Development of Asymmetric Polyethersulfone (PES) Membrane for O2/N2 Separation by

Using Difference Technique of Membrane Formation

Mardhiana Binti Ismail, Norida Binti Ridzuan

Faculty of Chemical Engineering & Natural Resource,

Universiti Malaysia Pahang, Lebuharaya Tun Razak. 26300 Gambang, Kuantan, Pahang Darul Makmur

Abstract

Asymmetric polyethersulfone membranes for gas separation by varying the technique of membrane formation have been successfully developed.,
the casting solution with the concentration of 32.62 wt% PES, 60.58 wt% NMP and 6.8 wt% H 2O were used to produce polyethersulfone flat
sheet asymmetric membrane. The produced membranes were characterized by pure gas permeation experiments by using permeation test unit and
the morphology of the membrane was identified using Scanning Electron Microscopy (SEM). For permeation test, oxygen (O 2) and nitrogen (N2)
were used as a test gases for both uncoated and coated membranes. For the coated membrane, pressure-normalized flux and selectivity showed a
more constant trend with increasing feed pressure compare to uncoated membrane for all method of drying process. Coated membrane exhibited
higher selectivity than uncoated membranes due to coating of the skin layer defects. Consequently, the best selectivity was found using the
dry/wet phase inversion compared than others. The pressure-normalized flux and O2/N2 selectivity were found 25.39 GPU for O2 and 10.12 GPU
for N2 and 2.53 respectively. For the Scanning Electron Microscopy (SEM) result, flat sheet membrane prepared by dry/wet phase inversion show
the formation of asymmetric membrane with a thin and dense skin layer supported by a thick porous sublayer compared to other which dry at
room temperature and dry in oven at 40C with formation of symmetric membrane with the diameter of the pores is almost constant throughout
the cross section of the membrane.flat sheet membrane prepared by dry/wet phase inversion show the a dense skin layer and sublayer with
existing of microvoid and macrovoid while flat sheet membrane prepared by dry at room temperature and dry in oven at 40C show the formation
of porous layer with small microvoid which look sponge like and existing of porous layer with macrovoid respectively. As a conclusion, dry/wet
phase inversion technique has successfully developed asymmetric membranes and can be applied for O2/N2 separation.

Keywords: Asymmetric membrane, Gas separation, Dry/wet phase inversion, Morphology

into four different techniques which thermal precipitation,

1. Introduction
Membrane separation process has become one of the
emerging technologies, which have undergone a rapid
growth during the past few decades. Membrane is a phase
or a group of phase that lies between two different phases,
which is physically and/ or chemically distinctive from
both of them and which, due to its properties and the force
field applied, is able to control the mass transport between
these phases [1]. In simple word, membranes are thin
layers, that can have significantly different structures, but
all have the common feature of selective transport to
different components in feed.
Gas separations become a major industrial application
of membrane technology only during the past 15 years, but
the study of gas separation actually began long before that
period [2]. Phase inversion techniques can be categorized
air casting of dope solution, precipitation from the vapour
phase and immersion precipitation [3]. Phase inversion is
important stage in the membrane formation to get high
performance which high selectivity and permeability of
membrane and defect-free asymmetric polyethersulfone
(PES) membrane for gas separation application. According
to previous researchers [4], the correlation of primary
dry/wet phase inversion with rheological aspects had
successfully developed defect-free and ultrathin-skinned
asymmetric membrane for gas separation. For the result,
membrane by polymer solution containing solvent ratio
which 4.0 wt % wt% resulted in asymmetric membrane
having a thin and porous skin layer with a macrovoid-filled
open cell substructure were formed.
From different perspective, [5, 6], had expressed that
ultrathin-skinned and defect-free asymmetric membrane by
dry-casting method. As a result, only solvent whereas
acetone evaporated because used the high boiling point of
nonsolvent in membrane formation.[5]. Membrane
formation of dry-casting method have correlation with
concentration with water (nonslovent) in the initial casting
solution and evaporation conditions. Without altering
polymer, solvent, or nonsolvent, it is possible to vary the
structure from dense to porous asymmetric by either
increasing the nonsolvent composition or decreasing the air
velocity during evaporation as has been carried out by
earlier researcher. [6]. As results, porous asymmetric
membrane produced with acetone 80m3 %, water 10m3 %
and cellulose acetone 10m3 %.
Integral skinned asymmetric gas separation
membranes were prepared by (i) dry, (ii) wet, and (iii)
dry/wet phase inversion processes. [3]. As a results,
membrane made by dry/wet phase inversion showed
optimum gas separation performance. The average O2/N2
and He/N2 selectivity of these membranes were within 85%
of those determined for a dense [7]. The average apparent
skin layer thickness of all samples tested was 270 Å. For
scanning electron microscopy, it consists of an ultrathin
skin layer, a tightly packed nodular transition layer, and an
open cell, sponge-like substructure. Dry phase inversion
membranes exhibited extremely low gas fluxes due to thick
(17.5µm) skin layers. On the other hand, wet phase
inversion membranes showed O2/N2 selectivity< 1,
indicating that gas transport was determined by pore flow
through skin layer defects.
Thus, different technique of membrane formation will
be studied where it strongly believes that will affect the
permeability and the selectivity of the membrane.
2. Experimental
2.1 Material
PES was used as polymer because PES is an
amorphous polymer with a glass transition temperature
220°C and shows excellent hydrolytic stability compared to
other membrane-forming polymer. NMP is chosen as the
solvent because it has good chemical stability, high
solvency and high boiling point. Distilled water use as
nonsolvent additives while tab water and methanol was
used as coagulation bath in this study. Distilled water is
was used nonsolvent additives in this study because
distilled water have high solubility compare to other
nonsolvent additives such as ethanol. Oxygen and nitrogen
was used as test gases with purity of both gases were
99.99%.
2.2 Membrane Preparation
The dope solution should contain polymer, a solvent
system, and a nonsolvent system. PES was first dried in a
vacuum oven at least 4 hours at temperature 60ºC in order
to remove all absorbed water vapor. Then, PES was
dissolved in NMP (solvent) and nonsolvent additives. The
dope solution was heated at 60-80 ºC and stirred for about
3-4 hours to achieve completely dissolve. Finally, the dope
solution was kept in storage bottle and was degassed by
using ultrasonic bath to remove any traces of micro bubbles
inside the dope solution.
2.3 Membrane Casting
The first technique was dry/wet phase inversion which
the dope solution was cast by using a casting block, at room
temperature. The small amount of dope solution was
poured into a glass plate with a casting block setting 400
μm. During the casting process, forced convective
evaporation was induced on membranes before being
immersed into the coagulation medium. Second technique
was dry-casting at room temperature which small amount
of casting solution was poured into a glass plate with a
casting block setting 400μm. After casting, the membrane
was leave at room temperature with ambient temperature
for 2 day until it pilled off from the glass plate. For the
third technique, dry-casting in oven at 40°C, the small
amount of dope solution was poured into a glass plate with
a casting block setting 400μm and immediately the
membrane was put in vacuum oven at temperature 40 ºC
for 10 minutes before leave it at room temperature for 2
days.
3. Result and Discussion
3.1 Effect of Drying Technique on O2/N2 Separation
Membrane Performance
3.1.1 Performance of Uncoated Polyethersulfone selection was based on the scanning image produced,
Membranes which show the formation of the asymmetric membrane
with a thin and dense skin layer supported by a thick
The polyethersulfone flat sheet asymmetric membrane porous sublayer compared to other which dry at room
were prepared with casting solution contained of temperature and dry in oven with formation of symmetric
polyethersulfone (PES) as polymer, 1-methyl-2- membrane with the diameter of the pore is almost constant.
pyrrolidone (NMP) was employed as a solvent while The activation energies for permeation of nitrogen and
distilled water (H2O) was used as nonsolvent additives oxygen were found to be higher in the asymmetric
(NSA). The composition of the casting solution which membrane, suggesting that the free volume of the polymer
contained 32.6wt% PES, 60.58wt% NMP and 6.8wt% H2O in the asymmetric skin layer is lower. [8]
were used to produce asymmetric membrane flat sheet
For the dry at room temperature, the porous layer with
membrane by using different drying technique. The drying
microvoid (sponge-like structure) while for the dry in oven
technique that used were dry/wet phase inversion, dry at
at 40°C show the formation of symmetric membrane with
room temperature and dry in oven at 40ºC. The pressure-
macrovoid. Plugging of membrane easily occur for the
normalized flux of the membranes was tested for pure
symmetric membrane. However, in this case all the
gases which are oxygen (O2) and Nitrogen (N2) at 25ºC and
uncoated membrane a poor performance of gas separation.
1 bar of feed pressure by mean of a permeation test unit.
Therefore, to obtain high performance polyethersulfone
The average range of the O2/N2 selectivities for membrane
membrane, skin layer should be coated using
samples prepared by dry/wet phase inversion was about
polydimethylsilicone (PDMS).
1.03 to 1.19 while selectivities for membrane sample
prepared by dry at room temperature was about 0.27 to 1.71
and selectivities for membrane sample prepared by dry in
oven at 40ºC was about 0 to 1.74. Pressure-normalized flux Figure 3.1: Pressure-normalized flux and selectivity vs
and selectivity of the membrane prepared by dry in oven at drying technique of uncoated membrane at different drying
40ºC was cannot be measured due to the membrane was technique at 3 bar
broken at high pressure. The membrane was broken at 3.1.2Performance of Uncoated Polyethersulfone
pressure 4 bar and it show that the membrane prepared by Membrane
dry in oven at 40 ºC was not good because this membrane
cannot stand at high pressure. As predicted, the membrane performance improved
after being coated with silicone rubber. Poor selectivities of
Figure 3.1 below show the pressure normalized flux
uncoated membranes are most probably contributed by
and selectivity of uncoated membrane at optimum pressure.
surface defects at the dense skin layer of the membranes.
The optimum pressures for the prepared membrane by 3
Therefore, coating is essential to heal the imperfections in
drying technique were 3 bars. All uncoated membrane
order to produce practically useful membranes. Coating
exhibit higher pressure normalized flux but low selectivity
results in reduction of pressure normalized flux of all gases,
due to the skin layer porous (defects) are dominant. From
but can greatly enhance the selectivities of the membranes
the Figure 3.1, it shows that the pressure normalized flux
by caulking the pinholes or defects on the membranes
for both gases are high with the value about 958.08 GPU to
dense layer. Figure 3.2 below show the pressure-
5391.793 GPU but low selectivity with the value about
normalized flux and selectivity vs drying technique of
1.04 to 1.71. However, in this study, dry/wet phase
coated membrane at different drying technique at 3 bar
inversion technique was chosen as the best technique even
though the average selectivity was about 1.05 lower than
dry at room temperature technique which was 1.71. This
Figure 3.2: Pressure-normalized flux and selectivity vs
drying technique of coated membrane at different drying
technique at 3 bar
Referring to Figure 3.2 above, the flat sheet membrane
prepared by dry/wet phase inversion showed high
selectivity but low pressure-normalized flux. The flat sheet
membrane prepared by dry at room temperature exhibits
high both pressure-normalized flux and selectivity while
for the flat sheet membrane prepared by dry in oven at
40°C show the low performance for both pressure-
normalized flux and selectivity. Even though the flat sheet
membranes prepared by dry at room temperature show the
high performance for both pressure-normalized flux and
selectivity, it does not choose due to the scanning image
produced, which show the symmetric membrane with the
formation of porous layer. The entire membrane thickness
causes resistance to mass transfer acting as selective
barrier.
Coating reduced the pressure normalized flux thus
enhance the membrane selectivity by caulking the pinholes
or defects on the membrane outer dense skin layer. The
PES membrane exhibited the best combination of pressure-
normalized flux and selectivity of O2/N2 was prepared by
dry/wet phase inversion. It average pressure-normalized
flux of about 25.39 GPU for O2, 10.12 GPU for N2 and
O2/N2 average selectivity of about 2.53 followed by dry at
room temperature technique and dry in oven at 40ºC
technique.
3.2 Effect of Pressure on O2/N2 Separation Membrane
Performance
3.2.1Performance of Uncoated Polyethersulfone
Membrane
All the uncoated membranes seem to exhibit higher
pressure-normalized flux but low selectivity. This is
probably due to the skin layer pores (defects) are dominant
between upstream and downstream side of the membrane
by a Knudsen or viscous flow process [7]. The extremely
high pressure-normalized fluxes of gases through the
membranes were due to the surface porosity [9]. The gas
transports through these membranes were predominantly
determined from the combination of Knudsen flow and
Poiseuille flow mechanism [9] and not fully by solution
diffusion. Knudsen flow happen when the pressure is low
mean pore in the barrier layer that are smaller diameter than
the distance a molecule would travel in the gas phase
between collisions to create a separation. The selectivity of
the uncoated asymmetric membranes is much lower
compare to the intrinsic value. According to Wang [9], the
O2/N2 intrinsic value of polyethersulfone dense film was
determined to be 6.1.Theoretically, the increase of the
pressure applied would increase the selectivity and
moreover the pressure-normalized flux would be decreased.
Figure 3.3 to Figure 3.5 show the summary of for
pressure-normalized flux and selectivity of uncoated
membranes with respects to pressure applied for each
drying technique.
Figure 3.3: Pressure-normalized flux and selectivity vs
pressure of uncoated membrane using dry/wet phase
inversion at different pressure
Figure 3.4: Pressure-normalized flux and selectivity vs
pressure of uncoated membrane using dry phase inversion
(dry-casting at room temperature) at different pressure
Figure 3.5: Pressure-normalized flux and selectivity vs
pressure of uncoated membrane using dry phase inversion
(dry in oven at 40ºC) at different pressure
3.2.2Performance of Coated Polyethersulfone Membrane
Membranes were coating using a standard coating
procedure in order to seal the skin layer defects [10]. The
advantage of using this coating is that it circumvents the
difficulty of membrane with a perfect skin [11]. Selectivity
of O2/N2 was higher than uncoated membrane for all
membrane prepared by all drying techniques.
 Figure 3.6 to 3.8 showed the pressure-normalized flux
was increase when the pressures increase for all membrane
prepared by all technique of drying. These happen due to
the gas transport through the membrane were
predominantly determined from the combination of
Knudsen flow and Poiseullie flow mechanism [9] and not
fully by solution diffusion. It’s showed that the highest
selectivities for each membrane with different drying
technique were at pressure 3 bar. These proved that, the
optimum pressure for all coated membrane prepared can be
achieved maximum pressure 3 bar. After pressure 3 bar, the
selectivities for all the membrane were decrease due to
molecule gases through the large pore which follow the
Poiseullie flow [9].
Figure 3.6: Pressure-normalized flux and selectivity vs
pressure of coated membrane using dry/wet phase inversion
at different pressure
Figure 3.7: Pressure-normalized flux and selectivity vs
pressure of coated membrane using dry phase inversion
(dry at room temperature) at different pressure
Figure 3.8: Pressure-normalized flux and selectivity vs
pressure of coated membrane using dry phase inversion
(dry in oven at 40ºC) at different pressure
The flat sheet membrane prepared by dry/wet phase
inversion show the higher selectivities which is 2.53 while
flat sheet membrane prepared by dry at room temperature
and dry in oven at 40°C show low selectivity of O 2/N2
which 2.06 and 1.29 respectively. The activation energies
for permeation of nitrogen and oxygen were higher for the
flat sheet membrane prepared by dry/wet phase inversion
than the flat sheet membrane prepared by dry at room
temperature and dry in oven at 40ºC due to the formation of
symmetric and asymmetric membrane [8]. Dry/wet phase
inversion technique form asymmetric membrane while dry
at room temperature and dry in oven at 40°C. The
activation energies for permeation of nitrogen and oxygen
was high in asymmetric due to the free volume of the
polymer in the asymmetric membrane skin layer is lower.
In symmetric membrane, pressure-normalized flux declined
with increasing pressure whilst for the asymmetric
membrane, pressure-normalized flux increase with
pressure. This clearly indicate that the skin layer
morphology of the flat sheet membrane prepared by
dry/wet phase inversion exhibits a smaller/different
distribution of free volume than the flat sheet membrane
prepared by the dry at room temperature and dry in oven at
40ºC.
3.3 Effect of Drying Technique on Morphology of
Uncoated and Coated membrane
The cross section morphologies of the flat sheet
membranes cast using different technique of drying were
investigated by scanning electron microscopy (SEM).
Figure 3.9: Cross section of coated membrane image by
using dry/wet phase inversion technique
Analysis on the cross section structure of membranes
that prepared by dry/wet phase inversion revealed that a
thin dense skin layer with highly porous substructure
appeared for both uncoated and coated membrane. Figure
4.9 show the formation of the asymmetric membrane with a
thin and a dense skin layer supported by a thick porous
sublayer compared to other. These structures look very
similar to those reported by Pesek and Koros (1993) [12].
and Pfromm, et al (1993)[13]. As shown in Figure 3.9,
there is an extremely well-defined skin layer supported on a
highly open-celled sponge-like structure that contained not
only microvoids but also bulbous macrovoids.
 According to Pinnau and Koros (1991) [12], and Figure 3.10: Cross section of coated membrane image by
Fleming (1993) [14], the dry/wet phase inversion processes using dry phase inversion (dry at room temperature)
comprises of the exposure of the nascent membrane to air technique
for a short duration (dry process) prior to entering a water
For the dry at room temperature technique, membrane
bath for coagulation (wet process). During this step,
consist of very thick, dense skin layer supported by a
solvent/or NSA evaporate from the surface layer of the
coarse, sponge-like, thick skin layer which look same as
nascent membrane, which results in increasing the local
sub layer and microvoid-free substructure as show in
polymer concentration. The rate of the evaporation depends
Figure 3.10 This structure may be explained by the
on the volatilities as well as temperature of the polymer
influences increasing the relative humidity of air affects the
solution and the atmosphere. A thin and dense skin layer is
formation process in two ways. First, the solution/air and
formed by gelatin and that the porous sublayer is the result
substrate/solution interfaces enter into the phase diagram
if liquid-liquid phase separation by nucleation and growth.
more rapidly and not at the same time. As the relative
The addition of solvent to the coagulation bath slows down
humidity of air increases, the driving force for the
the rate of the precipitation. As shown in Figure 3.9 above,
evaporation of water decreases causing more residual water
it show the existing of microvoid and macrovoids. The
trapped in the solution, and thus, more rapid phase
microvoids and macrovoids are believed to be formed by
separation. Second, increasing the relative humidity will
the intrusion of nonsolvent during the wet phase separation.
lead to a more graded and porous membrane structure with
As was suggested by Koenhen et al. (1977) [15], the a thinner skin layer.
skin is formed by gelation and that the porous sublayer is
result of liquid-liquid phase separation by nucleation and
growth. The factor determining the type of phase separation
at any point in the cast film is the local polymer
concentration at the moment of precipitation. In the first
split second after immersion there is a rapid depletion of
solvent from the film and a relatively small penetration of
non solvent. This means that the polymer concentration at
the film/ bath interface increases and dense gel layer that is
formed in this way, the skin, will act as a resistance to
solvent outdiffusion and at positions beneath the toplayer,
Figure 3.11: Cross section of coated membrane image by
demixing will occur at lower polymer and higher
using dry phase inversion (dry in oven at 40°C) technique
nonsolvent concentrations.

It look similar for the cross section structure for the

dry in oven at 40ºC technique which show the porous
membrane with macrovoid as show in Figure 3.13 and
Figure 3.14 for both uncoated and coated membrane
respectively. It is happen due to the temperature that use for
this technique nearly to room temperature. Hence, both of
the drying techniques show the formation of symmetric
membrane. The entire membrane thickness acts as selective
barrier, which mean the resistance of mass transfer, are
determined by the whole membrane. A decrease in
membrane thickness results in an increased permeation
rate.

Morphologies of the skin surface layer for uncoated

and coated membranes prepared from different technique
of drying are shown in Figure 3.12 (i), (ii) and (iii)
respectively. For coated membrane, the surface layer was
found to be quite smooth compared to uncoated
Uncoated Coated
membranes. It is because in asymmetric membranes usually
contained few defects, which attributed to the incomplete
(iii) Dry in oven at 40ºC
coalescence of the nodule aggregates of the composed skin
layer [16]. Membrane with polydimethylsiloxane (PDMS) Figure 3.12: Surface Layer for different technique of
coating was able to enhance the membrane performance,
drying
since the defects on the surface are seal smoothly as shown
in Figure 3.12 (ii). 4. Conclusion and Recommendation

4.1 Conclusion

Based on the results of this study, a number of conclusions

were drawn:

1) The dry/wet phase inversion technique was shown to

be more acceptable compared to than dry phase
inversion which dry at room temperature and dry in
Uncoated Coated oven at 40°C for the formation of PES asymmetric
membrane. Morphology of the flat sheet membrane
(i) Dry/wet Phase Inversion
show the asymmetric membrane structure with a thin
and dense skin layer supported by a thick porous
sublayer. For dry/wet phase inversion technique, the
formation of a dense skin layer has been shown to be
the result of the coalescence and deformation of the
polymer aggregates at the air –solution interface due
to capillary force and higher polymer concentration in
the surface layer compared to with that in the
supporting sublayer.
Uncoated Coated
2) All the uncoated membranes seem to exhibit higher
(ii)Dry at room temperature
pressure-normalized flux but low selectivity. This is
probably due to the skin layer pores (defects) are
dominant between upstream and downstream side of
the membrane by a Knudsen or viscous flow process.

3) The performance for the coated membrane show better

performance compare to the uncoated membrane due
to the skin layer defects for all techniques. Coating
 results in reduction of pressure normalized flux of all
gases, but can greatly enhance the selectivities of the
membranes by caulking the pinholes or defects on the
membranes dense layer. For flat sheet membrane
prepared by dry/wet for uncoated, the pressure-
normalized was found to be 1004.24 GPU for O2 while
for asymmetric membrane for coated was about 25.39
GPU for O2 and selectivity was low which is 2.52.
4) Optimum pressure for all flat sheet membrane
prepared by all drying technique shown at 3 bar. The
pressure-normalized flux proportionally with pressure
applied. The gas transports through these membranes
were predominantly determined from the combination
of Knudsen flow and Poiseuille flow mechanism [9]
and not fully by solution diffusion.
5) The O2/N2 selectivity of flat sheet membrane prepared
by dry/wet phase inversion show the highest value was
about 2.53 compared to others flat sheet membrane
prepared by others drying techniques. The selectivity
for the membrane prepared for the dry at room
temperature and dry in oven at 40°C was about 2.05
and 1.29 respectively.
4.2 Recommendation
Some recommendations have been made to improve
the result are given for future work.
1) The permeation test should be continued using
gas mixture. A variety factors can make mixed
gas separation results different from those test
with only pure gas
2) Instead of used casting block in membrane
casting procedure, the usage of pneumatically
controlled casting machine is applicable in order
to minimize error occuring during casting
process.
3) Asymmetric membrane should be prepared with a
variety of polymer, solvent and coagulation
medium in order to generalize membrane
formation process.
4) Comprehensive studies on other fabrication
parameters of asymmetric membrane such as
evaporation temperature, coagulation temperature
and drying method must be carried out to further
optimize membrane formation process.
5) Onsite testing should be conducted to determine
other effects such as operating temperature and
pressure, humidity and aging on membrane
properties in order to justify applicability of
asymmetric membrane in actual application
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