid-tight seal.
First of all, the dispersing medium is put
into the micro sieve and vibration is acti-
vated. Then a 2 - 3% suspension of the ma-
terial to be sieved is poured into the hop-
per_ The dispersing medium used is methanol,
and the diameter of the micro sieve is 75 mm.
Specification of the equipment used is as
follows:
Ultrasonic vibrator; frequency 20,28,40 kHz,
output 0 - 30 W
Electiomagnetic vibrator; frequency 60 Hz,
output 220 w;
Reciprocating pump; capacity 0 - 500 cc/min
at 12 r.p.m.
 163

RESULT AND DISCUSSION

Effect of ultrasonic and electromagnetic vi-

bration on sieving rate
Using one of the micro sieves whose open-
ing is 16 I.rrnor 20 pm, 3 g of silicon carbide
is sieved to investigate the effects of each vi-
bration on sieving rate. The particle size
distribution of silicon carbide used is shown
Particle size 4 CMm ) in Fig. 8.
Fig. 8. Particle size distribution of silicon carbide_ Effects of frequency and intensity of ultra-
sonic vibmtionr
The relationship between the residue on
the micro sieve and sieving time is shown in
Figs. 9 and IO where frequency of ultrasonic
vibration is 20, 28 and 40 kHz respectively,
and the effect of intensity is shown in Fig. 11.
As is evident from these figures, sieving rate
is accelerated by ultrasonic vibration, but the
degree of acceleration is not affected very
much by frequency.
A ztn~bo6;;)3$0 The micro sieve can be damaged by cavita-
Sreving time(Sec_)
tion and impinging of particles accelerated by
Fig. 9. Effect of frequency of ultrasonic wave on ultrasonic vibration to sieve surface. In parti-
sieving rate. (Silicon carbide (* lOOO), micro sieve, cular, impinging of pa&i&es on to the sieve
16 pm, K = centrifugal effect of electromagnetic
surface visibly damages the micro sieve.
vibration).
It has been reported by Neppiras and Noltingk
[4] that the impact force of particles
accelerated by ultrasonic vibration decreases
remarkably when the frequency becomes
higher than about 30 kHz. Therefore about
40 kHz is a suitable frequency for applying
to sieving when using an electroformed sieve
such as a micro sieve, and the intensity of
ultrasonic vibration required about 0.45
Sieving time( 52-C) W/cma.
Fig. 10. Effect of frequency of ultrasonic wave on

\
sieving rate. (SilicoE carbide (_’ 1200), micro sieve, Effect of electromagnetic vibration:
20 W)- Effect of intensity on the sieving rate is
shown in Fig. 12. Centrifugal effect of vibra-

P.. -K-2.51
o K _ i.L5
OK =0.90

Sieving time ( Sec.)

Sieving time(Sec.)
Fig. 11. Effect of intensity of ultrasonic wave on
sieving rate. (Silicon carbide (+ 1200), micro sieve, Fig. 12. Effect of intensity of electromagnetic vibra-
16 ~4. tion. (Silicon carbide (_” 1000) micro sieve, 16 pm).
164

tion R is varied by changing the amplitude of

electromagnetic vibration at constant frequen-
cy (60 Hz). It is found that the sieving action
is promoted by electromagnetic vibration and
as a larger centrifugal effect R is achieved,
the sieving rate is accelerated.

Figure 13 shows particle size distribution

of silicon carbide powder which can pass
through a 20 pm micro sieve at each sieving
Fig. 13. Particle size distribution of Sic which can pass
cycle. As shown in Fig. 7 particle size of sili-
through 20 pm micro sieve at each sieving cycIe.
con carbide (= 1000) is distributed over a nar-
row size range; a large amount of so called dif-
ficult particles for sieving, whose size ranges
from 0.750 to D (where D is the sieve osen-
ing), is included. However, it was found that
almost a.lIfiner particles than the sieve open-
ing passed through the sieve within 4 min. A
smah amount of partLies coarser than the
sieve opening passes through the sieve at the
end of the sieving operation as the shape of
the silicon carbide particles is irregular_ When
Sreving tlme(Sec.)
the weight of sampIe is excessive, the sieving
Fig. 14. Effect of sample weights on sieving rate. rate decreases suddemy as shown in Fig. 14.

Fractionation and particle size analysis

A stack of five micro sieves, whose openings
are 5,8,10,16, and 20 m respectively, was
mounted on the equipment and particle size
analysis was made. Materials used were sihca
beads whose shape was spherical, silicon car-
bide (R 800) which had narrow size distribu-
tion and irregular shape and sintered alumina
(AI&s) powder which had wide size distri-
bution end irregular shape.
Particle size i&oJ m 1 Sieving conditions were as foiIows. The
Fig. 15. Particle size distribution of silica beads frac- dispersing medium was ethanol, centrifugal
tionated by using the micro sieve. effect K was 2.5 and frequency of the ultra-

TABLE 3
The accuracy of micro sieve analysis (silicon carbide (_” 800))

Particle size Measured values R (X) R OR c-v.

(Crm) (%) (%) (%)
Run=1 2 3 4

45 0.07 0.14 0.11 0.09 0.10 0.10 0.03 30

82 O-14 0.21 0.27 0.18 0.20 0.36 0.66 27.4
20 25.33 27.07 25.06 27.90 26.34 26.64 1.36 5.2
16 35.00 34.26 35.23 33.13 34.40 61.04 0.97 2.8
10 37.13 35.49 37.11 36.96 36.67 97.71 0.88 2.4

g Average of the measured values (R)

c+; Standard deviation
C-V.; Coefficient of variation_
 165

0 Andreasen p~pet -Lo-

\
\

Fig. 16. Particle size distribution of silicon carbide Fig. 17. Particle size distribution of sintered alumina.
(-_ 800).

sonic wave was 40 kHz. Sample weights:
silica beads, 2 g, silicon carbide and sir&red
alumina, 3 g. The sieving time was 15 min.
To confirm the sharpness of separation on
this sieving method, particle size distribution
of silica beads retained on each micro sieve
was determined by microscopy and the results
are shown in Fig. 15. As is evident from the
figure, it is found that a high degree of sepa-
ration of fine particles is achieved within 15
_min. Particle size distribution obtained by
this sieving method is shown in Figs. 16 and
17 compared to those obtained by other
methods. The accuracy of this sieving method
is shown in Tables 3 and 4, which shows that
it is accurate enough for practical usage.
CONCLUSIONS
In order that efficient sieving of fine pow-
ders usually considered to be in the subsieve
region, is achieved, the wet sieving process
should be used and the sieving equipment
must satisfy the following conditions:
(1) to promote the passage of fine powders
through the sieve aperture the velocity of
dispersing medium through the sieve must
be high.

TABLE 4
The accuracy of micro sieve analysis (sintered alumina)
-
Particle size Measured values R (%) R *R c-v.

(cun) (XI &L (%I (%I

Run=1 2 3 4

20 43.69 44.34 43.95 43.36 43.84 43.84 0.414 0.90

16 4-83 4.40 5.33 5-21 4.94 48.78 O-412 8.34
10 15.63 i5.97 15.78 16.05 15.86 64.64 0.189 1.20
8 2.77 2.55 2.13 2.26 2.43 67.07 0.288 11.85
5 8.20 9.69 7.82 8-44 8.54 75.61 0.810 9.47

E; Average of the measured values (R)

uR ; Standard deviation
C.V.; Coefficient of variation.
166
(2) to reduce resistance due to surface tension
of the dispersing medium the sieve zxrface
must be immersed in a fluid.
(3) to reduce resistance due to fine particles
on the sieve, these particles should be fluid-
ized while sieving.
Fine particles in size range 45 - 5 pm are
sieved rapidly by using the sieving equipment
based on this concept. The pa.rticIe size dis-
tribution obtained by this sieT*ingmethod
agrees well with the distribution obtained by
Andreasen pipette and photosedimentation
and the accuracy is shown to be good.
This sieving method is useful for obtaining
a small amount of particles of narrow size
distribution.
REFERENCES
1 J. C. Armoar and J. N. Cannon, A.I.Ch.E. Journal,
14 (1968) 415.
2 S. Miwa, Furuiwake-Dokuhon, Sangyogijutsu
Center, Tokyo, 2nd edn., (1974) p_ 218.
3 0. Brandt, Trans. Faraday Sot.. 32 (1936) 1101.
4 E. A_ Neppiras and B. E. Noltingk, fioc. Phys.
Sot. 64b (1951) 1032.